Avoidance of stress corrosion susceptibility in high strength aluminum alloys by control of grain boundary and matrix microstructure

NASA Technical Reports Server (NTRS)

Adler, P.; Deiasi, R.

1974-01-01

The relation of microstructure to the mechanical strength and stress corrosion resistance of highest strength and overaged tempers of BAR and 7050 aluminum alloys was investigated. Comparison is made with previously studied 7075 aluminum alloy. Optical microscopy, transmission electron microscopy, and differential scanning calorimetry were used to characterize the grain morphology, matrix microstructure, and grain boundary microstructure of these tempers. Grain boundary interparticle spacing was significant to stress corrosion crack propagation for all three alloys; increasing interparticle spacing led to increased resistance to crack propagation. In addition, the fire grain size in Bar and 7050 appears to enhance crack propagation. The highest strength temper of 7050 has a comparatively high resistance to crack initiation. Overall stress corrosion behavior is dependent on environment pH, and evaluation over a range of pH is recommended.

Quantitative analysis and feature recognition in 3-D microstructural data sets

NASA Astrophysics Data System (ADS)

Lewis, A. C.; Suh, C.; Stukowski, M.; Geltmacher, A. B.; Spanos, G.; Rajan, K.

2006-12-01

A three-dimensional (3-D) reconstruction of an austenitic stainless-steel microstructure was used as input for an image-based finite-element model to simulate the anisotropic elastic mechanical response of the microstructure. The quantitative data-mining and data-warehousing techniques used to correlate regions of high stress with critical microstructural features are discussed. Initial analysis of elastic stresses near grain boundaries due to mechanical loading revealed low overall correlation with their location in the microstructure. However, the use of data-mining and feature-tracking techniques to identify high-stress outliers revealed that many of these high-stress points are generated near grain boundaries and grain edges (triple junctions). These techniques also allowed for the differentiation between high stresses due to boundary conditions of the finite volume reconstructed, and those due to 3-D microstructural features.

Effect of Austenite Deformation on the Microstructure Evolution and Grain Refinement Under Accelerated Cooling Conditions

NASA Astrophysics Data System (ADS)

Zhao, H.; Palmiere, E. J.

2017-07-01

Although there has been much research regarding the effect of austenite deformation on accelerated cooled microstructures in microalloyed steels, there is still a lack of accurate data on boundary densities and effective grain sizes. Previous results observed from optical micrographs are not accurate enough, because, for displacive transformation products, a substantial part of the boundaries have disorientation angles below 15 deg. Therefore, in this research, a niobium microalloyed steel was used and electron backscattering diffraction mappings were performed on all of the transformed microstructures to obtain accurate results on boundary densities and grain refinement. It was found that with strain rising from 0 to 0.5, a transition from bainitic ferrite to acicular ferrite occurs and the effective grain size reduces from 5.7 to 3.1 μm. When further increasing strain from 0.5 to 0.7, dynamic recrystallization was triggered and postdynamic softening occurred during the accelerated cooling, leading to an inhomogeneous and coarse transformed microstructure. In the entire strain range, the density changes of boundaries with different disorientation angles are distinct, due to different boundary formation mechanisms. Finally, the controversial influence of austenite deformation on effective grain size of low-temperature transformation products was argued to be related to the differences in transformation conditions and final microstructures.

On the role of grain boundary character distribution in grain growth of Al-Mg alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Matsumoto, K.; Shibayanagi, T.; Umakoshi, Y.

1997-02-01

Grain growth behavior of recrystallized Al-Mg alloys containing 0.3 and 2.7 mass% Mg was investigated, focusing on the interconnection between development of the texture and grain boundary character distribution. An Al-0.3 mass% Mg alloy showed two stages in the change of microstructure during grain growth: the frequency of cube oriented grains and the {Sigma}1 boundary significantly increased at an early stage and then decreased. In the second stage a small amount of isolated large grains with the non-cube component grew and consumed the surrounding cube grains. In contrast, the frequency of cube oriented grains and the grain boundary character distributionmore » showed no significant change during grain growth of Al-2.7 mass% Mg. Small clusters composed of several cube grains containing {Sigma}1 boundaries were formed and their spatial distribution played an important role in the change of microstructure during grain growth. The effect of the spatial distribution on the grain growth behavior was discussed considering the energy balance at triple junctions of grain boundaries.« less

Microstructural effects on damage evolution in shocked copper polycrystals

DOE PAGES

Lieberman, Evan J.; Lebensohn, Ricardo A.; Menasche, David B.; ...

2016-07-01

Three-dimensional crystal orientation fields of a copper sample, characterized before and after shock loading using High Energy Diffraction Microscopy, are used for input and validation of direct numerical simulations using a Fast Fourier Transform (FFT)-based micromechanical model. The locations of the voids determined by X-ray tomography in the incipiently-spalled sample, predominantly found near grain boundaries, were traced back and registered to the pre-shocked microstructural image. Using FFT-based simulations with direct input from the initial microstructure, micromechanical fields at the shock peak stress were obtained. Statistical distributions of micromechanical fields restricted to grain boundaries that developed voids after the shock aremore » compared with corresponding distributions for all grain boundaries. Distributions of conventional measures of stress and strain (deviatoric and mean components) do not show correlation with the locations of voids in the post-shocked image. Neither does stress triaxiality, surface traction or grain boundary inclination angle, in a significant way. On the other hand, differences in Taylor factor and accumulated plastic work across grain boundaries do correlate with the occurrence of damage. As a result, damage was observed to take place preferentially at grain boundaries adjacent to grains having very different plastic response.« less

The Formation, Transport Properties and Microstructure of 45 Degrees (001) Tilt Grain Boundaries in Yttrium BARIUM(2) COPPER(3) OXYGEN(7-X) Thin Films

NASA Astrophysics Data System (ADS)

Vuchic, Boris Vukan

1995-01-01

Most high angle grain boundaries in high-T _{c} superconductors exhibit weak link behavior. The Josephson-like properties of these grain boundaries can be used for many device applications such as superconducting quantum interference devices (SQUIDs). The structure-property relationship of different types of 45 ^circ (001) YBa_2 Cu_3O_{7-x} thin film grain boundary junctions are examined to study their weak link nature. A technique, termed sputter-induced epitaxy, is developed to form 45^circ (001) tilt grain boundaries in YBa_2Cu _3O_{7-x} thin films on (100) MgO substrates. A low voltage ion bombardment pre-growth substrate treatment is used to modify the epitaxial orientation relationship between the thin film and the substrate in selected regions. By modifying the orientation of the thin film, grain boundary junctions can be placed in any configuration on the substrate. A variety of pre-growth sputtering conditions in conjunction with atomic force microscopy and Rutherford backscatter spectrometry are used to determine the role of the ions in modifying the substrate surface. Sputter-induced epitaxy is extended to a multilayer MgO/LaAlO_3 substrate, allowing integration of the sputter -induced epitaxy junctions into multilayer structures. The low temperature transport properties of the sputter-induced epitaxy junctions and a set of bi-epitaxial grain boundaries are studied. Individual grain boundaries are isolated and characterized for resistance vs. temperature, current vs. voltage as a function of temperature and magnetic field behavior. Resistive and superconducting grain boundaries are compared. Microstructural analysis is performed using scanning electron microscopy, transmission electron microscopy and high resolution electron microscopy (HREM). Marked differences are observed in the microstructure of resistive and superconducting grain boundaries. HREM studies suggest the importance of the local atomic scale structure of the grain boundary in transport properties. A phenomenological grain boundary model is proposed to describe the structure -property relationship of the boundaries.

Modeling and characterization of as-welded microstructure of solid solution strengthened Ni-Cr-Fe alloys resistant to ductility-dip cracking Part II: Microstructure characterization

NASA Astrophysics Data System (ADS)

Unfried-Silgado, Jimy; Ramirez, Antonio J.

2014-03-01

In part II of this work is evaluated the as-welded microstructure of Ni-Cr-Fe alloys, which were selected and modeled in part I. Detailed characterization of primary and secondary precipitates, subgrain and grain structures, partitioning, and grain boundary morphology were developed. Microstructural characterization was carried out using optical microscopy, SEM, TEM, EBSD, and XEDS techniques. These results were analyzed and compared to modeling results displaying a good agreement. The Hf additions produced the highest waviness of grain boundaries, which were related to distribution of Hf-rich carbonitrides. Experimental evidences about Mo distribution into crystal lattice have provided information about its possible role in ductility-dip cracking (DDC). Characterization results of studied alloys were analyzed and linked to their DDC resistance data aiming to establish relationships between as-welded microstructure and hot deformation performance. Wavy grain boundaries, primary carbides distribution, and strengthened crystal lattice are metallurgical characteristics related to high DDC resistance.

Grain Boundary Engineering the Mechanical Properties of Allvac 718Plus(Trademark) Superalloy

NASA Technical Reports Server (NTRS)

Gabb, Timothy P.; Telesman, Jack; Garg, Anita; Lin, Peter; Provenzano, virgil; Heard, Robert; Miller, Herbert M.

2010-01-01

Grain Boundary Engineering can enhance the population of structurally-ordered "low S" Coincidence Site Lattice (CSL) grain boundaries in the microstructure. In some alloys, these "special" grain boundaries have been reported to improve overall resistance to corrosion, oxidation, and creep resistance. Such improvements could be quite beneficial for superalloys, especially in conditions which encourage damage and cracking at grain boundaries. Therefore, the effects of GBE processing on high-temperature mechanical properties of the cast and wrought superalloy Allvac 718Plus (Allvac ATI) were screened. Bar sections were subjected to varied GBE processing, and then consistently heat treated, machined, and tested at 650 C. Creep, tensile stress relaxation, and dwell fatigue crack growth tests were performed. The influences of GBE processing on microstructure, mechanical properties, and associated failure modes are discussed.

Role of Grain Boundaries under Long-Time Radiation

NASA Astrophysics Data System (ADS)

Zhu, Yichao; Luo, Jing; Guo, Xu; Xiang, Yang; Chapman, Stephen Jonathan

2018-06-01

Materials containing a high proportion of grain boundaries offer significant potential for the development of radiation-resistant structural materials. However, a proper understanding of the connection between the radiation-induced microstructural behavior of a grain boundary and its impact at long natural time scales is still missing. In this Letter, point defect absorption at interfaces is summarized by a jump Robin-type condition at a coarse-grained level, wherein the role of interface microstructure is effectively taken into account. Then a concise formula linking the sink strength of a polycrystalline aggregate with its grain size is introduced and is well compared with experimental observation. Based on the derived model, a coarse-grained formulation incorporating the coupled evolution of grain boundaries and point defects is proposed, so as to underpin the study of long-time morphological evolution of grains induced by irradiation. Our simulation results suggest that the presence of point defect sources within a grain further accelerates its shrinking process, and radiation tends to trigger the extension of twin boundary sections.

Room-Temperature and High-Temperature Tensile Mechanical Properties of TA15 Titanium Alloy and TiB Whisker-Reinforced TA15 Matrix Composites Fabricated by Vacuum Hot-Pressing Sintering

PubMed Central

Feng, Yangju; Zhang, Wencong; Zeng, Li; Cui, Guorong; Chen, Wenzhen

2017-01-01

In this paper, the microstructure, the room-temperature and high-temperature tensile mechanical properties of monolithic TA15 alloy and TiB whisker-reinforced TA15 titanium matrix composites (TiBw/TA15) fabricated by vacuum hot-pressing sintering were investigated. The microstructure results showed that there were no obvious differences in the microstructure between monolithic TA15 alloy and TiBw/TA15 composites, except whether or not the grain boundaries contained TiBw. After sintering, the matrix microstructure presented a typical Widmanstätten structure and the size of primary β grain was consistent with the size of spherical TA15 titanium metallic powders. This result demonstrated that TiBw was not the only factor limiting grain coarsening of the primary β grain. Moreover, the grain coarsening of α colonies was obvious, and high-angle grain boundaries (HAGBs) were distributed within the primary β grain. In addition, TiBw played an important role in the microstructure evolution. In the composites, TiBw were randomly distributed in the matrix and surrounded by a large number of low-angle grain boundaries (LAGBs). Globularization of α phase occurred prior, near the TiBw region, because TiBw provided the nucleation site for the equiaxed α phase. The room-temperature and high-temperature tensile results showed that TiBw distributed at the primary β grain boundaries can strengthen the grain boundary, but reduce the connectivity of the matrix. Therefore, compared to the monolithic TA15 alloy fabricated by the same process, the tensile strength of the composites increased, and the tensile elongation decreased. Moreover, with the addition of TiBw, the fracture mechanism was changed to a mixture of brittle fracture and ductile failure (composites) from ductile failure (monolithic TA15 alloy). The fracture surfaces of TiBw/TA15 composites were the grain boundaries of the primary β grain where the majority of TiB whiskers distributed, i.e., the surfaces of the spherical TA15 titanium metallic powders. PMID:28772786

Room-Temperature and High-Temperature Tensile Mechanical Properties of TA15 Titanium Alloy and TiB Whisker-Reinforced TA15 Matrix Composites Fabricated by Vacuum Hot-Pressing Sintering.

PubMed

Feng, Yangju; Zhang, Wencong; Zeng, Li; Cui, Guorong; Chen, Wenzhen

2017-04-18

In this paper, the microstructure, the room-temperature and high-temperature tensile mechanical properties of monolithic TA15 alloy and TiB whisker-reinforced TA15 titanium matrix composites (TiBw/TA15) fabricated by vacuum hot-pressing sintering were investigated. The microstructure results showed that there were no obvious differences in the microstructure between monolithic TA15 alloy and TiBw/TA15 composites, except whether or not the grain boundaries contained TiBw. After sintering, the matrix microstructure presented a typical Widmanstätten structure and the size of primary β grain was consistent with the size of spherical TA15 titanium metallic powders. This result demonstrated that TiBw was not the only factor limiting grain coarsening of the primary β grain. Moreover, the grain coarsening of α colonies was obvious, and high-angle grain boundaries (HAGBs) were distributed within the primary β grain. In addition, TiBw played an important role in the microstructure evolution. In the composites, TiBw were randomly distributed in the matrix and surrounded by a large number of low-angle grain boundaries (LAGBs). Globularization of α phase occurred prior, near the TiBw region, because TiBw provided the nucleation site for the equiaxed α phase. The room-temperature and high-temperature tensile results showed that TiBw distributed at the primary β grain boundaries can strengthen the grain boundary, but reduce the connectivity of the matrix. Therefore, compared to the monolithic TA15 alloy fabricated by the same process, the tensile strength of the composites increased, and the tensile elongation decreased. Moreover, with the addition of TiBw, the fracture mechanism was changed to a mixture of brittle fracture and ductile failure (composites) from ductile failure (monolithic TA15 alloy). The fracture surfaces of TiBw/TA15 composites were the grain boundaries of the primary β grain where the majority of TiB whiskers distributed, i.e., the surfaces of the spherical TA15 titanium metallic powders.

Influence of heat treatment on microstructure and hot crack susceptibility of laser-drilled turbine blades made from Rene 80

DOE Office of Scientific and Technical Information (OSTI.GOV)

Osterle, W.; Krause, S.; Moelders, T.

2008-11-15

Turbine components from conventionally cast nickel-base alloy Rene 80 show different hot cracking susceptibilities depending on their heat treatment conditions leading to slightly different microstructures. Electron probe micro-analysis, focused ion beam technique and analytical transmission electron microscopy were applied to reveal and identify grain boundary precipitates and the {gamma}-{gamma}'-microstructure. The distribution of borides along grain boundaries was evaluated statistically by quantitative metallography. The following features could be correlated with an increase of cracking susceptibility: i) Increasing grain size, ii) increasing fraction of grain boundaries with densely spaced borides, iii) lack of secondary {gamma}'-particles in matrix channels between the coarse cuboidalmore » {gamma}'-precipitates. The latter feature seems to be responsible for linking-up of cracked grain boundary precipitates which occurred as an additional cracking mechanism after one heat treatment, whereas decohesion at the boride-matrix-interface in the heat affected zone of laser-drilled holes was observed for both heat treatments.« less

Deformation-related recrystallization processes

NASA Astrophysics Data System (ADS)

Drury, Martyn R.; Urai, Janos L.

1990-02-01

Recrystallization is a common microstructural transformation that occurs during deformation, metamorphism and diagenesis of rocks. Studies on minerals and rock analogues have demonstrated that a wide range of recrystallization mechanisms can occur. The range of mechanisms is related to the various ways in which two basic processes, grain boundary migration and new grain boundary formation combine to transform the microstructure. Two recent papers (Drury et al., 1985; Urai et al., 1986) have proposed different schemes for the description of recrystallization mechanisms. The purpose of this paper is to provide a unified framework for the description of mechanisms. Recrystallization mechanisms are divided into three main types; rotation mechanisms which principally involve the formation of new grain boundaries; migration mechanisms which principally involve grain boundary migration; and general mechanisms which involve both basic processes. A further distinction is made on the basis of the continuity of the microstructural transformation with respect to time. Each of the three main types of mechanism can be divided into a number of sub-types depending on whether the processes of grain boundary migration, new grain boundary formation and new grain formation occur in a discontinuous or continuous manner with respect to time. As the terms continuous and discontinuous have been used in the metallurgical literature to signify the spatial continuity of the microstructural transformation, the terms discontinuai and continual are used to refer to the temporal continuity of the transformation. It is recommended that the following aspects should be specified, if possible, in a general description of recrystallization mechanisms: (1) How do the basic processes combine to transform the microstructure. (2) If new grain development occurs, what is the development mechanism, and does new grain formation occur in a continual or discontinuai manner. (3) If grain boundary migration is involved in the transformation, what is the migration mechanism (i.e. fast solute escape migration, slow solute loaded migration, fluid assisted migration, etc.), and is migration a continual or discontinuai process. The application of the unified scheme is illustrated by reviewing studies that have provided detailed information on the recrystallization mechanisms involved. The complicating effects of solid solution impurities, dispersed second phase particles and grain boundary fluid films are also considered and it is demonstrated that variations in content of these types of impurity can significantly effect the types of recrystallization that occur in a given material.

Appling grain boundary engineering to Alloy 690 tube for enhancing intergranular corrosion resistance

NASA Astrophysics Data System (ADS)

Xia, Shuang; Li, Hui; Liu, Ting Guang; Zhou, Bang Xin

2011-09-01

The feasibility of applying the grain boundary engineering (GBE) processing to Alloy 690 tube manufacturing for improving the intergranular corrosion resistance was studied. Through small amount of deformation by cold drawing using a draw-bench on a production line and subsequent short time annealing at high temperature, the proportion of low Σ coincidence site lattice (CSL) grain boundaries of the Alloy 690 tube can be enhanced to about 75% which mainly were of Σ3 n ( n = 1, 2, 3, …) type. In this case, the grain boundary network (GBN) was featured by the formation of highly twinned large size grain-clusters produced by multiple twinning during recrystallization. All of the grains inside this kind of cluster had Σ3 n mutual misorientations, and hence all the boundaries inside the cluster were of Σ3 n type and formed many interconnected Σ3 n type triple junctions. The weight losses due to grain dropping during intergranular corrosion for the samples with the modified GBN were much less than that with conventional microstructure. Based on the characterization by scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) technique, it was shown that the highly twinned large size grain-cluster microstructure played a key role in enhancing the intergranular corrosion resistance: (1) the large grain-cluster can arrest the penetration of intergranular corrosion; (2) the large grain-cluster can protect the underlying microstructure.

DOE Office of Scientific and Technical Information (OSTI.GOV)

El-Atwani, Osman; Taylor, Chase N.; Frishkoff, James

Here, microstructural changes due to displacement damage and helium desorption are two phenomena that occur in tungsten plasma facing materials in fusion reactors. Nanocrystalline metals are being investigated as radiation tolerant materials that can mitigate these microstructural changes and better trap helium along their grain boundaries. Here, we investigate the performance of three tungsten grades (nanocrystalline, ultrafine and ITER grade tungsten), exposed to a high fluence of 4 keV helium at both RT and 773 K, during a thermal desorption spectroscopy (TDS) experiment. An investigation of the microstructure in pre-and post-TDS sample sets was performed. The amount of desorbed heliummore » was shown to be highest in the ITER grade tungsten and lowest in the nanocrystalline tungsten. Correlating the desorption spectra and the microstructure (grain boundaries decorated with nanopores and crack formation) and comparing with previous literature on coarse grained tungsten samples at similar irradiation and TDS conditions, revealed the importance of grain boundaries in trapping helium and limiting helium desorption up to a high temperature of 1350 K in agreement with transmission electron microscopy studies on helium irradiated tungsten which showed preferential and large facetted bubble formation along the grain boundaries in the nanocrystalline tungsten grade.« less

Microstructural characterization and electron backscatter diffraction analysis across the welded interface of duplex stainless steel

NASA Astrophysics Data System (ADS)

Zhang, Zhiqiang; Jing, Hongyang; Xu, Lianyong; Han, Yongdian; Gao, Zhanqi; Zhao, Lei; Zhang, Jianli

2017-08-01

The microstructural evolution, orientation relationships, boundary characteristics, grain type, local deformation, and microhardness across the welded interface of duplex stainless steel (DSS) were investigated. The DSS welded joint consisted of four typical zones: base metal (BM), low-temperature heat-affected zone (LTHAZ), high-temperature heat-affected zone (HTHAZ), and weld metal (WM). The apparent microstructural changes in the HTHAZ and LTHAZ were secondary austenite and Cr2N precipitation. A modified cooperative precipitation mechanism of secondary austenite and Cr2N at the interface was proposed. Furthermore, the ferrite in both the HTHAZ and LTHAZ maintained the same distribution as the ferrite texture in the BM, while this ferrite texture disappeared completely in the WM. Different austenite grains in the different zones exhibited different orientation relationships with the ferrite matrix. Special grain boundaries were mainly distributed between the austenite grains, while the ferrite grains primarily contained random grain boundaries. Austenite twins constituted the largest proportion of the special boundaries. The special austenite grain boundaries in the BM and LTHAZ were higher in relative frequency than those in the HTHAZ and WM. The ferrite grains in the HTHAZ and WM mainly consisted of substructured grains. In the BM, the recrystallization degree of ferrite was significantly lower than that of austenite grains. The local deformations were mainly generated in the grain boundaries and within the deformed grains. The HTHAZ exhibited the highest hardness, while the BM had the lowest hardness. The LTHAZ had a lower hardness than the HTHAZ and higher hardness than the BM.

Experimental Characterization and Simulation of Slip Transfer at Grain Boundaries and Microstructurally-Sensitive Crack Propagation

NASA Technical Reports Server (NTRS)

Gupta, Vipul; Hochhalter, Jacob; Yamakov, Vesselin; Scott, Willard; Spear, Ashley; Smith, Stephen; Glaessgen, Edward

2013-01-01

A systematic study of crack tip interaction with grain boundaries is critical for improvement of multiscale modeling of microstructurally-sensitive fatigue crack propagation and for the computationally-assisted design of more durable materials. In this study, single, bi- and large-grain multi-crystal specimens of an aluminum-copper alloy are fabricated, characterized using electron backscattered diffraction (EBSD), and deformed under tensile loading and nano-indentation. 2D image correlation (IC) in an environmental scanning electron microscope (ESEM) is used to measure displacements near crack tips, grain boundaries and within grain interiors. The role of grain boundaries on slip transfer is examined using nano-indentation in combination with high-resolution EBSD. The use of detailed IC and EBSD-based experiments are discussed as they relate to crystal-plasticity finite element (CPFE) model calibration and validation.

Effects of Intergranular Gas Bubbles on Thermal Conductivity

DOE Office of Scientific and Technical Information (OSTI.GOV)

K. Chockalingam; Paul C. Millett; M. R. Tonks

2012-11-01

Model microstructures obtained from phase-field simulations are used to study the effective heat transfer across bicrys- tals with stationary grain boundary bubble populations. We find that the grain boundary coverage, irrespective of the intergranular bubble radii, is the most relevant parameter to the thermal resistance, which we use to derive effec- tive Kapitza resistances that are dependent on the grain boundary coverage and Kaptiza resistance of the intact grain boundary. We propose a model to predict thermal conductivity as a function of porosity, grain-size, Kaptiza resistance of the intact grain boundary, and grain boundary bubble coverage.

Three-dimensional study of grain boundary engineering effects on intergranular stress corrosion cracking of 316 stainless steel in high temperature water

NASA Astrophysics Data System (ADS)

Liu, Tingguang; Xia, Shuang; Bai, Qin; Zhou, Bangxin; Zhang, Lefu; Lu, Yonghao; Shoji, Tetsuo

2018-01-01

The intergranular cracks and grain boundary (GB) network of a GB-engineered 316 stainless steel after stress corrosion cracking (SCC) test in high temperature high pressure water of reactor environment were investigated by two-dimensional and three-dimensional (3D) characterization in order to expose the mechanism that GB-engineering mitigates intergranular SCC. The 3D microstructure shown that the essential characteristic of the GB-engineered microstructure is formation of many large twin-boundaries as a result of multiple-twinning, which results in the formation of large grain-clusters. The large grain-clusters played a key role to the improvement of intergranular SCC resistance by GB-engineering. The main intergranular cracks propagated in a zigzag along the outer boundaries of these large grain-clusters because all inner boundaries of the grain-clusters were twin-boundaries (∑3) or twin-related boundaries (∑3n) which had much lower susceptibility to SCC than random boundaries. These large grain-clusters had tree-ring-shaped topology structure and very complex morphology. They got tangled so that difficult to be separated during SCC, resulting in some large crack-bridges retained in the crack surface.

Intergranular degradation assessment via random grain boundary network analysis

DOEpatents

Kumar, Mukul; Schwartz, Adam J.; King, Wayne E.

2002-01-01

A method is disclosed for determining the resistance of polycrystalline materials to intergranular degradation or failure (IGDF), by analyzing the random grain boundary network connectivity (RGBNC) microstructure. Analysis of the disruption of the RGBNC microstructure may be assess the effectiveness of materials processing in increasing IGDF resistance. Comparison of the RGBNC microstructures of materials exposed to extreme operating conditions to unexposed materials may be used to diagnose and predict possible onset of material failure due to

Grain boundary microstructure, chemistry, and IGSCC in Alloy 600 and Alloy 690

DOE Office of Scientific and Technical Information (OSTI.GOV)

Norring, K.; Stiller, K.; Nilsson, J.O.

1992-12-31

The resistance to intergranular stress corrosion cracking of six different Alloy 600 and Alloy 690 steam generator tubes has been investigated. The composition of the materials at grain boundaries has been investigated using analytical transmission electron microscopy and atom probe field ion microscopy techniques. The depletion of chromium at the grain boundaries has been related to the type of grain boundary precipitates. Segregation of carbon and boron to the grain boundaries has been observed and quantified.

Selective Growth of Low Stored Energy Grains During δ Sub-solvus Annealing in the Inconel 718 Nickel-Based Superalloy

NASA Astrophysics Data System (ADS)

Agnoli, Andrea; Bernacki, Marc; Logé, Roland; Franchet, Jean-Michel; Laigo, Johanne; Bozzolo, Nathalie

2015-09-01

The microstructure stability during δ sub-solvus annealing in Inconel 718 was investigated, focusing on the conditions that may lead to the development of very large grains (about 100 μm) in a recrystallized fine grained matrix (4 to 5 μm) despite the presence of second-phase particles. Microstructure evolution was analyzed by EBSD (grain size, intragranular misorientation) and SEM ( δ phase particles). Results confirm that, in the absence of stored energy, the grain structure is controlled by the δ phase particles, as predicted by the Smith-Zener equation. If the initial microstructure is strained ( ɛ < 0.1) before annealing, then low stored energy grains grow to a large extent, despite the Zener pinning forces exerted by the second-phase particles on the grain boundaries. Those selectively growing grains could be those of the initial microstructure that were the least deformed, or they could result from a nucleation process. The balance of three forces acting on boundary migration controls the growth process: if the sum of capillarity and stored energy driving forces exceeds the Zener pinning force, then selective grain growth occurs. Such phenomenon could be simulated, using a level set approach in a finite element context, by taking into account the three forces acting on boundary migration and by considering a realistic strain energy distribution (estimated from EBSD measurements).

Thermal desorption spectroscopy of high fluence irradiated ultrafine and nanocrystalline tungsten: helium trapping and desorption correlated with morphology

NASA Astrophysics Data System (ADS)

El-Atwani, O.; Taylor, C. N.; Frishkoff, J.; Harlow, W.; Esquivel, E.; Maloy, S. A.; Taheri, M. L.

2018-01-01

Microstructural changes due to displacement damage and helium desorption are two phenomena that occur in tungsten plasma facing materials in fusion reactors. Nanocrystalline metals are being investigated as radiation tolerant materials that can mitigate these microstructural changes and better trap helium along their grain boundaries. Here, we investigate the performance of three tungsten grades (nanocrystalline, ultrafine and ITER grade tungsten), exposed to a high fluence of 4 keV helium at both RT and 773 K, during a thermal desorption spectroscopy (TDS) experiment. An investigation of the microstructure in pre-and post-TDS sample sets was performed. The amount of desorbed helium was shown to be highest in the ITER grade tungsten and lowest in the nanocrystalline tungsten. Correlating the desorption spectra and the microstructure (grain boundaries decorated with nanopores and crack formation) and comparing with previous literature on coarse grained tungsten samples at similar irradiation and TDS conditions, revealed the importance of grain boundaries in trapping helium and limiting helium desorption up to a high temperature of 1350 K in agreement with transmission electron microscopy studies on helium irradiated tungsten which showed preferential and large facetted bubble formation along the grain boundaries in the nanocrystalline tungsten grade.

Thermal desorption spectroscopy of high fluence irradiated ultrafine and nanocrystalline tungsten: helium trapping and desorption correlated with morphology

DOE PAGES

El-Atwani, Osman; Taylor, Chase N.; Frishkoff, James; ...

2017-11-09

Here, microstructural changes due to displacement damage and helium desorption are two phenomena that occur in tungsten plasma facing materials in fusion reactors. Nanocrystalline metals are being investigated as radiation tolerant materials that can mitigate these microstructural changes and better trap helium along their grain boundaries. Here, we investigate the performance of three tungsten grades (nanocrystalline, ultrafine and ITER grade tungsten), exposed to a high fluence of 4 keV helium at both RT and 773 K, during a thermal desorption spectroscopy (TDS) experiment. An investigation of the microstructure in pre-and post-TDS sample sets was performed. The amount of desorbed heliummore » was shown to be highest in the ITER grade tungsten and lowest in the nanocrystalline tungsten. Correlating the desorption spectra and the microstructure (grain boundaries decorated with nanopores and crack formation) and comparing with previous literature on coarse grained tungsten samples at similar irradiation and TDS conditions, revealed the importance of grain boundaries in trapping helium and limiting helium desorption up to a high temperature of 1350 K in agreement with transmission electron microscopy studies on helium irradiated tungsten which showed preferential and large facetted bubble formation along the grain boundaries in the nanocrystalline tungsten grade.« less

Microstructural Damage During High-Strain Torsion Experiments on Calcite-Anhydrite Aggregates

NASA Astrophysics Data System (ADS)

Cross, A. J.; Skemer, P. A.

2016-12-01

Ductile shear zones play a critical role in localising deformation in the Earth's crust and mantle. Severe grain size reduction - a ubiquitous feature of natural mylonites - is commonly thought to cause strain weakening via a transition to grain size sensitive deformation mechanisms. Although grain size reduction is modulated by grain growth in single-phase aggregates, grain boundary pinning in well-mixed poly-phase composites can inhibit grain growth, leading to microstructural `damage' which is likely a critical element of strain localization in the lithosphere. While dynamic recrystallization has been widely explored in rock mechanics and materials science, the mechanisms behind phase-mixing remain poorly understood. In this contribution we present results from high-strain, deformation experiments on calcite-anhydrite composites. Experiments were conducted in torsion at T = 500-700°C and P 1.5 GPa, using the new Large Volume Torsion (LVT) solid-medium apparatus, to shear strains of 0.5-30. As shear strain increases, progressive thinning and necking of initially large (≤ 1 mm) calcite domains is observed, resulting in an increase in the proportion of interphase boundaries. Grain-size is negatively correlated with the fraction of interphase boundaries, such that calcite grains in well-mixed regions are significantly smaller than those in single-phase domains. Crucially, progressive deformation leads to a reduction in grain-size beyond the lower limit established by the grain size piezometer for mono-phase calcite, implying microstructural damage. These data therefore demonstrate continued microstructural evolution in two-phase composites that is not possible in single-phase aggregates. These observations mark a new `geometric' mechanism for phase mixing, complementing previous models for phase mixing involving chemical reactions, material diffusion, and/or grain boundary sliding.

Capturing the Complexity of Additively Manufactured Microstructures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Livescu, Veronica; Bronkhorst, Curt Allan; Vander Wiel, Scott Alan

2016-05-12

The underlying mechanisms and kinetics controlling damage nucleation and growth as a function of material microstructure and loading paths are discussed. These experiments indicate that structural features such as grain boundaries, grain size distribution, grain morphology crystallographic texture are all factors that influence mechanical behavior.

Microstructure, texture, and mechanical properties of friction stir welded commercial brass alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Heidarzadeh, A., E-mail: ak.hz62@gmail.com

Microstructural evolution during friction stir welding of single-phase brass and corresponding mechanical properties were investigated. For this purpose, 2 mm thick brass plate was friction stir welded at a rotational speed of 450 rpm and traverse speed of 100 mm/min. The microstructure of the joint was studied using optical microscopy, scanning electron microscopy equipped with electron back scattered diffraction system, and scanning transmission electron microscopy. The mechanical properties were measured using hardness and tensile tests. The formation of subgrains and their transformation into new grains in conjunction with existence of A{sub 1}{sup ⁎}, A{sub 2}{sup ⁎} and C texture componentsmore » revealed that the continuous dynamic recrystallization plays a dominant role in the microstructural evolution. However, grain boundary bulging, along with the formation of twin boundaries, and presence of the G texture component showed that the discontinues dynamic recrystallization may participate in the new grain formation. Furthermore, the different strengthening mechanisms, which caused the higher strength of the joint, were discussed. - Highlights: •Microstructural evolution during FSW of a single phase brass was investigated. •CDRX and DDRX were the main mechanisms of the grain structure formation during FSW. •GDRX and SRX were not contributed in grain structure formation. •The lamellas TBs were formed in the SZ of the joints. •Grain boundary, dislocation, and texture effects resulted in higher strength.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Wei, E-mail: wang_wei_310@163.com; Lu, Yonghao, E-mail: lu_yonghao@mater.ustb.edu.cn; Ding, Xianfei, E-mail: xfding@ustb.edu.cn

Microstructures and microhardness at fusion boundary of a weld joint were investigated in a 316 stainless steel/Inconel 182 dissimilar weldment. The results showed that there were two alternately distributed typical fusion boundaries, a narrow random boundary (possessed 15% in length) with a clear sharp interface and an epitaxial fusion one with (100){sub BM}//(100){sub WM} at the joint interface. The composition transition, microstructure and hardness across the fusion boundary strongly depended on the type of the fusion boundary. For the random boundary, there was a clear sharp interface and the composition transition with a width of 100 μm took place symmetricallymore » across the grain boundary. For the epitaxial fusion one, however, there were Type-I and Type-II grain boundaries perpendicular and parallel to the epitaxial fusion boundary, respectively. The composition transition took place in the Inconel 182 weld side. Σ3 boundaries in the HAZ of 316SS side and Σ5 grain boundaries in weld metal were usually observed, despite the type of fusion boundary, however the former was much more in epitaxial fusion boundary. Microhardness was continuously decreased across the random fusion boundary from the side of Inconel 182 to 316SS, but a hardening phenomenon appeared in the epitaxial fusion boundary zone because of its fine cellular microstructure. - Highlights: • Two typical fusion boundaries alternately distributed in the fusion interface • The microstructure, composition and hardness across fusion boundary depended on its type. • Different regions in welded joint have different special CSL value boundaries. • Hardening phenomenon only appeared in the epitaxial fusion boundary.« less

Microstructural Evolution at Micro/Meso-Scale in an Ultrafine-Grained Pure Aluminum Processed by Equal-Channel Angular Pressing with Subsequent Annealing Treatment.

PubMed

Xu, Jie; Li, Jianwei; Zhu, Xiaocheng; Fan, Guohua; Shan, Debin; Guo, Bin

2015-11-04

Micro-forming with ultrafine-grained (UFG) materials is a promising direction for the fabrication of micro-electro-mechanical systems (MEMS) components due to the improved formability, good surface quality, and excellent mechanical properties it provides. In this paper, micro-compression tests were performed using UFG pure aluminum processed by equal-channel angular pressing (ECAP) with subsequent annealing treatment. Microstructural evolution was investigated by electron back-scattered diffraction (EBSD) and transmission electron microscopy (TEM). The results show that microstructural evolutions during compression tests at the micro/meso-scale in UFG pure Al are absolutely different from the coarse-grained (CG) materials. A lot of low-angle grain boundaries (LAGBs) and recrystallized fine grains are formed inside of the original large grains in CG pure aluminum after micro-compression. By contrast, ultrafine grains are kept with few sub-grain boundaries inside the grains in UFG pure aluminum, which are similar to the original microstructure before micro-compression. The surface roughness and coordinated deformation ability can be signmicrostructure; micro/meso-forming; ultrafine grains; ECAP; aluminumificantly improved with UFG pure aluminum, which demonstrates that the UFG materials have a strong potential application in micro/meso-forming.

The spinodal decomposition in 17-4PH stainless steel subjected to long-term aging at 350 deg. C

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang Jun; Zou Hong; Li Cong

2008-05-15

The influence of aging time on the microstructure evolution of 17-4 PH martensitic stainless steel was studied by transmission electron microscopy (TEM). Results showed that the martensite decomposed by a spinodal decomposition mechanism after the alloy was subjected to long-term aging at 350 deg. C. The fine scale spinodal decomposition of {alpha}-ferrite brought about a Cr-enriched bright stripe and a Fe-enriched dark stripe, i.e., {alpha}' and {alpha} phases, separately, which were perpendicular to the grain boundary. The spinodal decomposition started at the grain boundary. Then with prolonged aging time, the decomposition microstructure expanded from the grain boundary to interior. Themore » wavelength of the spinodally decomposed microstructure changed little with extended aging time.« less

Linking Grain Boundary Microstructure to Stress Corrosion Cracking of Cold Rolled Alloy 690 in PWR Primary Water

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bruemmer, Stephen M.; Olszta, Matthew J.; Toloczko, Mychailo B.

2012-10-01

Grain boundary microstructures and microchemistries are examined in cold-rolled alloy 690 tubing and plate materials and comparisons are made to intergranular stress corrosion cracking (IGSCC) behavior in PWR primary water. Chromium carbide precipitation is found to be a key aspect for materials in both the mill annealed and thermally treated conditions. Cold rolling to high levels of reduction was discovered to produce small IG voids and cracked carbides in alloys with a high density of grain boundary carbides. The degree of permanent grain boundary damage from cold rolling was found to depend directly on the initial IG carbide distribution. Formore » the same degree of cold rolling, alloys with few IG precipitates exhibited much less permanent damage. Although this difference in grain boundary damage appears to correlate with measured SCC growth rates, crack tip examinations reveal that cracked carbides appeared to blunt propagation of IGSCC cracks in many cases. Preliminary results suggest that the localized grain boundary strains and stresses produced during cold rolling promote IGSCC susceptibility and not the cracked carbides and voids.« less

Three dimensional microstructural characterization of nanoscale precipitates in AA7075-T651 by focused ion beam (FIB) tomography

DOE Office of Scientific and Technical Information (OSTI.GOV)

Singh, Sudhanshu S.; Loza, Jose J.

2016-08-15

The size and distribution of precipitates in Al 7075 alloys affects both the mechanical and corrosion behavior (including stress corrosion cracking and fatigue corrosion) of the alloy. Three dimensional (3D) quantitative microstructural analysis of Al 7075 in the peak aged condition (T651) allows for a better understanding of these behaviors. In this study, Focused ion beam (FIB) tomography was used to characterize the microstructure in three dimensions. Analysis of grains and precipitates was performed in terms of volume, size, and morphology. It was found that the precipitates at the grain boundaries are larger in size, higher in aspect ratios andmore » maximum Feret diameter compared to the precipitates inside the grains, due to earlier nucleation of the precipitates at the grain boundaries. Our data on the precipitates at the interface between grains and Mg{sub 2}Si inclusion show that the surfaces of inclusion (impurity) particles can serve as a location for heterogeneous nucleation of precipitates. - Highlights: •Focused ion beam (FIB) tomography was used to characterize the microstructure of Al 7075 in three dimensions. •Analysis of grains and precipitates was performed in terms of volume, size, and morphology. •Precipitates at the grain boundaries have larger size and aspect ratio compared to the precipitates inside the grains.« less

Serial sectioning of grain microstructures under junction control: An old problem in a new guise

NASA Astrophysics Data System (ADS)

Zöllner, D.; Streitenberger, P.

2015-04-01

In the present work the importance of 3D and 4D microstructure analyses are shown. To that aim, we study polycrystalline grain microstructures obtained by grain growth under grain boundary, triple line and quadruple point control. The microstructures themselves are obtained by mesoscopic computer simulations, which enjoy a far greater control over the kinetic and thermodynamic parameters affecting grain growth than can be realized experimentally. In extensive simulation studies we find by 3D respectively 4D microstructure analyses that metrical and topological properties of the microstructures depend strongly on the microstructural feature controlling the growth kinetics. However, the differences between the growth kinetics vanish when we look at classical 2D sections of the 3D ensembles making a differentiation of the controlling grain feature near impossible.

A thermally activated dislocation-based constitutive flow model of nanostructured FCC metals involving microstructural evolution

NASA Astrophysics Data System (ADS)

Zhang, J. Y.; Li, J.; Wu, K.; Liu, G.; Sun, J.

2017-03-01

Due to their interface and nanoscale effects associated with structural peculiarities of nanostructured, face-centered-cubic (FCC) ultrafine-grained/nanocrystalline (UFG/NC) metals, in particular nanotwinned (NT) metals exhibit unexpected deformation behaviours fundamentally different from their coarse-grained (CG) counterparts. These internal boundaries, including grain boundaries and twin boundaries in UFG/NC metals, strongly interact with dislocations as deformation barriers to enhance the strength and strain rate sensitivity (SRS) of materials on the one hand, and play critical roles in their microstructural evolution as dislocation sources/sinks to sustain plastic deformation on the other. In this work, building on the findings of twin softening and (de)twinning-mediated grain growth/refinement in stretched free-standing NT-Ni foils, a constitutive model based on the thermally activated depinning process of dislocations residing in boundaries has been proposed to predict the steady-state grain size and simulate the plastic flow of NT-Ni, by considering the blocking effects of nanotwins on the absorption of dislocations emitted from boundaries. It is uncovered that the stress ratio (ηstress) of effective-to-internal stress can be taken as a signature to estimate the stability of microstructures during plastic deformation. This model not only reproduces well the plastic flow of the stretched NT-Ni foils as well as reported NT-Cu and the steady-state grain size, but also sheds light on the size-dependent SRS and failure of FCC UFG/NC metals. This theoretical framework offers the opportunity to tune the microstructures in the polycrystalline materials to synthesise high performance engineering materials with high strength and great ductility.

Evolution of Grain Boundary Precipitates in an Al-Cu-Li Alloy During Aging

NASA Astrophysics Data System (ADS)

Ott, Noémie; Kairy, Shravan K.; Yan, Yuanming; Birbilis, Nick

2017-01-01

The grain boundary microstructure of Al-Cu-Li alloy AA2050 was investigated for different isothermal aging times to rationalize intergranular corrosion (IGC) characteristics. In the underaged condition, the dominant grain boundary precipitates are fine T1 (Al2CuLi). Extended aging revealed that grain boundaries were decorated by large T1 precipitates and S' phase (Al2CuMg), with S' growth not dimensionally constrained. Such a transition in the precipitate type at grain boundaries is a unique feature of the Al-Cu-Li system.

The role of microstructure on deformation and damage mechanisms in a Nickel-based superalloy at elevated temperatures

NASA Astrophysics Data System (ADS)

Maciejewski, Kimberly E.

The overall objective of this research work is the development and implementation of a mechanistic based time-dependent crack growth model which considers the role of creep, fatigue and environment interactions on both the bulk and the grain boundary phase in ME3 disk material. The model is established by considering a moving crack tip along a grain boundary path in which damage events are described in terms of the grain boundary deformation and related accommodation processes. Modeling of these events was achieved by adapting a cohesive zone approach (an interface with internal singular surfaces) in which the grain boundary dislocation network is smeared into a Newtonian fluid element. The deformation behavior of this element is controlled by the continuum in both far field (internal state variable model) and near field (crystal plasticity model) and the intrinsic grain boundary viscosity which is characterized by microstructural parameters, including grain boundary precipitates and morphology, and is able to define the mobility of the element by scaling the motion of dislocations into a mesoscopic scale. Within the cohesive zone element, the motion of gliding dislocations in the tangential direction relates to the observed grain boundary sliding displacement, the rate of which is limited by the climb of dislocations over grain boundary obstacles. Effects of microstructural variation and orientation of the surrounding continuum are embedded in the tangential stress developing in the grain boundary. The mobility of the element in the tangential direction (i.e. by grain boundary sliding) characterizes the accumulation of irreversible displacement while the vertical movement (migration), although present, is assumed to alter stress by relaxation and, thus, is not considered a contributing factor in the damage process. This process is controlled by the rate at which the time-dependent sliding reaches a critical displacement and as such, a damage criterion is introduced by considering the mobility limit in the tangential direction leading to strain incompatibility and failure. This limit is diminished by environmental effects which are introduced as a dynamic embrittlement process that hinders grain boundary mobility due to oxygen diffusion. The concepts described herein indicate that implementation of the cohesive zone model requires the knowledge of the grain boundary external and internal deformation fields. The external field is generated by developing and coupling two continuum constitutive models including (i) a microstructure-explicit coarse scale crystal plasticity model with strength provided by tertiary and secondary gamma' precipitates. This scale is appropriate for the representation of the continuum region at the immediate crack tip, and (ii) a macroscopic internal state variable model for the purpose of modeling the response of the far field region located several grains away from the crack path. The hardening contributions of the gamma' precipitates consider dislocation/precipitate interactions in terms of gamma' particles shearing and/or Orowan by-passing mechanisms. The material parameters for these models are obtained from results of low cycle fatigue tests which were performed at three temperatures; 650, 704 and 760°C. Furthermore, a series of microstructure controlled experiments were carried out in order to develop and validate the microstructure dependency feature of the continuum constitutive models. The second requirement in the implementation of the cohesive zone model is a grain boundary deformation model which has been developed, as described above, on the basis of viscous flow rules of the boundary material. This model is supported by dwell crack growth experiments carried out at the three temperatures mentioned above, in both air and vacuum environments. Results of these tests have identified the frequency range in which the grain boundary cohesive zone model is applicable and also provided data to calculate the grain boundary activation energy as well as identifying the relative contributions of creep and environment in the critical sliding displacement leading to failure. Validation of the cohesive zone model has been carried out by comparing the simulated crack growth data with that obtained experimentally. This comparison is used to optimize the different model components and to provide a route to assess the relative significance of each of these components in relation to the intergranular damage associated with dwell fatigue crack growth in the ME3 alloy. For this purpose, a set of case studies were performed in order to illustrate the sensitivity of the cohesive zone model to variations in microstructure parameters (gamma ' statistics and grain boundary morphology) examined within the range of temperatures utilized in this study.

Chemical signature of a migrating grain boundaries in polycrystalline olivine

NASA Astrophysics Data System (ADS)

Boneh, Y.; Marquardt, K.; Skemer, P. A.

2017-12-01

Olivine is the most abundant phase and influences strongly the physical and chemical properties of the upper mantle. The structure and chemistry of olivine grain-boundaries is important to understand, as these interfaces provide a reservoir for incompatible elements and partial melt, and serve as a fast pathway for chemical diffusion. This project investigates the chemical characteristics of grain boundaries in an olivine-rich aggregate. The sample is composed of Fo50 olivine crystals with minor amounts of enstatite. It was previously deformed (Hansen et al., 2016) and then annealed (Boneh et al., 2017) to investigate the microstructural changes during recrystallization. This transient microstructure has a bimodal grain size distribution and includes grains that experienced abnormal grain-growth, (porphyroblasts) and highly strained grains with no significant recrystallization or growth (matrix). Using high-resolution transmission electron microscopy (HR-TEM) with energy dispersive X-ray (EDX) at the Bayerisches Geoinstitut (BGI), we characterized boundaries between pairs of porphyroblasts, pairs of matrix grains, and mixed boundaries between porphyroblast and matrix grains. It was found that the boundary between porphyroblasts is enriched in Al and Ca and depleted in Mg, in comparison to grain interiors. However, matrix-matrix boundaries show less chemical segregation of these elements. The relatively high level of chemical segregation to porphyroblast grain boundaries offers different possible interpretations: 1) During grain boundary migration incompatible elements are swept up by the migrating grain boundary. 2) Large angle grain boundaries provide a large density of energetically favorable storage sites for incompatible elements. 3) Diffusion along low angle grain boundaries is too slow to allow for fast chemical equilibration between the different grain boundaries. 4) Dislocations cores serve as an important transport media for impurities (i.e., Cottrell atmosphere). We will further discuss these different interpretations, their feasibility, and implications for the geochemistry of the mantle.

Microstructural and rheological evolution of calcite mylonites during shear zone thinning: Constraints from the Mount Irene shear zone, Fiordland, New Zealand

NASA Astrophysics Data System (ADS)

Negrini, Marianne; Smith, Steven A. F.; Scott, James M.; Tarling, Matthew S.

2018-01-01

Layers of calc-mylonite in the Mount Irene shear zone, Fiordland, New Zealand, show substantial variations in thickness due to deflection of the shear zone boundaries around wall rock asperities. In relatively thick parts (c. 2.6 m) of the shear zone, calcite porphyroclasts are internally strained, contain abundant subgrain boundaries and have a strong shape preferred orientation (SPO) and crystallographic preferred orientation (CPO), suggesting that deformation occurred mainly by dislocation creep involving subgrain-rotation recrystallization. In relatively thin parts (c. 1.5 m) of the shear zone, aggregates of fine-grained recrystallized calcite surrounding flattened porphyroclasts have a weak SPO and CPO, and contain polygonal calcite grains with low degrees of internal misorientation. The recrystallized aggregates also contain microstructures (e.g. grain quadruple junctions, randomized misorientation axes) similar to those reported for neighbor-switching processes during grain-boundary sliding. Comparison of subgrain sizes in the porphyroclasts to published grain-size differential-stress relationships indicates that stresses and strain rates were substantially higher in relatively thin parts of the shear zone. The primary microstructural response to higher stresses and strain rates was an increase in the amount of recrystallization to produce aggregates that deformed by grain-boundary sliding. However, even after the development of interconnected networks of recrystallized grains, dislocation creep by subgrain-rotation recrystallization continued to occur within porphyroclasts. This behavior suggests that the bulk rheology of shear zones undergoing thinning and thickening can be controlled by concomitant grain-size insensitive and grain-size sensitive mechanisms. Overall, our observations show that shear zone thickness variations at constant P-T can result in highly variable stresses and strain rates, which in turn modifies microstructure, deformation mechanism and shear zone rheology.

Stress Dependence of Microstructures in Experimentally Deformed Calcite

NASA Astrophysics Data System (ADS)

Platt, J. P.; De Bresser, J. H. P.

2017-12-01

Measurements of dynamically recrystallized grain size (Dr), subgrain size (Sg), minimum bulge size (Blg), and the maximum scale length for surface-energy driven grain-boundary migration (γGBM) in experimentally deformed Cararra marble help define the dependence of these microstructural features on stress and temperature. Measurements were made optically on ultra-thin sections in order to allow these features to be defined during measurement on the basis of microstructural setting and geometry. Taken together with previously published data Dr defines a paleopiezometer with a stress exponent of -1.09. There is no discernible temperature dependence over the 500°C temperature range of the experiments. Recrystallization occured mainly by bulging and subgrain rotation, and the two processes operated together, so that it is not possible to separate grains nucleated by the two mechanisms. Sg and Dr measured in the same samples are closely similar in size, suggesting that new grains do not grow significantly after nucleation, and that subgrain size is likely to be the primary control on recrystallized grain size. Blg and γGBM measured on each sample define a relationship to stress with an exponent of approximately -1.6, which helps define the boundary in stress - grain-size space between a region of dominant strain-energy-driven grain-boundary migration at high stress, from a region of dominant surface-energy-driven grain-boundary migration at low stress.

Multiscale modeling of thermal conductivity of high burnup structures in UO 2 fuels

DOE PAGES

Bai, Xian -Ming; Tonks, Michael R.; Zhang, Yongfeng; ...

2015-12-22

The high burnup structure forming at the rim region in UO 2 based nuclear fuel pellets has interesting physical properties such as improved thermal conductivity, even though it contains a high density of grain boundaries and micron-size gas bubbles. To understand this counterintuitive phenomenon, mesoscale heat conduction simulations with inputs from atomistic simulations and experiments were conducted to study the thermal conductivities of a small-grain high burnup microstructure and two large-grain unrestructured microstructures. We concluded that the phonon scattering effects caused by small point defects such as dispersed Xe atoms in the grain interior must be included in order tomore » correctly predict the thermal transport properties of these microstructures. In extreme cases, even a small concentration of dispersed Xe atoms such as 10 -5 can result in a lower thermal conductivity in the large-grain unrestructured microstructures than in the small-grain high burnup structure. The high-density grain boundaries in a high burnup structure act as defect sinks and can reduce the concentration of point defects in its grain interior and improve its thermal conductivity in comparison with its large-grain counterparts. Furthermore, an analytical model was developed to describe the thermal conductivity at different concentrations of dispersed Xe, bubble porosities, and grain sizes. Upon calibration, the model is robust and agrees well with independent heat conduction modeling over a wide range of microstructural parameters.« less

Effect of Aluminum on the Microstructure and Properties of Two Refractory High-Entropy Alloys (Postprint)

DTIC Science & Technology

2014-04-01

The chemical compositions of the recrystallized ic release; distribution unlimited. Fig. 5. (a) Equiaxed grain structure of the annealed...deformation bands crossing a grain boundary; (c) fine recrystallized grains formed at grain boundaries; (d) a higher magnification image shows the...presence of nano-precipitates at the boundaries of the recrystallized grains. 220 O.N. Senkov et al. / Acta Materialia 68 (2014) 214–228and non

Comparison of microstructure of superplastically deformed synthetic materials and ultramylonite: Coalescence of secondary mineral grains via grain boundary sliding

NASA Astrophysics Data System (ADS)

Hiraga, T.; Miyazaki, T.; Tasaka, M.; Yoshida, H.

2011-12-01

Using very fine-grained aggregates of forsterite containing ~10vol% secondary mineral phase such as periclase and enstatite, we have been able to demonstrate their superplascity, that is, achievement of more than a few 100 % tensile strain (Hiraga et al. 2010). Superplastic deformation is commonly considered to proceed via grain boundary sliding (GBS) which results in grain switching in the samples. Hiraga et al. (2010) succeeded in detecting the operation of GBS from observing the coalescence of grains of secondary phase in superplastically deformed samples. The secondary phase pins the motion of grain boundaries of the primary phase; however, the reduction of the number of the grains of secondary phase due to their coalescence allows grain growth of the primary phase. We analyzed the relationships between grain size of the primary and secondary phases, between strain and grain size, and between strain and the number of coalesced grains in the superplastically deformed samples. The results supports participation of all the grains of the primary phase in grain switching process indicating that the grain boundary sliding accommodates almost entire strain during the deformation. Mechanical properties of these materials such as their stress and grain size exponents of 1-2 do not conflict this conclusion. We applied the relationships obtained from analyzing superplastic materials to the microstructure of the natural samples, which has been considered to have deformed via grain boundary sliding, that is, ultramylonite. The microstructure of greenschist-grade ultramylonite reported by Fliervoet et al. (1997) was analyzed. Distributions of the mineral phases (i.e., quartz, plagioclase, K-feldspar and biotite) show distinct coalescence of the same mineral phases in the direction almost perpendicular to the foliation of the rock. The number of coalesced grains indicates that the strain that rock experienced is > 2. [reference] Hiraga et al. (2010) Nature 468, 1091-1094; Fliervoet et al. (1997) Journal of Structural Geology 19, 1495-1520

Texture enhancement during grain growth of magnesium alloy AZ31B

DOE PAGES

Bhattacharyya, Jishnu J.; Agnew, S. R.; Muralidharan, G.

2015-01-03

In this paper, the microstructure and texture evolution during annealing of rolled Mg alloy AZ31B, at temperatures ranging from 260 to 450°C, is characterized, and a grain growth exponent of n=5, indicating inhibition of grain growth, is observed. Broadening of the normalized grain size distributions, which indicates abnormal grain growth, was observed at all temperatures investigated. It is shown, using a Zener-type analysis for pinning of grain boundaries by particles, that impurity-based particles are responsible for grain growth inhibition and abnormal grain growth. The strong basal texture which develops during rolling of the Mg alloy, resulting in an initial peakmore » intensity in the (0002) pole figure of nine multiples of a random distribution (MRD), increases to ~15 MRD during annealing at 400 and 450°C. Furthermore, a specific texture component {0001}(1120) is observed in the orientation distribution, which increases from 10 to 23 MRD at 400°C. It is hypothesized that the anisotropic grain boundary properties (i.e. low angle boundaries have low energy and mobility) are responsible for the texture strengthening. Additionally, electron backscattered diffraction reveals the recrystallized microstructure to contain a significant number of boundaries with ~30° misorientation about the <0001> direction, and this boundary type persists throughout most annealing treatments explored.« less

Determination of grain boundary mobility during recrystallization by statistical evaluation of electron backscatter diffraction measurements

DOE Office of Scientific and Technical Information (OSTI.GOV)

Basu, I., E-mail: basu@imm.rwth-aachen.de; Chen, M.; Loeck, M.

One of the key aspects influencing microstructural design pathways in metallic systems is grain boundary motion. The present work introduces a method by means of which direct measurement of grain boundary mobility vs. misorientation dependence is made possible. The technique utilizes datasets acquired by means of serial electron backscatter diffraction (EBSD) measurements. The experimental EBSD measurements are collectively analyzed, whereby datasets were used to obtain grain boundary mobility and grain aspect ratio with respect to grain boundary misorientation. The proposed method is further validated using cellular automata (CA) simulations. Single crystal aluminium was cold rolled and scratched in order tomore » nucleate random orientations. Subsequent annealing at 300 °C resulted in grains growing, in the direction normal to the scratch, into a single deformed orientation. Growth selection was observed, wherein the boundaries with misorientations close to Σ7 CSL orientation relationship (38° 〈111〉) migrated considerably faster. The obtained boundary mobility distribution exhibited a non-monotonic behavior with a maximum corresponding to misorientation of 38° ± 2° about 〈111〉 axes ± 4°, which was 10–100 times higher than the mobility values of random high angle boundaries. Correlation with the grain aspect ratio values indicated a strong growth anisotropy displayed by the fast growing grains. The observations have been discussed in terms of the influence of grain boundary character on grain boundary motion during recrystallization. - Highlights: • Statistical microstructure method to measure grain boundary mobility during recrystallization • Method implementation independent of material or crystal structure • Mobility of the Σ7 boundaries in 5N Al was calculated as 4.7 × 10{sup –8} m{sup 4}/J ⋅ s. • Pronounced growth selection in the recrystallizing nuclei in Al • Boundary mobility values during recrystallization 2–3 orders of magnitude larger vis-à-vis curvature driven motion.« less

Microstructural evolution of AZ31 magnesium alloy subjected to sliding friction treatment

NASA Astrophysics Data System (ADS)

Zhang, Wei; Lu, Jinwen; Huo, Wangtu; Zhang, Yusheng; Wei, Q.

2018-06-01

Microstructural evolution and grain refinement mechanism in AZ31 magnesium alloy subjected to sliding friction treatment were investigated by means of transmission electron microscopy. The process of grain refinement was found to involve the following stages: (I) coarse grains were divided into fine twin plates through mechanical twinning; then the twin plates were transformed to lamellae with the accumulation of residual dislocations at the twin boundaries; (II) the lamellae were separated into subgrains with increasing grain boundary misorientation and evolution of high angle boundaries into random boundaries by continuous dynamic recrystallisation (cDRX); (III) the formation of nanograins. The mechanisms for the final stage, the formation of nanograins, can be classified into three types: (i) cDRX; (ii) discontinuous dynamic recrystallisation (dDRX); (iii) a combined mechanism of prior shear-band and subsequent dDRX. Stored strain energy plays an important role in determining deformation mechanisms during plastic deformation.

Effects of thermal aging on the microstructure of Type-II boundaries in dissimilar metal weld joints

NASA Astrophysics Data System (ADS)

Yoo, Seung Chang; Choi, Kyoung Joon; Bahn, Chi Bum; Kim, Si Hoon; Kim, Ju Young; Kim, Ji Hyun

2015-04-01

In order to investigate the effects of long-term thermal aging on the microstructural evolution of Type-II boundary regions in the weld metal of Alloy 152, a representative dissimilar metal weld was fabricated from Alloy 690, Alloy 152, and A533 Gr.B. This mock-up was thermally aged at 450 °C to accelerate the effects of thermal aging in a nuclear power plant operation condition (320 °C). The microstructure of the Type-II boundary region of the weld root, which is parallel to and within 100 μm of the fusion boundary and known to be more susceptible to material degradation, was then characterized after different aging times using a scanning electron microscope equipped with an energy dispersive X-ray spectroscope for micro-compositional analysis, electron backscattered diffraction detector for grain and grain boundary orientation analysis, and a nanoindenter for measurement of mechanical properties. Through this, it was found that a steep compositional gradient and high grain average misorientation is created in the narrow zone between the Type-II and fusion boundaries, while the concentration of chromium and number of low-angle grain boundaries increases with aging time. A high average hardness was also observed in the same region of the dissimilar metal welds, with hardness peaking with thermal aging simulating an operational time of 15 years.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liang, Linyun; Mei, Zhi-Gang; Yacout, Abdellatif M.

We have developed a mesoscale phase-field model for studying the effect of recrystallization on the gas-bubble-driven swelling in irradiated U-Mo alloy fuel. The model can simulate the microstructural evolution of the intergranular gas bubbles on the grain boundaries as well as the recrystallization process. Our simulation results show that the intergranular gas-bubble-induced fuel swelling exhibits two stages: slow swelling kinetics before recrystallization and rapid swelling kinetics with recrystallization. We observe that the recrystallization can significantly expedite the formation and growth of gas bubbles at high fission densities. The reason is that the recrystallization process increases the nucleation probability of gasmore » bubbles and reduces the diffusion time of fission gases from grain interior to grain boundaries by increasing the grain boundary area and decreasing the diffusion distance. The simulated gas bubble shape, size distribution, and density on the grain boundaries are consistent with experimental measurements. We investigate the effect of the recrystallization on the gas-bubble-driven fuel swelling in UMo through varying the initial grain size and grain aspect ratio. We conclude that the initial microstructure of fuel, such as grain size and grain aspect ratio, can be used to effectively control the recrystallization and therefore reduce the swelling in U-Mo fuel.« less

Defects-tolerant Co-Cr-Mo dental alloys prepared by selective laser melting.

PubMed

Qian, B; Saeidi, K; Kvetková, L; Lofaj, F; Xiao, C; Shen, Z

2015-12-01

CrCoMo alloy specimens were successfully fabricated using selective laser melting (SLM). The aim of this study was to carefully investigate microstructure of the SLM specimens in order to understand the influence of their structural features inter-grown on different length scales ranging from nano- to macro-levels on their mechanical properties. Two different sets of processing parameters developed for building the inner part (core) and the surface (skin) of dental prostheses were tested. Microstructures were characterized by SEM, EBSD and XRD analysis. The elemental distribution was assessed by EDS line profile analysis under TEM. The mechanical properties of the specimens were measured. The microstructures of both specimens were characterized showing formation of grains comprised of columnar sub-grains with Mo-enrichment at the sub-grain boundaries. Clusters of columnar sub-grains grew coherently along one common crystallographic direction forming much larger single crystal grains which are intercrossing in different directions forming an overall dendrite-like microstructure. Three types of microstructural defects were occasionally observed; small voids (<10 μm), fine cracks at grain boundaries (<10 μm) and cracks at weld line boundaries (>10 μm). Despite the presence of these defects, the yield and the ultimate tensile strength (UTS) were 870 and 430MPa and 1300MPa and 1160MPa, respectively, for the skin and core specimens which are higher than casted dental alloy. Although the formation of microstructural defects is hard to be avoided during the SLM process, the SLM CoCrMo alloys can achieve improved mechanical properties than their casted counterparts, implying they are "defect-tolerant". Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effect of surface microstructure on electrochemical performance of garnet solid electrolytes.

PubMed

Cheng, Lei; Chen, Wei; Kunz, Martin; Persson, Kristin; Tamura, Nobumichi; Chen, Guoying; Doeff, Marca

2015-01-28

Cubic garnet phases based on Al-substituted Li7La3Zr2O12 (LLZO) have high ionic conductivities and exhibit good stability versus metallic lithium, making them of particular interest for use in next-generation rechargeable battery systems. However, high interfacial impedances have precluded their successful utilization in such devices until the present. Careful engineering of the surface microstructure, especially the grain boundaries, is critical to achieving low interfacial resistances and enabling long-term stable cycling with lithium metal. This study presents the fabrication of LLZO heterostructured solid electrolytes, which allowed direct correlation of surface microstructure with the electrochemical characteristics of the interface. Grain orientations and grain boundary distributions of samples with differing microstructures were mapped using high-resolution synchrotron polychromatic X-ray Laue microdiffraction. The electrochemical characteristics are strongly dependent upon surface microstructure, with small grained samples exhibiting much lower interfacial resistances and better cycling behavior than those with larger grain sizes. Low area specific resistances of 37 Ω cm(2) were achieved; low enough to ensure stable cycling with minimal polarization losses, thus removing a significant obstacle toward practical implementation of solid electrolytes in high energy density batteries.

Stress dependence of microstructures in experimentally deformed calcite

NASA Astrophysics Data System (ADS)

Platt, John P.; De Bresser, J. H. P.

2017-12-01

Optical measurements of microstructural features in experimentally deformed Carrara marble help define their dependence on stress. These features include dynamically recrystallized grain size (Dr), subgrain size (Sg), minimum bulge size (Lρ), and the maximum scale length for surface-energy driven grain-boundary migration (Lγ). Taken together with previously published data Dr defines a paleopiezometer over the range 15-291 MPa and temperature over the range 500-1000 °C, with a stress exponent of -1.09 (CI -1.27 to -0.95), showing no detectable dependence on temperature. Sg and Dr measured in the same samples are closely similar in size, suggesting that the new grains did not grow significantly after nucleation. Lρ and Lγ measured on each sample define a relationship to stress with an exponent of approximately -1.6, which helps define the boundary between a region of dominant strain-energy-driven grain-boundary migration at high stress, from a region of dominant surface-energy-driven grain-boundary migration at low stress.

Microstructural Response of Directionally Solidified René 80 Superalloy to Gas-Tungsten Arc Welding

NASA Astrophysics Data System (ADS)

Sidhu, R. K.; Ojo, O. A.; Chaturvedi, M. C.

2009-01-01

The microstructural response of directionally solidified René 80 (DS René 80) superalloy to gas-tungsten-arc (GTA) welding was investigated. Rapid heating during welding resulted in a significant grain-boundary liquation of solid-state reaction product γ' precipitates, intergranular elemental segregation induced M5B3 borides, and secondary solidification constituents MC carbides and sulfocarbides, which were all present in the preweld heat-treated alloy. Liquation of these particles embrittled the grain boundaries in the heat-affected zone (HAZ) and caused microfissuring along the liquated grain boundaries. Nevertheless, contrary to the generally observed increase in HAZ cracking in superalloys with an increase in Ti and Al concentration, due to increase in the alloy’s hardness, significantly reduced cracking was observed in DS René 80 compared to the conventionally cast IN738 welded under the same conditions, despite its hardness being higher than that of IN738. This was related to the nature of base-metal grain- boundary intersections at the fusion-zone boundary in these materials.

3D Microstructural Characterization of Uranium Oxide as a Surrogate Nuclear Fuel: Effect of Oxygen Stoichiometry on Grain Boundary Distributions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rudman, K.; Dickerson, P.; Byler, Darrin David

The initial microstructure of an oxide fuel can play a key role in its performance. At low burn-ups, the diffusion of fission products can depend strongly on grain size and grain boundary (GB) characteristics, which in turn depend on processing conditions and oxygen stoichiometry. Serial sectioning techniques using Focused Ion Beam were developed to obtain Electron Backscatter Diffraction (EBSD) data for depleted UO2 pellets that were processed to obtain 3 different oxygen stoichiometries. The EBSD data were used to create 3D microstructure reconstructions and to gather statistical information on the grain and GB crystallography, with emphasis on identifying the charactermore » (twist, tilt, mixed) for GBs that meet the Coincident Site Lattice (CSL) criterion as well as GBs with the most common misorientation angles. Data on dihedral angles at triple points were also collected. The results were compared across different samples to understand effects of oxygen content on microstructure evolution.« less

Microstructural evolution during thermal annealing of ice-Ih

NASA Astrophysics Data System (ADS)

Hidas, Károly; Tommasi, Andréa; Mainprice, David; Chauve, Thomas; Barou, Fabrice; Montagnat, Maurine

2017-06-01

We studied the evolution of the microstructure of ice-Ih during static recrystallization by stepwise annealing experiments. We alternated thermal annealing and electron backscatter diffraction (EBSD) analyses on polycrystalline columnar ice pre-deformed in uniaxial compression at temperature of -7 °C to macroscopic strains of 3.0-5.2. Annealing experiments were carried out at -5 °C and -2 °C up to a maximum of 3.25 days, typically in 5-6 steps. EBSD crystal orientation maps obtained after each annealing step permit the description of microstructural changes. Decrease in average intragranular misorientation at the sample scale and modification of the misorientation across subgrain boundaries provide evidence for recovery from the earliest stages of annealing. This initial evolution is similar for all studied samples irrespective of their initial strain or annealing temperature. After an incubation period ≥1.5 h, recovery is accompanied by recrystallization (nucleation and grain boundary migration). Grain growth proceeds at the expense of domains with high intragranular misorientations, consuming first the most misorientated parts of primary grains. Grain growth kinetics fits the parabolic growth law with grain growth exponents in the range of 2.4-4.0. Deformation-induced tilt boundaries and kink bands may slow down grain boundary migration. They are stable features during early stages of static recrystallization, only erased by normal growth, which starts after >24 h of annealing.

Meso-scale anisotropic hydrogen segregation near grain-boundaries in polycrystalline nickel characterized by EBSD/SIMS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oudriss, A.; Le Guernic, Solenne; Wang, Zhaoying

2016-02-15

To study anisotropic hydrogen segregation and diffusion in nickel polycrystalline, Secondary Ion Mass Spectrometry (SIMS) and Electron Back Scattered Diffraction (EBSD) are integrated to investigate hydrogen distribution around grain boundaries. Hydrogen distribution in pre-charged samples were correlated with grain boundary character by integrating high-resolution grain microstructure from EBSD inverse pole figure map and low-resolution hydrogen concentration profile map from SIMS. This multimodal imaging instrumentation shows that grain boundaries in nickel can be categorized into two families based on behavior of hydrogen distribution crossing grain boundary: the first one includes random grain boundaries with fast hydrogen diffusivity, showing a sharp gapmore » for hydrogen concentration profile cross the grain boundaries. The second family are special Σ3n grain boundaries with low hydrogen diffusivity, showing a smooth gradient of hydrogen concentration cross the grain boundary. Heterogeneous hydrogen distributions due to grain boundary family revealed by SIMS/EBSD on mesoscale further validate the recent hydrogen permeation data and anisotropic ab-initio calculations in nanoscale. The results highlight the fact that grain boundaries character impacts hydrogen distribution significantly.« less

An electron back-scattered diffraction study on the microstructure evolution of severely deformed aluminum AI6061 alloy

NASA Astrophysics Data System (ADS)

Vaseghi, M.; Karimi Taheri, A.; Kim, H. S.

2014-08-01

In this paper dynamic strain ageing behavior in an Al-Mg-Si alloy related to equal channel angular pressing (ECAP) was investigated. In order to examine the combined plastic deformation and ageing effects on microstructure evolutions and strengthening characteristics, the Al6061 alloy were subjected to phi=90° ECAP die for up to 4 passes via route Bc at high temperatures. For investigating the effects of ageing temperature and strain rate in ECAP, Vickers hardness tests were performed. The combination of the ECAP process with dynamic ageing at higher temperatures resulted in a significant increase in hardness. The microstructural evolution of the samples was studied using electron back-scattering diffraction (EBSD). The grains of Al6061 aluminum alloy were refined significantly at 100 and 150 °C with greater pass numbers and the distributions of grain size tended to be more uniform with pass number increasing. Frequency of sub-boundaries and low angle grain boundaries (LAGBs) increased at initial stage of deformation, and sub-boundaries and LAGBs evolved into highangle grain boundaries (HAGBs) with further deformation, which resulted in the high frequency of HAGBs in the alloy after ECAP 4 passes.

Investigation of Microstructure and Mechanical Properties of ECAP-Processed AM Series Magnesium Alloy

NASA Astrophysics Data System (ADS)

Gopi, K. R.; Nayaka, H. Shivananda; Sahu, Sandeep

2016-09-01

Magnesium alloy Mg-Al-Mn (AM70) was processed by equal channel angular pressing (ECAP) at 275 °C for up to 4 passes in order to produce ultrafine-grained microstructure and improve its mechanical properties. ECAP-processed samples were characterized for microstructural analysis using optical microscopy, scanning electron microscopy, and transmission electron microscopy. Microstructural analysis showed that, with an increase in the number of ECAP passes, grains refined and grain size reduced from an average of 45 to 1 µm. Electron backscatter diffraction analysis showed the transition from low angle grain boundaries to high angle grain boundaries in ECAP 4 pass sample as compared to as-cast sample. The strength and hardness values an showed increasing trend for the initial 2 passes of ECAP processing and then started decreasing with further increase in the number of ECAP passes, even though the grain size continued to decrease in all the successive ECAP passes. However, the strength and hardness values still remained quite high when compared to the initial condition. This behavior was found to be correlated with texture modification in the material as a result of ECAP processing.

New atom probe approaches to studying segregation in nanocrystalline materials.

PubMed

Samudrala, S K; Felfer, P J; Araullo-Peters, V J; Cao, Y; Liao, X Z; Cairney, J M

2013-09-01

Atom probe is a technique that is highly suited to the study of nanocrystalline materials. It can provide accurate atomic-scale information about the composition of grain boundaries in three dimensions. In this paper we have analysed the microstructure of a nanocrystalline super-duplex stainless steel prepared by high pressure torsion (HPT). Not all of the grain boundaries in this alloy display obvious segregation, making visualisation of the microstructure challenging. In addition, the grain boundaries present in the atom probe data acquired from this alloy have complex shapes that are curved at the scale of the dataset and the interfacial excess varies considerably over the boundaries, making the accurate characterisation of the distribution of solute challenging using existing analysis techniques. In this paper we present two new data treatment methods that allow the visualisation of boundaries with little or no segregation, the delineation of boundaries for further analysis and the quantitative analysis of Gibbsian interfacial excess at boundaries, including the capability of excess mapping. Copyright © 2013 Elsevier B.V. All rights reserved.

Application of Electron Backscatter Diffraction to evaluate the ASR risk of concrete aggregates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rößler, C., E-mail: christiane.roessler@uni-weimar.de; Möser, B.; Giebson, C.

Alkali-Silica Reaction (ASR) is a frequent cause of reduced concrete durability. Eliminating the application of alkali reactive aggregates would reduce the quantity of ASR concrete deterioration in the field. This study introduces an Electron Backscatter Diffraction (EBSD) technique to distinguish the ASR risk of slow-late reacting aggregates by measuring microstructural properties of quartz. Quantifying the amount of quartz grain boundaries and the associated misorientation of grains can thereby be used to differentiate microstructures bearing an ASR risk. It is also shown that dissolution of quartz in high pH environments occurs along quartz grain and subgrain boundaries. Results of EBSD analysismore » are compared with ASR performance testing on concrete prisms and optical light microscopy characterization of quartz microstructure. EBSD opens new possibilities to quantitatively characterize microstructure of quartz in concrete aggregates with respect to ASR. This leads to a better understanding on the actual cause of ASR.« less

The role of boundary variability in polycrystalline grain-boundary diffusion

NASA Astrophysics Data System (ADS)

Moghadam, M. M.; Rickman, J. M.; Harmer, M. P.; Chan, H. M.

2015-01-01

We investigate the impact of grain-boundary variability on mass transport in a polycrystal. More specifically, we perform both numerical and analytical studies of steady-state diffusion in prototypical microstructures in which there is either a discrete spectrum of grain-boundary activation energies or else a complex distribution of grain-boundary character, and hence a continuous spectrum of boundary activation energies. An effective diffusivity is calculated for these structures using simplified multi-state models and, for the case of a continuous spectrum, employing experimentally obtained grain-boundary energy data. We identify different diffusive regimes for these cases and quantify deviations from Arrhenius behavior using effective medium theory. Finally, we examine the diffusion kinetics of a simplified model of an interfacial layering (i.e., complexion) transition.

Effect of prior deformation on microstructural development and Laves phase precipitation in high-chromium stainless steel.

PubMed

Hsiao, Z-W; Chen, D; Kuo, J-C; Lin, D-Y

2017-04-01

This study investigated the influence of deformation on precipitation behaviour and microstructure change during annealing. Here, the prior deformation of high-chromium stainless steel was tensile deformation of 3%, 6% and 10%, and the specimens were then annealed at 700˚C for 10 h. The specimens were subsequently analyzed using backscattered electron image and electron backscattering diffraction measurements with SEM. Compared with the deformation microstructure, the grains revealed no preferred orientation. The precipitates of TiN and NbC were formed homogenously in the grain interior and at grain boundaries after annealing. Fine Laves phase precipitates were observed in grains and along subgrain boundaries as the deformation increased. Furthermore, the volume fraction of Laves phase increased, but the average particle diameter of precipitate was reduced as the deformation increased. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

Microstructural and hardness investigations on a dissimilar metal weld between low alloy steel and Alloy 82 weld metal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Z.R., E-mail: raymix@aliyun.com

The investigation on microstructure and hardness at the fusion boundary (FB) region of a dissimilar metal weld (DMW) between low alloy steel (LAS) A508-III and Alloy 82 weld metal (WM) was carried out. The results indicated that there were two kinds of FBs, martensite FB and sharp FB, with obvious different microstructures, alternately distributed in the same FB. The martensite FB region had a gradual change of elemental concentration across FB, columnar WM grains with high length/width ratios, a thick martensite layer and a wide heat affected zone (HAZ) with large prior austenite grains. By comparison, the sharp FB regionmore » had a relatively sharp change of elemental concentration across the FB, WM grains with low length/width ratios and a narrow HAZ with smaller prior austenite grains. The martensite possessed a K-S orientation relationship with WM grains, while no orientation relationship was found between the HAZ grains and WM grains at the sharp FB. Compared with sharp FB there were much more Σ3 boundaries in the HAZ beside martensite FB. The hardness maximum of the martensite FB was much higher than that of the sharp FB, which was attributed to the martensite layer at the martensite FB. - Highlights: •Martensite and sharp FBs with different microstructures were found in the same FB. •There were high length/width-ratio WM grains and a wide HAZ beside martensite FB. •There were low length/width-ratio WM grains and a narrow HAZ beside sharp FB. •Compared with sharp FB, there were much more Σ3 boundaries in HAZ of martensite FB. •Hardness maximium of martensite FB was much higher than that of sharp FB.« less

Grain-Boundary Roughening in Colloidal Crystals

NASA Astrophysics Data System (ADS)

Liao, Maijia; Xiao, Xiao; Chui, Siu Tat; Han, Yilong

2018-04-01

In polycrystals, faceted grains may become round and rough at high temperatures. Such a roughening phenomenon remains poorly understood, partly because of the lack of experimental observations. Here, we directly visualize the roughening dynamics of grain boundaries inside thin-film colloidal crystals at the single-particle level using video microscopy. The thermal fluctuations of grain boundaries appear to exhibit both static and dynamic critical-like behaviors, in contrast to the Kosterlitz-Thouless transition in typical free surface roughening. The roughening point shifts towards the melting point as the grain boundary's mismatch angle θ decreases and is preempted by melting when θ <18 ° . Counterintuitively, the amplitude of grain-boundary fluctuations decreases above the roughening point. This could be attributed to the observed widening of the grain boundary. The roughening strongly affects the mobility of the grain boundary but not the stiffness. These results provide new guidance for the control of microstructures in polycrystals and further development of roughening theory.

Influence of Homogenization on Microstructural Response and Mechanical Property of Al-Cu-Mn Alloy.

PubMed

Wang, Jian; Lu, Yalin; Zhou, Dongshuai; Sun, Lingyan; Li, Renxing; Xu, Wenting

2018-05-29

The evolution of the microstructures and properties of large direct chill (DC)-cast Al-Cu-Mn alloy ingots during homogenization was investigated. The results revealed that the Al-Cu-Mn alloy ingots had severe microsegregation and the main secondary phase was Al₂Cu, with minimal Al₇Cu₂Fe phase. Numerous primary eutectic phases existed in the grain boundary and the main elements were segregated at the interfaces along the interdendritic region. The grain boundaries became discontinuous, residual phases were effectively dissolved into the matrix, and the segregation degree of all elements was reduced dramatically during homogenization. In addition, the homogenized alloys exhibited improved microstructures with finer grain size, higher number density of dislocation networks, higher density of uniformly distributed θ' or θ phase (Al₂Cu), and higher volume fraction of high-angle grain boundaries compared to the nonhomogenized samples. After the optimal homogenization scheme treated at 535 °C for 10 h, the tensile strength and elongation% were about 24 MPa, 20.5 MPa, and 1.3% higher than those of the specimen without homogenization treatment.

The Microstructural Evolution and Special Flow Behavior of Ti-5Al-2Sn-2Zr-4Mo-4Cr During Isothermal Compression at a Low Strain Rate

NASA Astrophysics Data System (ADS)

Sun, J. Z.; Li, M. Q.; Li, H.

2017-09-01

The microstructural evolution and special flow behavior of Ti-5Al-2Sn-2Zr-4Mo-4Cr during isothermal compression at a strain rate of 0.0001 s-1 were investigated. The dislocation climbs in elongated α grains resulted in the formation of low-angle boundaries that transform into high-angle boundaries with greater deformation, and the elongated α grains subsequently separated into homogenous globular α grains with the penetration of the β phase. The simultaneous occurrence of discontinuous dynamic recrystallization and continuous dynamic recrystallization in the primary β grains resulted in a trimode grain distribution. The β grains surrounded by dislocations presented an equilateral-hexagonal morphology, which suggests that grain boundary sliding through dislocation climbs was the main deformation mechanism. The true stress-strain curves for 1073 and 1113 K abnormally intersect at a strain of 0.35, related to the α → β phase transformation and distinct growth of the β grain size.

Microstructure characterisation of Ti-6Al-4V from different additive manufacturing processes

NASA Astrophysics Data System (ADS)

Neikter, M.; Åkerfeldt, P.; Pederson, R.; Antti, M.-L.

2017-10-01

The focus of this work has been microstructure characterisation of Ti-6Al-4V manufactured by five different additive manufacturing (AM) processes. The microstructure features being characterised are the prior β size, grain boundary α and α lath thickness. It was found that material manufactured with powder bed fusion processes has smaller prior β grains than the material from directed energy deposition processes. The AM processes with fast cooling rate render in thinner α laths and also thinner, and in some cases discontinuous, grain boundary α. Furthermore, it has been observed that material manufactured with the directed energy deposition processes has parallel bands, except for one condition when the parameters were changed, while the powder bed fusion processes do not have any parallel bands.

Microstructure evolution in the fusion zone of laser-welded Mg–Gd–Y–Zr alloy during solution and aging treatment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Lyuyuan

The microstructure evolution in the fusion zone of laser-welded Mg-Gd-Y-Zr alloy during solution and aging treatment is investigated. The morphology of the Mg{sub 24}(Gd,Y){sub 5} in the divorced eutectic at the grain boundary transforms from a continuous network to disconnected and fragmentized islands and then to spheroidal particles before complete dissolution during the solution treatment at 430 °C. During the subsequent aging treatment at 225 °C, the precipitation sequence in the fusion zone follows the order of supersaturated solid solution (SSSS) → βʺ(D0{sub 19}) → βʹ(cbco) → β{sub 1}(fcc) → β(fcc). High-density precipitates are present at the original grain boundariesmore » of the fusion zone from the welded structure but there are less precipitates in the interior of the original grains. The grain growth during the solution treatment at 430 °C comprises the slowly increasing stage, rapidly increasing stage, and stable stage. The network-distributed Mg{sub 24}(Gd,Y){sub 5} impedes migration of the grain boundaries, restricts grain growth in the first slowly increasing stage, and segregation of zirconium near the grain boundaries also affects migration of the grain boundaries. - Highlights: •Different quantities of precipitates are present at different location of grain. •The network-distributed Mg{sub 24}(Gd,Y){sub 5} restricts grain growth. •Segregation of Zr affects migration of grain boundaries.« less

Evidence for stable grain boundary melt films in experimentally deformed olivine-orthopyroxene rocks

NASA Astrophysics Data System (ADS)

de Kloe, R.; Drury, M. R.; van Roermund, H. L. M.

The microstructure of olivine-olivine grain boundaries has been studied in experimentally deformed (1200-1227°C, 300MPa) partially molten olivine and olivine-orthopyroxene rocks. In-situ melting produced 1vol% melt in all samples studied. Grain boundary analyses were carried out using a number of transmission electron microscopy techniques. The grain boundary chemistry in undeformed olivine-orthopyroxene starting material showed evidence for the presence of an intergranular phase along some, but not all, of the olivine-olivine boundaries. In the deformed samples, ultrathin Si-rich, Al- and Ca-bearing amorphous films have been observed along all investigated olivine-olivine grain boundaries. The chemistry of the grain boundaries, which is considered to be indicative for the presence of a thin film, was measured with energy-dispersive X-ray spectroscopy (EDX) and energy-filtering imaging. The amorphous nature of the films was confirmed with diffuse dark field imaging, Fresnel fringe imaging, and high-resolution electron microscopy. The films range in thickness from 0.6 to 3.0nm, and EDX analyses show that the presence of Al and Ca is restricted to this ultrathin film along the grain boundaries. Because thin melt films have been observed in all the samples, they are thought to be stable features of the melt microstructure in deformed partially molten rocks. The transition from the occasional presence of films in the undeformed starting material to the general occurrence of the films in deformed materials suggests that deformation promotes the formation and distribution of the films. Alternatively, hot-pressing may be too short for films to develop along all grain boundaries. A difference in creep strength between the studied samples could not be attributed to grain boundary melt films, as these have been found in all deformed samples. However, a weakening effect of grain boundary melt films on olivine rheology could not be ruled out due to the lack of confirmed melt-film free experiments.

Effect of retrogression duration on the grain boundary microstructure and microchemistry of AA7010

NASA Astrophysics Data System (ADS)

Nandana, M. S.; Bhat, K. Udaya; Manjunatha, C. M.

2018-04-01

The paper presents the microstructural characterization of the aluminium alloy 7010 in retrogression and re- ageing (RRA) condition by using Transmission Electron Microscope (TEM). The grain boundary microstructure is analyzed with the focus on variation of GBP's (grain boundary precipitate) size and PFZ (precipitate free zone) size during retrogression performed at 200 °C for duration of 10-60 min. The microchemistry of the GBP's is analyzed by using TEM-EDS (Energy Dispersive X-ray spectroscopy). The results reveal the coarsening of discrete GBP's along with enrichment of the Cu in them. The average size of the GBP's in RRA treated sample vary from 30 nm during 10 min of retrogression to 59 nm at 60 min of retrogression. The PFZ size varied from 35 nm to 51 nm for 10 min and 60 min of retrogression time, respectively. The Cu content of the GBP's increased from 3.54 wt% for 10 min of retrogression to 5.27 wt% for 60 min of retrogression and re-aged sample.

Effect of Interface Structure on the Microstructural Evolution of Ceramics

DTIC Science & Technology

2007-11-06

because almost all the material properties are de - pendent upon their internal microstructures. Therefore, the microstructural evolution during the...growing interface de - pends upon the density of kinks on that interface. It fol- lows that the atomically smooth interface, which is char- acterized by...grain, and its de - tailed coarsening process has been treated elsewhere.139 During liquid-phase sintering, the formation of grain boundaries between

Linking Initial Microstructure to ORR Related Property Degradation in SOFC Cathode: A Phase Field Simulation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lei, Y.; Cheng, T. -L.; Wen, Y. H.

Microstructure evolution driven by thermal coarsening is an important factor for the loss of oxygen reduction reaction rates in SOFC cathode. In this work, the effect of an initial microstructure on the microstructure evolution in SOFC cathode is investigated using a recently developed phase field model. Specifically, we tune the phase fraction, the average grain size, the standard deviation of the grain size and the grain shape in the initial microstructure, and explore their effect on the evolution of the grain size, the density of triple phase boundary, the specific surface area and the effective conductivity in LSM-YSZ cathodes. Itmore » is found that the degradation rate of TPB density and SSA of LSM is lower with less LSM phase fraction (with constant porosity assumed) and greater average grain size, while the degradation rate of effective conductivity can also be tuned by adjusting the standard deviation of grain size distribution and grain aspect ratio. The implication of this study on the designing of an optimal initial microstructure of SOFC cathodes is discussed.« less

Linking Initial Microstructure to ORR Related Property Degradation in SOFC Cathode: A Phase Field Simulation

DOE PAGES

Lei, Y.; Cheng, T. -L.; Wen, Y. H.

2017-07-05

Microstructure evolution driven by thermal coarsening is an important factor for the loss of oxygen reduction reaction rates in SOFC cathode. In this work, the effect of an initial microstructure on the microstructure evolution in SOFC cathode is investigated using a recently developed phase field model. Specifically, we tune the phase fraction, the average grain size, the standard deviation of the grain size and the grain shape in the initial microstructure, and explore their effect on the evolution of the grain size, the density of triple phase boundary, the specific surface area and the effective conductivity in LSM-YSZ cathodes. Itmore » is found that the degradation rate of TPB density and SSA of LSM is lower with less LSM phase fraction (with constant porosity assumed) and greater average grain size, while the degradation rate of effective conductivity can also be tuned by adjusting the standard deviation of grain size distribution and grain aspect ratio. The implication of this study on the designing of an optimal initial microstructure of SOFC cathodes is discussed.« less

Electrical transport through individual nanowires with transverse grain boundaries

NASA Astrophysics Data System (ADS)

Xue, X. Y.; Feng, P.; Wang, C.; Chen, Y. J.; Wang, Y. G.; Wang, T. H.

2006-07-01

V2O4•0.25H2O nanowires are synthesized via hydrothermal route. The nanowires are of metastable phase, and transverse grain boundaries are observed in their microstructures. Transport through individual V2O4•0.25H2O nanowires shows nonlinear current-voltage (I-V) characteristics in the bias range of -3to3V. The resistance rapidly decreases from 2.54to0.5MΩ as the bias is raised from 0to1V. Such behaviors can be attributed to the presence of the barrier at the transverse grain boundary. By analyzing the I-V curves at various temperatures, the effective barrier height is estimated to be about 0.13eV. Our results provide important information about how the microstructure mismatch affects the electrical properties.

Transfer function concept for ultrasonic characterization of material microstructures

NASA Technical Reports Server (NTRS)

Vary, A.; Kautz, H. E.

1986-01-01

The approach given depends on treating material microstructures as elastomechanical filters that have analytically definable transfer functions. These transfer functions can be defined in terms of the frequency dependence of the ultrasonic attenuation coefficient. The transfer function concept provides a basis for synthesizing expressions that characterize polycrystalline materials relative to microstructural factors such as mean grain size, grain-size distribution functions, and grain boundary energy transmission. Although the approach is nonrigorous, it leads to a rational basis for combining the previously mentioned diverse and fragmented equations for ultrasonic attenuation coefficients.

A study of the microstructure of a rapidly solidified nickel-base superalloy modified with boron. M.S. Thesis. Final Contractor Report

NASA Technical Reports Server (NTRS)

Speck, J. S.

1986-01-01

The microstructures of melt-spun superalloy ribbons with variable boron levels have been studied by transmission electron microscopy. The base alloy was of approximate composition Ni-11% Cr-5%Mo-5%Al-4%Ti with boron levels of 0.06, 0.12, and 0.60 percent (all by weight). Thirty micron thick ribbons display an equiaxed chill zone near the wheel contact side which develops into primary dendrite arms in the ribbon center. Secondary dendrite arms are observed near the ribbon free surface. In the higher boron bearing alloys, boride precipitates are observed along grain boundaries. A concerted effort has been made to elucidate true grain shapes by the use of bright field/dark field microscopy. In the low boron alloy, grain shapes are often convex, and grain faces are flat. Boundary faces frequently have large curvature, and grain shapes form concave polygons in the higher boron level alloys. It is proposed that just after solidification, in all of the alloys studied, grain shapes were initially concave and boundaries were wavy. Boundary straightening is presumed to occur on cooling in the low boron alloy. Boundary migration is precluded in the higher boron alloys by fast precipitation of borides at internal interfaces.

Dislocation creep accommodated Grain Boundary Sliding: A high strain rate/low temperature deformation mechanism in calcite ultramylonites

NASA Astrophysics Data System (ADS)

Rogowitz, Anna; Grasemann, Bernhard

2014-05-01

Grain boundary sliding (GBS) is an important grain size sensitive deformation mechanism that is often associated with extreme strain localization and superplasticity. Another mechanism has to operate simultaneously to GBS in order to prevent overlaps and voids between sliding grains. One of the most common accommodating mechanisms is diffusional creep but, recently, dislocation creep has been reported to operate simultaneous to GBS. Due to the formation of a flanking structure in nearly pure calcite marble on Syros (Cyclades, Greece) at lower greenschist facies conditions, an extremely fine grained ultramylonite developed. The microstructure of the layer is characterized by (1) calcite grains with an average grain size of 3.6 µm (developed by low temperature/high strain rate grain boundary migration recrystallization, BLG), (2) grain boundary triple junctions with nearly 120° angles and (3) small cavities preferentially located at triple junctions and at grain boundaries in extension. These features suggest that the dominant deformation mechanism was GBS. In order to get more information on the accommodation mechanism detailed microstructural and textural analyses have been performed on a FEI Quanta 3D FEG instrument equipped with an EDAX Digiview IV EBSD camera. The misorientation distribution curves for correlated and uncorrelated grains follow almost perfect the calculated theoretical curve for a random distribution, which is typical for polycrystalline material deformed by GBS. However, the crystallographic preferred orientation indicates that dislocation creep might have operated simultaneously. We also report Zener-Stroh cracks resulting from dislocation pile up, indicating that dislocation movement was active. We, therefore, conclude that the dominant deformation mechanism was dislocation creep accommodated grain boundary sliding. This is consistent with the observed grain size range that plots at the field boundary between grain size insensitive and grain size sensitive creep, in a deformation mechanism map for calcite.

Microstructure-sensitive small fatigue crack growth assessment. Effect of strain ratio multiaxial strain state and geometric discontinuities

DOE Office of Scientific and Technical Information (OSTI.GOV)

Castelluccio, Gustavo M.; McDowell, David L.

Fatigue crack initiation in the high cycle fatigue regime is strongly influenced by microstructural features. Research efforts have usually focused on predicting fatigue resistance against crack incubation without considering the early fatigue crack growth after encountering the first grain boundary. However, a significant fraction of the variability of the total fatigue life can be attributed to growth of small cracks as they encounter the first few grain boundaries, rather than crack formation within the first grain. Our paper builds on the framework previously developed by the authors to assess microstructure-sensitive small fatigue crack formation and early growth under complex loadingmore » conditions. Moreover, the scheme employs finite element simulations that explicitly render grains and crystallographic directions along with simulation of microstructurally small fatigue crack growth from grain to grain. The methodology employs a crystal plasticity algorithm in ABAQUS that was previously calibrated to study fatigue crack initiation in RR1000 Ni-base superalloy. Our work present simulations with non-zero applied mean strains and geometric discontinuities that were not previously considered for calibration. Results exhibit trends similar to those found in experiments for multiple metallic materials, conveying a consistent physical description of fatigue damage phenomena.« less

Microstructure-sensitive small fatigue crack growth assessment. Effect of strain ratio multiaxial strain state and geometric discontinuities

DOE PAGES

Castelluccio, Gustavo M.; McDowell, David L.

2015-09-16

Fatigue crack initiation in the high cycle fatigue regime is strongly influenced by microstructural features. Research efforts have usually focused on predicting fatigue resistance against crack incubation without considering the early fatigue crack growth after encountering the first grain boundary. However, a significant fraction of the variability of the total fatigue life can be attributed to growth of small cracks as they encounter the first few grain boundaries, rather than crack formation within the first grain. Our paper builds on the framework previously developed by the authors to assess microstructure-sensitive small fatigue crack formation and early growth under complex loadingmore » conditions. Moreover, the scheme employs finite element simulations that explicitly render grains and crystallographic directions along with simulation of microstructurally small fatigue crack growth from grain to grain. The methodology employs a crystal plasticity algorithm in ABAQUS that was previously calibrated to study fatigue crack initiation in RR1000 Ni-base superalloy. Our work present simulations with non-zero applied mean strains and geometric discontinuities that were not previously considered for calibration. Results exhibit trends similar to those found in experiments for multiple metallic materials, conveying a consistent physical description of fatigue damage phenomena.« less

Characterization of ultrafine grained Cu-Ni-Si alloys by electron backscatter diffraction

NASA Astrophysics Data System (ADS)

Altenberger, I.; Kuhn, H. A.; Gholami, M.; Mhaede, M.; Wagner, L.

2014-08-01

A combination of rotary swaging and optimized precipitation hardening was applied to generate ultra fine grained (UFG) microstructures in low alloyed high performance Cu-based alloy CuNi3Si1Mg. As a result, ultrafine grained (UFG) microstructures with nanoscopically small Ni2Si-precipitates exhibiting high strength, ductility and electrical conductivity can be obtained. Grain boundary pinning by nano-precipitates enhances the thermal stability. Electron channeling contrast imaging (ECCI) and especially electron backscattering diffraction (EBSD) are predestined to characterize the evolving microstructures due to excellent resolution and vast crystallographic information. The following study summarizes the microstructure after different processing steps and points out the consequences for the most important mechanical and physical properties such as strength, ductility and conductivity.

Microstructure Characterization Of Lead-Free Solders Depending On Alloy Composition

NASA Astrophysics Data System (ADS)

Panchenko, Iuliana; Mueller, Maik; Wolter, Klaus-Juergen

2010-11-01

Fatigue and crack nucleation in solder joints is basically associated with changes in the microstructure. Therefore the microstructure evolution of SnAgCu solder joints during solidification and subsequent application is an important subject for reliability investigations and physics of failure analysis. The scope of this study is a systematic overview of the as-cast microstructures in small sized lead-free SnAgCu solder spheres after solidification. A total of 32 alloy compositions have been investigated with varying Ag content from 0 to 5 wt.% and varying Cu content from 0 to 1.2 wt.%. The solder spheres had a diameter of approx. 270 μm and were all manufactured under the similar conditions. Subsequent cross-sectioning was carried out in order to analyze the microstructure by optical and electron microscopy as well as Electron Backscatter Diffraction and Energy Dispersive X-ray Spectroscopy. The results allow a comprehensive overview of the dependence of the as-cast microstructure on the solder composition. It is shown that strong changes in microstructure can be caused by small changes in solder composition. In addition, a solidification phenomenon known as cyclic twinning has been found in the samples. Three different microstructures related to that phenomenon will be presented and detailed characterizations of these structures are given in this study. These microstructures differ in their appearance by solidification morphology, phase distribution as well as grain structure and can be described as follows: 1. large dentritic areas of different grain orientations which are characterized by approx. 60° twin boundaries; 2. areas of small β-Sn cells with approx. 60° twin relation and larger intermetallic precipitates; 3. large grains consisting of a β-Sn matrix with very fine intermetallic precipitates and high angle grain boundaries between adjacent grains.

Damage Tolerance and Mechanics of Interfaces in Nanostructured Metals

NASA Astrophysics Data System (ADS)

Foley, Daniel J.

The concept of interface driven properties in crystalline metals has been one of the most intensely discussed topics in materials science for decades. Since the 1980s researchers have been exploring the concept of grain boundary engineering as route for tuning properties such as fracture toughness and irradiation resistance. This is especially true in ultra-fine grained and nanocrystalline materials where grain boundary mediated properties become dominant. More recently, materials composed of hierarchical nanostructures, such as amorphous-crystalline nanolaminates, have attracted considerable attention due to their favorable properties, ease of manufacture and highly tunable microstructure. While both grain boundary engineering and hierarchical nanostructures have shown promise there are still questions remaining regarding the role of specific attributes of the microstructure (such as grain boundaries, grain/layer size and inter/intralayer morphology) in determining material properties. This thesis attempts to address these questions by using atomistic simulations to perform deformation and damage loading studies on a series of nanolaminate and bicrystalline structures. During the course of this thesis the roles of layer thickness, interlayer structure and interlayer chemistry on the mechanical properties of Ni-NiX amorphous-crystalline nanolaminates were explored using atomistic simulations. This thesis found that layer thickness/thickness ratio and amorphous layer chemistry play a crucial role in yield strength and Young's modulus. Analysis of the deformation mechanisms at the atomic scale revealed that structures containing single crystalline, crystalline layers undergo plastic deformation when shear transformation zones form in the amorphous layer and impinge on the amorphous-crystalline interface, leading to dislocation emission. However, structures containing nanocrystalline, crystalline layers (both equiaxed and columnar nanocrystalline) undergo plastic deformation through a combination of grain boundary sliding and grain boundary mediated dislocation nucleation. Since grain boundaries were found to play a critical role as sources and sinks for dislocations in amorphous-crystalline nanolaminates a follow-up study on the effect of grain boundary character on damage accumulation/accommodation in copper symmetric tilt grain boundaries was performed. This study found that grain boundaries will become saturated with damage, a state where grain boundary energy and grain boundary free volume oscillate about a plateau during continuous defect loading (vacancy, interstitial and frenkel pair loading were all considered). Further, grain boundary character (specifically equilibrium grain boundary energy) was strongly correlated to the damage accommodation behavior of grain boundaries in copper. Finally, a study that attempted to link grain boundary damage saturation behavior to variations in grain boundary mechanical properties was performed. This study found no direct relationships between grain boundary damage saturation behavior and variations in grain boundary properties. The results of this thesis provide researchers with several strategies for tuning the properties of amorphous-crystalline nanolaminates. These strategies include manipulated bulk attributes such as layer thickness and morphology as well as manipulation of microscale attributes such as grain boundary engineering. Finally, this thesis provides valuable insight into the damage loading/accommodation behavior of FCC symmetric tilt grain boundaries.

Grain dissection as a grain size reducing mechanism during ice microdynamics

NASA Astrophysics Data System (ADS)

Steinbach, Florian; Kuiper, Ernst N.; Eichler, Jan; Bons, Paul D.; Drury, Martin R.; Griera, Albert; Pennock, Gill M.; Weikusat, Ilka

2017-04-01

Ice sheets are valuable paleo-climate archives, but can lose their integrity by ice flow. An understanding of the microdynamic mechanisms controlling the flow of ice is essential when assessing climatic and environmental developments related to ice sheets and glaciers. For instance, the development of a consistent mechanistic grain size law would support larger scale ice flow models. Recent research made significant progress in numerically modelling deformation and recrystallisation mechanisms in the polycrystalline ice and ice-air aggregate (Llorens et al., 2016a,b; Steinbach et al., 2016). The numerical setup assumed grain size reduction is achieved by the progressive transformation of subgrain boundaries into new high angle grain boundaries splitting an existing grain. This mechanism is usually termed polygonisation. Analogue experiments suggested, that strain induced grain boundary migration can cause bulges to migrate through the whole of a grain separating one region of the grain from another (Jessell, 1986; Urai, 1987). This mechanism of grain dissection could provide an alternative grain size reducing mechanism, but has not yet been observed during ice microdynamics. In this contribution, we present results using an updated numerical approach allowing for grain dissection. The approach is based on coupling the full field theory crystal visco-plasticity code (VPFFT) of Lebensohn (2001) to the multi-process modelling platform Elle (Bons et al., 2008). VPFFT predicts the mechanical fields resulting from short strain increments, dynamic recrystallisation process are implemented in Elle. The novel approach includes improvements to allow for grain dissection, which was topologically impossible during earlier simulations. The simulations are supported by microstructural observations from NEEM (North Greenland Eemian Ice Drilling) ice core. Mappings of c-axis orientations using the automatic fabric analyser and full crystallographic orientations using electron backscatter diffraction (EBSD) are presented. Numerical simulations predict and resolve the microstructural evolution over strain and time. The occurrence of processes such as grain dissection can only be proven using such time resolved movies of microstructure evolution. We will present movies that show grain dissection as a common process during the simulations. Microstructures obtained from NEEM ice core support the observations and we provide evidence for grain dissection in natural ice. Grain dissection is observed to be most efficient relative to polygonisation, when the microstructure approaches steady state grain sizes. This is consistent with analogue experiments observing grain dissection by Jessell (1986) and Urai (1987). Our research suggests a novel grain size reducing mechanisms in ice microdynamics that should be considered when developing a consistent grain size law.

Microalloying Ultrafine Grained Al Alloys with Enhanced Ductility

PubMed Central

Jiang, L.; Li, J. K.; Cheng, P. M.; Liu, G.; Wang, R. H.; Chen, B. A.; Zhang, J. Y.; Sun, J.; Yang, M. X.; Yang, G.

2014-01-01

Bulk ultrafine grained (UFG)/nanocrystal metals possess exceptional strength but normally poor ductility and thermal stability, which hinder their practical applications especially in high-temperature environments. Through microalloying strategy that enables the control of grains and precipitations in nanostructured regime, here we design and successfully produce a highly microstructure-stable UFG Al-Cu-Sc alloy with ~275% increment in ductility and simultaneously ~50% enhancement in yield strength compared with its Sc-free counterpart. Although the precipitations in UFG alloys are usually preferentially occurred at grain boundaries even at room temperature, minor Sc addition into the UFG Al-Cu alloys is found to effectively stabilize the as-processed microstructure, strongly suppress the θ-Al2Cu phase precipitation at grain boundary, and remarkably promote the θ′-Al2Cu nanoparticles dispersed in the grain interior in artificial aging. A similar microalloying strategy is expected to be equally effective for other UFG heat-treatable alloys. PMID:24398915

Multiscale Modeling of Grain Boundaries in ZrB2: Structure, Energetics, and Thermal Resistance

NASA Technical Reports Server (NTRS)

Lawson, John W.; Daw, Murray S.; Squire, Thomas H.; Bauschlicher, Charles W., Jr.

2012-01-01

A combination of ab initio, atomistic and finite element methods (FEM) were used to investigate the structures, energetics and lattice thermal conductance of grain boundaries for the ultra high temperature ceramic ZrB2. Atomic models of idealized boundaries were relaxed using density functional theory. Information about bonding across the interfaces was determined from the electron localization function. The Kapitza conductance of larger scale versions of the boundary models were computed using non-equilibrium molecular dynamics. The interfacial thermal parameters together with single crystal thermal conductivities were used as parameters in microstructural computations. FEM meshes were constructed on top of microstructural images. From these computations, the effective thermal conductivity of the polycrystalline structure was determined.

Microstructural evidence of melting in crustal rocks (Invited)

NASA Astrophysics Data System (ADS)

Holness, M. B.; Cesare, B.; Sawyer, E. W.

2010-12-01

The signature of the former presence of melt on a microscopic scale is highly variable, subject to modification both during the melting event and during its subsequent history. Static pyrometamorphism results in melt films on grain boundaries between reactant phases. If a volume increase is involved, melting results in hydrofracture. On a longer timescale, as demonstrated by fragments of the crustal source in lava flows at El Hoyazo (SE Spain), melt occurs throughout the rock. These examples are highly unusual: the great majority of rocks that underwent melting cooled more slowly, permitting microstructural modification driven by a combination of textural equilibration, reaction and deformation. In the absence of deformation, and at constant temperature, melt-bearing rocks approach textural equilibrium, characterised by uniform grain size, smoothly curved grain boundaries and the establishment at all three-grain junctions of the equilibrium dihedral angle. The dihedral angle controls melt connectivity, with consequences for melt mobility and rock rheology. However, deformation is the rule rather than the exception in regional metamorphic terrains with profound effects on melt distribution. If deformation occurs predominantly by diffusive processes, textural equilibration can keep pace. At higher deformation rates melt is squeezed into planar pockets aligned parallel to the shearing direction or perpendicular to the extensional stress. Microstructures formed during solidification are controlled by cooling rate, H2O, and the size of the melt pockets. Large pockets solidify to look like igneous rocks. In small pores the supersaturation required for crystal growth is high and melt persist to lower temperatures, even being preserved as tiny glassy inclusions (“nanogranites”) in regional terranes. The pore size effect changes crystallization order, resulting in small, highly cuspate grains on grain boundaries with low dihedral angles. Crystallisation microstructures of poly-component liquids are highly dependent on diffusion rates, and therefore H2O content. Dry conditions result in diffusion-limited crystallisation to form intergrowths and symplectites (e.g. granophyre). The cooling rate must be slow in order to nucleate and grow individual grains from the melt. If the melt was primarily concentrated in thick films on grain boundaries this results in the “string of beads” texture. If there is sufficient water, and the rocks stay sufficiently hot, the microstructures will move towards a granular texture, driven by the reduction in interfacial energy. Highly cuspate pseudomorphs of melt at three-grain junctions will become rounded as the dihedral angle increases (generally towards the range 110-140°). Melt-related microstructures are more likely to be retained in dry rocks: in migmatite terranes in which melting was driven by infiltration of aqueous fluids and where melt extraction wasn’t pervasive, microstructures are likely to have been significantly modified by sub-solidus recrystallisation, especially likely if the rock underwent intense deformation on the retrograde path.

Characterization of microstructure and texture across dissimilar super duplex/austenitic stainless steel weldment joint by super duplex filler metal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eghlimi, Abbas, E-mail: a.eghlimi@ma.iut.ac.ir; Shamanian, Morteza; Eskandarian, Masoomeh

In the present paper, microstructural changes across an as-welded dissimilar austenitic/duplex stainless steel couple welded by a super duplex stainless steel filler metal using gas tungsten arc welding process is characterized with optical microscopy and electron back-scattered diffraction techniques. Accordingly, variations of microstructure, texture, and grain boundary character distribution of base metals, heat affected zones, and weld metal were investigated. The results showed that the weld metal, which was composed of Widmanstätten austenite side-plates and allotriomorphic grain boundary austenite morphologies, had the weakest texture and was dominated by low angle boundaries. The welding process increased the ferrite content but decreasedmore » the texture intensity at the heat affected zone of the super duplex stainless steel base metal. In addition, through partial ferritization, it changed the morphology of elongated grains of the rolled microstructure to twinned partially transformed austenite plateaus scattered between ferrite textured colonies. However, the texture of the austenitic stainless steel heat affected zone was strengthened via encouraging recrystallization and formation of annealing twins. At both interfaces, an increase in the special character coincident site lattice boundaries of the primary phase as well as a strong texture with <100> orientation, mainly of Goss component, was observed. - Graphical abstract: Display Omitted - Highlights: • Weld metal showed local orientation at microscale but random texture at macroscale. • Intensification of <100> orientated grains was observed adjacent to the fusion lines. • The austenite texture was weaker than that of the ferrite in all duplex regions. • Welding caused twinned partially transformed austenites to form at SDSS HAZ. • At both interfaces, the ratio of special CSL boundaries of the primary phase increased.« less

Grain Boundary Sliding in Deforming Wehrlite: Rheology and Microstructure

NASA Astrophysics Data System (ADS)

Zhao, N.; Hirth, G.; Cooper, R. F.; Kruckenberg, S. C.

2016-12-01

Elastic anisotropy of Earth's upper mantle used to be attributed exclusively to dislocation creep. However, recent experimental results suggest that crystallographic preferred orientation (CPO) in olivine, which contributes to elastic anisotropy, could also form during grain boundary sliding [e.g., 1-3]. Nevertheless, the fundamental problem of how CPO forms during grain boundary sliding is not fully understood. Our current efforts examine the grain-size-sensitive flow of wehrlite, to characterize the influence of the second phase (clinopyroxene) both on olivine CPO formation as well as the propensity of grain boundary sliding and accumulated strain to effect solid-state phase separation (i.e., metamorphic layering). Creep tests on fine-grain-size (2-5 µm) olivine and clinopyroxene aggregates (T =1100-1200ºC; P = 1.5 GPa; γ=3-7) have been conducted. These reveal strong type-B fabric for olivine. Characterization of effects of grain size, temperature and applied strain rate reveal the grain size dependence, stress exponent and activation energy of the flow kinetics of wehrlite. The stress exponent, which is similar to stress exponent for harzburgite reported by Sundberg & Cooper [1], and grain-size dependence suggest that the dominant deformation mechanism in our experiments may be grain boundary sliding. A large stress drop in early segments of experiments suggest an evolution of microstructure. The Fourier transform of backscatter images demonstrates that there exists a direction of foliation, defined by Ol-Cpx heterophase boundaries, which may be the key to understand the development of CPO formation. [1] Sundberg, M. & Cooper, R. F., J. Geophys. Res., 2008. [2] Miyazaki, T., Sueyoshi, K., and Hiraga, T., Nature, 2013. [3] Tielke, J. A., L. N. Hansen, M. Tasaka, C. Meyers, M. E. Zimmerman, and D. L. Kohlstedt, J. Geophys. Res., 2016.

Strain induced grain boundary migration effects on grain growth of an austenitic stainless steel during static and metadynamic recrystallization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Paggi, A., E-mail: alpaggi@tenaris.com; Angella, G.; Donnini, R.

Static and metadynamic recrystallization of an AISI 304L austenitic stainless steel was investigated at 1100 °C and 10{sup −} {sup 2} s{sup −} {sup 1} strain rate. The kinetics of recrystallization was determined through double hit compression tests. Two strain levels were selected for the first compression hit: ε{sub f} = 0.15 for static recrystallization (SRX) and 0.25 for metadynamic recrystallization (MDRX). Both the as-deformed and the recrystallized microstructures were investigated through optical microscopy and electron back-scattered diffraction (EBSD) technique. During deformation, strain induced grain boundary migration appeared to be significant, producing a square-like grain boundary structure aligned along themore » directions of the maximum shear stresses in compression. EBSD analysis revealed to be as a fundamental technique that the dislocation density was distributed heterogeneously in the deformed grains. Grain growth driven by surface energy reduction was also investigated, finding that it was too slow to explain the experimental data. Based on microstructural results, it was concluded that saturation of the nucleation sites occurred in the first stages of recrystallization, while grain growth driven by strain induced grain boundary migration (SIGBM) dominated the subsequent stages. - Highlights: • Recrystallization behavior of a stainless steel was investigated at 1100 °C. • EBSD revealed that the dislocation density distribution was heterogeneous during deformation. • Saturation of nucleation sites occurred in the first stages of recrystallization. • Strain induced grain boundary migration (SIGBM) effects were significant. • Grain growth driven by SIGBM dominated the subsequent stages.« less

Effects of microstructural variation on Charpy impact properties in heavy-section Mn-Mo-Ni low alloy steel for reactor pressure vessel

NASA Astrophysics Data System (ADS)

Hong, Seokmin; Song, Jaemin; Kim, Min-Chul; Choi, Kwon-Jae; Lee, Bong-Sang

2016-03-01

The effects of microstructural changes in heavy-section Mn-Mo-Ni low alloy steel on Charpy impact properties were investigated using a 210 mm thick reactor pressure vessel. Specimens were sampled from 5 different positions at intervals of 1/4 thickness from the inner surface to the outer surface. A detailed microstructural analysis of impact-fractured specimens showed that coarse carbides along the lath boundaries acted as fracture initiation sites, and cleavage cracks deviated at prior-austenite grain boundaries and bainite lath boundaries. Upper shelf energy was higher and energy transition temperature was lower at the surface positon, where fine bainitic microstructure with homogeneously distributed fine carbides were present. Toward the center, coarse upper bainite and precipitation of coarse inter-lath carbides were observed, which deteriorated impact properties. At the 1/4T position, the Charpy impact properties were worse than those at other positions owing to the combination of elongated-coarse inter-lath carbides and large effective grain size.

Shock induced damage in copper: A before and after, three-dimensional study

NASA Astrophysics Data System (ADS)

Menasche, David B.; Lind, Jonathan; Li, Shiu Fai; Kenesei, Peter; Bingert, John F.; Lienert, Ulrich; Suter, Robert M.

2016-04-01

We report on the microstructural features associated with the formation of incipient spall and damage in a fully recrystallized, high purity copper sample. Before and after ballistic shock loading, approximately 0.8 mm3 of the sample's crystal lattice orientation field is mapped using non-destructive near-field High Energy Diffraction Microscopy. Absorption contrast tomography is used to image voids after loading. This non-destructive interrogation of damage initiation allows for novel characterization of spall points vis-a-vis microstructural features and a fully 3D examination of microstructural topology and its influence on incipient damage. The spalled region is registered with and mapped back onto the pre-shock orientation field. As expected, the great majority of voids occur at grain boundaries and higher order microstructural features; however, we find no statistical preference for particular grain boundary types. The damaged region contains a large volume of Σ-3 (60 °<111 >) connected domains with a large area fraction of incoherent Σ-3 boundaries.

Experimental constraints and theoretical bases for microstructural damage in plate boundary shear zones

NASA Astrophysics Data System (ADS)

Skemer, P. A.; Cross, A. J.; Bercovici, D.

2016-12-01

(Ultra)mylonites from plate boundary shear zones are characterized by severe grain-size reduction and well-mixed mineral phases. The evolution from relatively undeformed tectonite protoliths to highly deformed (ultra)mylonites via the formation of new grain and phase boundaries is described as microstructural `damage.' Microstructural damage is important for two reasons: grain-size reduction is thought to result in significant rheological weakening, while phase mixing inhibits mechanical recovery and preserves the zone of weakness to be reactivated repeatedly throughout the tectonic cycle. Grain-size reduction by dynamic recrystallization has been studied extensively in both geologic and engineered materials, yet the progressive mixing of mineral phases during high pressure/temperature shear - the other essential element of damage or mylonitization - is not well understood. In this contribution we present new experimental results and theory related to two distinct phase mixing processes. First, we describe high strain torsion experiments on calcite and anhydrite mixtures and a simple geometric mixing model related to the stretching and thinning of monophase domains. Second, we describe a grain-switching mechanism that is driven by the surface-tension driven migration of newly formed interphase triple junctions. Unlike dynamic recrystallization, which occurs at relatively small strains, both phase mixing mechanisms described here appear to require extremely large strains, a prediction that is consistent with geologic observations. These data suggest that ductile shear zones experience long, transient intervals of microstructural evolution during which rheology is not at steady state. Microstructural damage may be interpreted as the product of several interconnected physical processes, which are collectively essential to the preservation of long-lived, Earth-like plate tectonics.

Effect of Hot Rolling on the Microstructure and Mechanical Properties of Nitrogen Alloyed Austenitic Stainless Steel

NASA Astrophysics Data System (ADS)

Chenna Krishna, S.; Karthick, N. K.; Jha, Abhay K.; Pant, Bhanu; Cherian, Roy M.

2018-05-01

In the present investigation, the effect of multi-pass hot rolling in the temperature range of 700-1000 °C on the microstructure and mechanical properties of nitrogen alloyed austenitic stainless steel was studied with the aid of optical microscopy, tensile testing and x-ray diffraction measurements. The microstructural changes that occurred in the hot rolled specimens were elongation of grains in rolling direction, nucleation of new grains at the grain boundaries of elongated grains and growth of nucleated grains to form fully recrystallized grains. Elongated grains formed at lower rolling temperature (700-800 °C) due to inadequate strain/temperature for the initiation of dynamic recrystallization. At higher rolling temperature (900-1000 °C), fine grains formed due to dynamic recrystallization. Tensile properties showed strong dependency on the rolling temperature. Tensile strength increased with the decrease in the rolling temperature at the cost of ductility. Maximum strength was observed in samples hot rolled at 700 °C with yield strength of 917 MPa and ductility of 25%. This variation in the tensile properties with the rolling temperature is attributed to changes in the dislocation density and grain structure. The estimated yield strength from the dislocation density, solid solution and grain boundary strengthening closely matched with experimentally determined yield strength confirming the role of dislocation density and grain size in the strengthening.

Effect of Hot Rolling on the Microstructure and Mechanical Properties of Nitrogen Alloyed Austenitic Stainless Steel

NASA Astrophysics Data System (ADS)

Chenna Krishna, S.; Karthick, N. K.; Jha, Abhay K.; Pant, Bhanu; Cherian, Roy M.

2018-04-01

In the present investigation, the effect of multi-pass hot rolling in the temperature range of 700-1000 °C on the microstructure and mechanical properties of nitrogen alloyed austenitic stainless steel was studied with the aid of optical microscopy, tensile testing and x-ray diffraction measurements. The microstructural changes that occurred in the hot rolled specimens were elongation of grains in rolling direction, nucleation of new grains at the grain boundaries of elongated grains and growth of nucleated grains to form fully recrystallized grains. Elongated grains formed at lower rolling temperature (700-800 °C) due to inadequate strain/temperature for the initiation of dynamic recrystallization. At higher rolling temperature (900-1000 °C), fine grains formed due to dynamic recrystallization. Tensile properties showed strong dependency on the rolling temperature. Tensile strength increased with the decrease in the rolling temperature at the cost of ductility. Maximum strength was observed in samples hot rolled at 700 °C with yield strength of 917 MPa and ductility of 25%. This variation in the tensile properties with the rolling temperature is attributed to changes in the dislocation density and grain structure. The estimated yield strength from the dislocation density, solid solution and grain boundary strengthening closely matched with experimentally determined yield strength confirming the role of dislocation density and grain size in the strengthening.

Evolution of microstructure and grain boundary character distribution of a tin bronze annealed at different temperatures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huang, Weijiu; Chongqing Municipal Key Laboratory of Institutions of Higher Education for Mould Technology, Chongqing University of Technology, Chongqing 400054; Chai, Linjiang, E-mail: chailinjiang@cqut.edu.cn

2016-04-15

Specimens cut from a rolled tin bronze sheet were annealed at 400–800 °C for 1 h and evolution of their microstructures was then characterized in details by electron channeling contrast imaging and electron backscatter diffraction techniques. Particularly, statistics on special boundaries (SBs) with Σ ≤ 29 and network connectivity of random high angle boundaries (HABs) in the annealed specimens were examined to probe optimization potentials of grain boundary character distribution (GBCD) for this material. Results show that the deformed microstructure in the as-received material begins to be recrystallized when the annealing temperature increase to 500 °C and average grain sizesmore » surge with further increasing temperatures. As a result of the recrystallization, a large number of annealing twins (with Σ3 misorientation) are produced, leading to remarkably increased fractions of SBs (f{sub SBs}). Thanks to preexisting dense low angle boundaries, the majority of SBs in the 500 °C specimen with only partial recrystallization are Σ3{sub ic} (incoherent) boundaries, which effectively disrupt connectivity of random HABs network. Although the f{sub SBs} can be further increased (up to 72.5%) in specimens with full recrystallization (at higher temperatures), the Σ3{sub ic} boundaries would be replaced to some extent by Σ3{sub c} (coherent) boundaries which do not contribute directly to optimizing the GBCD. This work should be able to provide clear suggestions on applying the concept of grain boundary engineering to tin bronze alloys. - Highlights: • The rolled tin bronze begins to be recrystallized as temperature increases to 500 °C. • A lot of SBs are produced after recrystallization and the highest f{sub SBs} is 72.5%. • Partially recrystallized specimen has the optimum GBCD due to more Σ3{sub ic} boundaries. • The Σ3{sub ic} boundaries are replaced by Σ3{sub c} boundaries after full recrystallization.« less

Anisotropic and Heterogeneous Development of Microstructures. Combining Laboratory/Synchrotron X-rays and EBSD on a few SPD Metallic Systems

NASA Astrophysics Data System (ADS)

Bolmaro, Raúl E.; De Vincentis, Natalia S.; Benatti, Emanuel; Kliauga, Andrea M.; Avalos, Martina C.; Schell, Norbert; Brokmeier, Heinz-Günter

2014-08-01

The onset of Severe Plastic Deformation (SPD) regime is quite instructive on the possible origins of the nano-microstructures developed in metals and alloys. It is known that grain fragmentation and dislocation accumulation, among other defects, proceed at different paces depending fundamentally on grain orientations and active deformation mechanisms. There have been many attempts to characterize nano-microstructure anisotropy, leading all of them to sometimes contradictory conclusions. Moreover, the characterizations rely on different measurements techniques and pos-processing approaches, which can be observing different manifestations of the same phenomena. On the current presentation we show a few experimental and computer pos-processing and simulation approaches, applied to some SPD/alloy systems. Williamson-Hall and Convolutional Multiple Whole Profile (CMWP) techniques will be applied to peak broadening analysis on experimental results stemming from laboratory Cu Ka X-rays, and synchrotron radiation from LNLS (Laboratório Nacional de Luz Síncrotron, Campinas, Brazil) and Petra III line (HEMS station, at DESY, Hamburg, Germany). Taking advantage of the EBSD capability of giving information on orientational and topological characteristics of grain boundaries, microstructures, grain sizes, etc., we also performed investigations on dislocation density and Geometrically Necessary Dislocation Boundaries (GNDB) and their correlation with texture components. Orientation dependent nano-microstructures and domain sizes are shown on the scheme of generalized pole figures and discussions provide some hints on nano-microstructure anisotropy.

Preparation of porous (Ba,Sr)TiO3 by adding corn-starch

NASA Astrophysics Data System (ADS)

Kim, J.-G.; Sim, J.-H.; Cho, W.-S.

2002-11-01

A new method of preparing porous (Ba,Sr)TiO3 ceramics has been introduced, using an ordinary ceramics processing technique. The effect of corn-starch on the positive temperature coefficient of resistivity characteristics and microstructure of the porous (Ba,Sr)TiO3 ceramics has been investigated. When the corn-starch addition was 1-20 wt%, the PTCR jump was over 106 and 1-2 orders higher than that of samples without corn-starch. Also, it was found that the (Ba,Sr)TiO3 ceramics had porous microstructure by the addition of corn-starch. The porosity of the ceramics with 20 wt% corn-starch was 44%. The electrical properties of the (Ba,Sr)TiO3 ceramics have been discussed, based on the microstructure, resistivity of grain boundaries, donor concentration of grains and the electrical potential barrier of grain boundaries.

Creep deformation and mechanisms in Haynes 230 at 800 °C and 900 °C

NASA Astrophysics Data System (ADS)

Pataky, Garrett J.; Sehitoglu, Huseyin; Maier, Hans J.

2013-11-01

Creep was studied in Haynes 230, a material candidate for the very high temperature reactor's intermediate heat exchanger, at 800 °C and 900 °C. This study focused on the differences between the behavior at the two elevated temperature, and using the microstructure, grain boundary serrations and triple junction strain concentrations were quantitatively identified. There was significant damage in the 900 °C samples and the creep was almost entirely tertiary. In contrast, the 800 °C sample exhibited secondary creep. Using an Arrhenius equation, the minimum creep rate exponents were found to be n ≈ 3 and n ≈ 5 for 900 °C and 800 °C, respectively. The creep mechanisms were identified as solute drag for n ≈ 3 and dislocation climb for n ≈ 5. Strain concentrations were identified at triple junctions and grain boundary serrations using high resolution digital image correlation overlaid on the microstructure. The grain boundary serrations restrict grain boundary sliding which may reduce the creep damage at triple junctions and extend the creep life of Haynes 230 at elevated temperatures.

Heterogeneous Creep Deformations and Correlation to Microstructures in Fe-30Cr-3Al Alloys Strengthened by an Fe 2Nb Laves Phase

DOE PAGES

Shassere, Benjamin; Yamamoto, Yukinori; Poplawsky, Jonathan; ...

2017-08-07

We have develooped a new Fe-Cr-Al (FCA) alloy system with good oxidation resistance and creep strength at high temperature. The alloy system is a candidate for use in future fossil-fueled power plants. The creep strength of these alloys at 973 K (700 °C) was found to be comparable with traditional 9 pct Cr ferritic–martensitic steels. A few FCA alloys with general composition of Fe-30Cr-3Al-.2Si-xNb (x = 0, 1, or 2) with a ferrite matrix and Fe 2Nb-type Laves precipitates were prepared. The detailed microstructural characterization of samples, before and after creep rupture testing, indicated precipitation of the Laves phase withinmore » the matrix, Laves phase at the grain boundaries, and a 0.5 to 1.5 μm wide precipitate-free zone (PFZ) parallel to all the grain boundaries. In these alloys, the areal fraction of grain boundary Laves phase and the width of the PFZ controlled the cavitation nucleation and eventual grain boundary ductile failure. Finally, we used a phenomenological model to compare the creep strain rates controlled by the effects of the particles on the dislocations within the grain and at grain boundaries. (The research sponsored by US-DOE, Office of Fossil Energy, the Crosscutting Research Program).« less

Multiscale modeling of localized resistive heating in nanocrystalline metals subjected to electropulsing

NASA Astrophysics Data System (ADS)

Zhao, Jingyi; Wang, G.-X.; Dong, Yalin; Ye, Chang

2017-08-01

Many electrically assisted processes have been reported to induce changes in microstructure and metal plasticity. To understand the physics-based mechanisms behind these interesting phenomena, however, requires an understanding of the interaction between the electric current and heterogeneous microstructure. In this work, multiscale modeling of the electric current flow in a nanocrystalline material is reported. The cellular automata method was used to track the nanoscale grain boundaries in the matrix. Maxwell's electromagnetic equations were solved to obtain the electrical potential distribution at the macro scale. Kirchhoff's circuit equation was solved to obtain the electric current flow at the micro/nano scale. The electric current distribution at two representative locations was investigated. A significant electric current concentration was observed near the grain boundaries, particularly near the triple junctions. This higher localized electric current leads to localized resistive heating near the grain boundaries. The electric current distribution could be used to obtain critical information such as localized resistive heating rate and extra system free energy, which are critical for explaining many interesting phenomena, including microstructure evolution and plasticity enhancement in many electrically assisted processes.

In-situ TEM observation of the response of ultrafine- and nanocrystalline-grained tungsten to extreme irradiation environments

PubMed Central

El-Atwani, O.; Hinks, J. A.; Greaves, G.; Gonderman, S.; Qiu, T.; Efe, M.; Allain, J. P.

2014-01-01

The accumulation of defects, and in particular He bubbles, can have significant implications for the performance of materials exposed to the plasma in magnetic-confinement nuclear fusion reactors. Some of the most promising candidates for deployment into such environments are nanocrystalline materials as the engineering of grain boundary density offers the possibility of tailoring their radiation resistance properties. In order to investigate the microstructural evolution of ultrafine- and nanocrystalline-grained tungsten under conditions similar to those in a reactor, a transmission electron microscopy study with in situ 2 keV He+ ion irradiation at 950°C has been completed. A dynamic and complex evolution in the microstructure was observed including the formation of defect clusters, dislocations and bubbles. Nanocrystalline grains with dimensions less than around 60 nm demonstrated lower bubble density and greater bubble size than larger nanocrystalline (60–100 nm) and ultrafine (100–500 nm) grains. In grains over 100 nm, uniform distributions of bubbles and defects were formed. At higher fluences, large faceted bubbles were observed on the grain boundaries, especially on those of nanocrystalline grains, indicating the important role grain boundaries can play in trapping He and thus in giving rise to the enhanced radiation tolerance of nanocrystalline materials. PMID:24796578

Two-Step Sintering Behavior of Sol-Gel Derived Dense and Submicron-Grained YIG Ceramics

NASA Astrophysics Data System (ADS)

Chen, Ruoyuan; Zhou, Jijun; Zheng, Liang; Zheng, Hui; Zheng, Peng; Ying, Zhihua; Deng, Jiangxia

2018-04-01

In this work, dense and submicron-grain yttrium iron garnet (YIG, Y3Fe5O12) ceramics were fabricated by a two-step sintering (TSS) method using nano-size YIG powder prepared by a citrate sol-gel method. The densification, microstructure, magnetic properties and ferromagnetic resonance (FMR) linewidth of the ceramics were investigated. The sample prepared at 1300°C in T 1, 1225°C in T 2 and 18 h holding time has a density higher than 98% of the theoretical value and exhibits a homogeneous microstructure with fine grain size (0.975 μm). In addition, the saturation magnetization ( M S) of this sample reaches 27.18 emu/g. High density and small grain size can also achieve small FMR linewidth. Consequently, these results show that the sol-gel process combined with the TSS process can effectively suppress grain-boundary migration while maintaining active grain-boundary diffusion to obtain dense and fine-grained YIG ceramics with appropriate magnetic properties.

Phase-field study of grain boundary tracking behavior in crack-seal microstructures

NASA Astrophysics Data System (ADS)

Ankit, Kumar; Nestler, Britta; Selzer, Michael; Reichardt, Mathias

2013-12-01

In order to address the growth of crystals in veins, a multiphase-field model is used to capture the dynamics of crystals precipitating from a super-saturated solution. To gain a detailed understanding of the polycrystal growth phenomena in veins, we investigate the influence of various boundary conditions on crystal growth. In particular, we analyze the formation of vein microstructures resulting from the free growth of crystals as well as crack-sealing processes. We define the crystal symmetry by considering the anisotropy in surface energy to simulate crystals with flat facets and sharp corners. The resulting growth competition of crystals with different orientations is studied to deduce a consistent orientation selection rule in the free-growth regime. Using crack-sealing simulations, we correlate the grain boundary tracking behavior depending on the relative rate of crack opening, opening trajectory, initial grain size, and wall roughness. Further, we illustrate how these parameters induce the microstructural transition between blocky (crystals growing anisotropically) to fibrous morphology (isotropic) and formation of grain boundaries. The phase-field simulations of crystals in the free-growth regime (in 2D and 3D) indicate that the growth or consumption of a crystal is dependent on the orientation difference with neighboring crystals. The crack-sealing simulation results (in 2D and 3D) reveal that crystals grow isotropically and grain boundaries track the opening trajectory if the wall roughness is high, opening increments are small, and crystals touch the wall before the next crack increment starts. Further, we find that within the complete crack-seal regime, anisotropy in surface energy results in the formation of curved/oscillating grain boundaries (instead of straight) when the crack-opening velocity is increased and wall roughness is not sufficiently high. Additionally, the overall capability of phase-field method to simulate large-scale polycrystal growth in veins (in 3D) is demonstrated enumerating the main advantages of adopting the novel approach.

Microstructural characterization of ultrasonic impact treated aluminum-magnesium alloy

NASA Astrophysics Data System (ADS)

Tran, Kim Ngoc Thi

Aluminum 5456-H116 has high as-welded strength, is formable, and highly corrosion resistant, however, it can become sensitized when exposed to elevated temperatures for a prolonged time. Sensitization results in the formation of a continuous β phase at the grain boundaries that is anodic to the matrix. Thus the grain boundaries become susceptible to stress corrosion cracking (SCC) and intergranular corrosion cracking (IGC). Cracking issues on aluminum superstructures have prompted the use of a severe plastic deformation processes, such as ultrasonic impact treatment (UIT), to improve SCC resistance. This study correlated the effects of UIT on the properties of 5456-H116 alloy to the microstructural evolution of the alloy and helped develop a fundamental understanding of the mechanisms that cause the microstructural evolution. Ultrasonic impact treatment produces a deformed layer at the surface ˜ 10 to 18 µm thick that is characterized by micro-cracks, tears, and voids. Ultrasonic impact treatment results in grain refinement within the deformation layer and extending below the deformed layer. The microstructure exhibits weak crystallographic texture with larger fraction of high angle grain boundaries. Nanocrystalline grains within the deformation layer vary in size from 2 to 200 nm in diameter and exhibit curved or wavy grain boundaries. The nanocrystalline grains are thermally stable up to 300°C. Above 300°C, grain growth occurs with an activation energy of ˜ 32 kJ/mol. Below the deformation layer, the microstructure is characterized by submicron grains, complex structure of dislocations, sub-boundaries, and Moiré fringes depicting overlapping grains. The deformation layer does not exhibit the presence of a continuous β phase, however below the deformation layer; a continuous β phase along the grain boundaries is present. In general the highest hardness and yield strength is at the UIT surface which is attributed to the formation of nanocrystalline grains. Although the highest hardness and yield strength was observed at the UIT surface, the results were mixed with some lower values. The lower hardness and yield strength values at the UIT surface are attributed to the voids and micro cracking/micro voids observed in the deformation layer. The fracture mode was transgranular ductile fracture with micro void coalescence and dimples. Both UIT and untreated material exhibit similar levels of intergranular corrosion susceptibility. Corrosive attack was intergranular with slightly deeper attack in the untreated material. Numerical simulation modeling showed that the calculated residual stress under the tool, ˜80 MPa, is of the same order of magnitude as the compressive residual stresses measured by XRD measurements near the surface. Modeling also showed that high effective strains were induced almost immediately. The UIT process also resulted in rapid localized heating to a maximum temperature of ˜32°C during the first eleven pin tool cycles. The model also showed that during UIT processing, the material undulates as the pin tool impacts and retracts from the surface of the material. The undulations represent the elastic response of the surface to the compressive stresses built up during a pin tool cycle.

Strain-Annealing Based Grain Boundary Engineering to Evaluate its Sole Implication on Intergranular Corrosion in Extra-Low Carbon Type 304L Austenitic Stainless Steel

NASA Astrophysics Data System (ADS)

Pradhan, S. K.; Bhuyan, P.; Kaithwas, C.; Mandal, Sumantra

2018-05-01

Strain-annealing based thermo-mechanical processing has been performed to promote grain boundary engineering (GBE) in an extra-low carbon type austenitic stainless steel without altering the grain size and residual strain to evaluate its sole influence on intergranular corrosion. Single-step processing comprising low pre-strain ( 5 and 10 pct) followed by annealing at 1273 K for 1 hour have resulted in a large fraction of Σ3 n boundaries and significant disruption in random high-angle grain boundaries (RHAGBs) connectivity. This is due to the occurrence of prolific multiple twinning in these specimens as confirmed by their large twin-related domain and twin-related grain size ratio. Among the iterative processing, the schedule comprising two cycles of 10 and 5 pct deformation followed by annealing at 1173 K for 1 hour has yielded the optimum GBE microstructure with the grain size and residual strain akin to the as-received condition. The specimens subjected to the higher number of iterations failed to realize GBE microstructures due to the occurrence of partial recrystallization. Owing to the optimum grain boundary character distribution, the GBE specimen has exhibited remarkable resistance against sensitization and intergranular corrosion as compared to the as-received condition. Furthermore, the lower depth of percolation in the GBE specimen is due to the significant disruption of RHAGBs connectivity as confirmed from its large twin-related domain and lower fractal dimension.

Strain-Annealing Based Grain Boundary Engineering to Evaluate its Sole Implication on Intergranular Corrosion in Extra-Low Carbon Type 304L Austenitic Stainless Steel

NASA Astrophysics Data System (ADS)

Pradhan, S. K.; Bhuyan, P.; Kaithwas, C.; Mandal, Sumantra

2018-07-01

Strain-annealing based thermo-mechanical processing has been performed to promote grain boundary engineering (GBE) in an extra-low carbon type austenitic stainless steel without altering the grain size and residual strain to evaluate its sole influence on intergranular corrosion. Single-step processing comprising low pre-strain ( 5 and 10 pct) followed by annealing at 1273 K for 1 hour have resulted in a large fraction of Σ3 n boundaries and significant disruption in random high-angle grain boundaries (RHAGBs) connectivity. This is due to the occurrence of prolific multiple twinning in these specimens as confirmed by their large twin-related domain and twin-related grain size ratio. Among the iterative processing, the schedule comprising two cycles of 10 and 5 pct deformation followed by annealing at 1173 K for 1 hour has yielded the optimum GBE microstructure with the grain size and residual strain akin to the as-received condition. The specimens subjected to the higher number of iterations failed to realize GBE microstructures due to the occurrence of partial recrystallization. Owing to the optimum grain boundary character distribution, the GBE specimen has exhibited remarkable resistance against sensitization and intergranular corrosion as compared to the as-received condition. Furthermore, the lower depth of percolation in the GBE specimen is due to the significant disruption of RHAGBs connectivity as confirmed from its large twin-related domain and lower fractal dimension.

Evolution of the viscosity of Earth's upper mantle: Grain-boundary sliding and the role of microstructure in olivine deformation

NASA Astrophysics Data System (ADS)

Hansen, Lars N.

Many features of plate tectonics cannot be explained with standard rheological models of the upper mantle. In particular, the localization of deformation at plate boundaries requires the viscosity of the constituent rocks to evolve spatially and temporally. Such rheological complexity may arise from changing microstructural state variables (e.g., grain size and crystallographic-fabric strength), but the degree to which microstructure contributes to the evolution of viscosity is unclear given our current understanding of deformation mechanisms in mantle minerals. Dislocation-accommodated grain-boundary sliding (GBS) is a potentially critical mechanism for localizing deformation in olivine because it imparts a sensitivity of the viscosity to the state of the microstructure while simultaneously providing mechanisms for changing the microstructure. However, many details of GBS in olivine are currently unknown including 1) the magnitude of the sensitivity of strain rate to crystallographic fabric and grain size, 2) the strength of the crystallographic fabrics produced, and 3) the anisotropy in viscosity of polycrystalline aggregates. Detailed knowledge of these unknowns is necessary to assess the importance of microstructural evolution in the operation of plate tectonics. This dissertation investigates the details of GBS in olivine through four sets of laboratory-based experiments. In Chapter 2, triaxial compressive creep experiments on aggregates of San Carlos olivine are used to develop a flow law for olivine deforming by GBS. Extrapolations of strain rate to geological conditions using the derived flow law indicate that GBS is the dominant deformation mechanism throughout the uppermost mantle. Crystallographic fabrics observed in deformed samples are consistent with upper-mantle seismic anisotropy. In Chapter 3, torsion experiments on iron-rich olivine are used to determine the rheological behavior of olivine deforming by GBS at large strains. The sensitivity of the strain rate to grain size and stress is demonstrated to be consistent with low-strain experiments. Additionally, the sensitivity of strain rate to the development of a crystallographic fabric is determined. Constitutive relationships including microstructural evolution are developed that accurately predict the observed stress as a function of strain. The results of Chapter 3 confirm that significant weakening is associated with both grain-size reduction and crystallographic-fabric development. In Chapter 4, torsion experiments on iron-rich olivine are used to determine if microstructural evolution can lead to strain localization. Experiments were conducted with either constant-strain-rate or constant-stress boundary conditions. Localization is only observed in samples deformed at constant-stress, which suggests boundary conditions affect the critical size of strength perturbation necessary for localization to occur. Strain localization is correlated with fine-grained regions, and a feedback mechanism between grain-size reduction and strain rate is proposed. In Chapter 5, both torsion and tension experiments are used to assess the mechanical anisotropy of previously deformed samples. Based on the direction of the applied stress relative to the orientation of a pre-existing crystallographic fabric, the viscosity is demonstrated to vary by over an order of magnitude. This observation suggests deformation can localize in regions that were previously deformed and retained a strong crystallographic fabric. The results of this dissertation elucidate the interplay between microstructure and deformation of olivine in the GBS regime. Because the viscosity of olivine-rich rocks deforming by GBS is dependent on both grain size and crystallographic fabric, heterogeneities in these microstructural parameters can lead to spatial and temporal variations in viscosity, possibly explaining the large-scale patterns of deformation in the upper mantle. Future numerical simulations can test the importance of microstructure in geodynamic processes by incorporating the constitutive relationships outlined in this dissertation.

Investigation of nucleation processes during dynamic recrystallization of ice using cryo-EBSD.

PubMed

Chauve, T; Montagnat, M; Barou, F; Hidas, K; Tommasi, A; Mainprice, D

2017-02-13

Nucleation mechanisms occurring during dynamic recrystallization play a crucial role in the evolution of microstructures and textures during high temperature deformation. In polycrystalline ice, the strong viscoplastic anisotropy induces high strain heterogeneities between grains which control the recrystallization mechanisms. Here, we study the nucleation mechanisms occurring during creep tests performed on polycrystalline columnar ice at high temperature and stress (T=-5°C;σ=0.5 MPa) by post-mortem analyses of deformation microstructures using cryogenic electron backscatter diffraction. The columnar geometry of the samples enables discrimination of the nuclei from the initial grains. Various nucleation mechanisms are deduced from the analysis of the nuclei relations with the dislocation sub-structures within grains and at grain boundaries. Tilt sub-grain boundaries and kink bands are the main structures responsible for development of polygonization and mosaic sub-structures. Nucleation by bulging at serrated grain boundaries is also an efficient nucleation mechanism near the grain boundaries where strain incompatibilities are high. Observation of nuclei with orientations not related to the 'parent' ones suggests the possibility of 'spontaneous' nucleation driven by the relaxation of the dislocation-related internal stress field. The complexity of the nucleation mechanisms observed here emphasizes the impact of stress and strain heterogeneities on dynamic recrystallization mechanisms.This article is part of the themed issue 'Microdynamics of ice'. © 2016 The Author(s).

Investigation of nucleation processes during dynamic recrystallization of ice using cryo-EBSD

PubMed Central

Barou, F.; Hidas, K.; Tommasi, A.; Mainprice, D.

2017-01-01

Nucleation mechanisms occurring during dynamic recrystallization play a crucial role in the evolution of microstructures and textures during high temperature deformation. In polycrystalline ice, the strong viscoplastic anisotropy induces high strain heterogeneities between grains which control the recrystallization mechanisms. Here, we study the nucleation mechanisms occurring during creep tests performed on polycrystalline columnar ice at high temperature and stress (T=−5°C;σ=0.5 MPa) by post-mortem analyses of deformation microstructures using cryogenic electron backscatter diffraction. The columnar geometry of the samples enables discrimination of the nuclei from the initial grains. Various nucleation mechanisms are deduced from the analysis of the nuclei relations with the dislocation sub-structures within grains and at grain boundaries. Tilt sub-grain boundaries and kink bands are the main structures responsible for development of polygonization and mosaic sub-structures. Nucleation by bulging at serrated grain boundaries is also an efficient nucleation mechanism near the grain boundaries where strain incompatibilities are high. Observation of nuclei with orientations not related to the ‘parent’ ones suggests the possibility of ‘spontaneous’ nucleation driven by the relaxation of the dislocation-related internal stress field. The complexity of the nucleation mechanisms observed here emphasizes the impact of stress and strain heterogeneities on dynamic recrystallization mechanisms. This article is part of the themed issue ‘Microdynamics of ice’. PMID:28025294

High-temperature deformation and microstructural analysis for Si3N4-Sc2O3

NASA Technical Reports Server (NTRS)

Cheong, Deock-Soo; Sanders, William A.

1990-01-01

It was indicated that Si3N4 doped with Sc2O3 may exhibit high temperature mechanical properties superior to Si3N4 systems with various other oxide sintered additives. High temperature deformation of samples was studied by characterizing the microstructures before and after deformation. It was found that elements of the additive, such as Sc and O, exist in small amounts at very thin grain boundary layers and most of them stay in secondary phases at triple and multiple grain boundary junctions. These secondary phases are devitrified as crystalline Sc2Si2O7. Deformation of the samples was dominated by cavitational processes rather than movements of dislocations. Thus the excellent deformation resistance of the samples at high temperature can be attributed to the very small thickness of the grain boundary layers and the crystalline secondary phase.

High-temperature deformation and microstructural analysis for silicon nitride-scandium(III) oxide

NASA Technical Reports Server (NTRS)

Cheong, Deock-Soo; Sanders, William A.

1992-01-01

It was indicated that Si3N4 doped with Sc2O3 may exhibit high temperature mechanical properties superior to Si3N4 systems with various other oxide sintered additives. High temperature deformation of samples was studied by characterizing the microstructures before and after deformation. It was found that elements of the additive, such as Sc and O, exist in small amounts at very thin grain boundary layers and most of them stay in secondary phases at tripple and multiple grain boundary junctions. These secondary phases are devitrified as crystalline Sc2Si2O7. Deformation of the samples was dominated by cavitational processes rather than movements of dislocations. Thus the excellent deformation resistance of the samples at high temperature can be attributed to the very small thickness of the grain boundary layers and the crystalline secondary phase.

Measuring grain boundary character distributions in Ni-base alloy 725 using high-energy diffraction microscopy

DOE PAGES

Bagri, Akbar; Hanson, John P.; Lind, J. P.; ...

2016-10-25

We use high-energy X-ray diffraction microscopy (HEDM) to characterize the microstructure of Ni-base alloy 725. HEDM is a non-destructive technique capable of providing three-dimensional reconstructions of grain shapes and orientations in polycrystals. The present analysis yields the grain size distribution in alloy 725 as well as the grain boundary character distribution (GBCD) as a function of lattice misorientation and boundary plane normal orientation. We find that the GBCD of Ni-base alloy 725 is similar to that previously determined in pure Ni and other fcc-base metals. We find an elevated density of Σ9 and Σ3 grain boundaries. We also observe amore » preponderance of grain boundaries along low-index planes, with those along (1 1 1) planes being the most common, even after Σ3 twins have been excluded from the analysis.« less

Effects of local film properties on the nucleation and growth of tin whiskers and hillocks

NASA Astrophysics Data System (ADS)

Sarobol, Pylin

Whiskers and hillocks grow spontaneously on Pb-free Sn electrodeposited films as a response to thin film stresses. Stress relaxation occurs by atom deposition to specific grain boundaries in the plane of the film, with hillocks being formed when grain boundary migration accompanies growth out of the plane of the film. The implication for whisker formation in electronics is serious: whiskers can grow to be millimeters long, sometimes causing short circuiting between adjacent components and, thereby, posing serious electrical reliability risks. In order to develop more effective whisker mitigation strategies, a predictive physics-based model has been needed. A growth model is developed, based on grain boundary faceting, localized Coble creep, as well as grain boundary sliding for whiskers, and grain boundary sliding with shear induced grain boundary migration for hillocks. In this model of whisker formation, two mechanisms are important: accretion of atoms by Coble creep on grain boundary planes normal to the growth direction inducing a grain boundary shear and grain boundary sliding in the direction of whisker growth. The model accurately captures the importance of the geometry of "surface grains"---shallow grains on film surfaces whose depths are significantly less than their in-plane grain sizes. A critical factor in the analysis is the ratio of the grain boundary sliding coefficient to the in-plane film compressive stress. If the accretion-induced shear stresses are not coupled to grain boundary motion and sliding occurs, a whisker forms. If the shear stress is coupled to grain boundary migration, a hillock forms. Based on this model, long whiskers grow from shallow surface grains with easy grain boundary sliding in the direction of growth. Other observed growth morphologies will be discussed in light of our model. Additional insights into the preferred sites for whisker and hillock growth were developed based on elastic anisotropy, local film microstructure, grain misorientation, and elastic strain energy density (ESED) as the driving force for growth. Local grain orientations and strains measured by synchrotron micro-diffraction in regions containing whiskers or hillocks were compared with elastic finite element analysis simulations, including Sn elastic anisotropy. Whisker and hillock grains were observed to have higher crystallographic misorientations with neighboring grains than generally observed in the microstructure. While elastic simulations predicted higher local out-of-plane elastic strains and ESEDs for whisker and hillock grains, synchrotron measurements of out-of-plane strains of whisker and hillock grains after growth showed relaxation, with correspondingly low ESEDs calculated from measured strains. This suggests that, before whisker or hillock formation, highly misoriented grains with high out-of-plane elastic strains and ESEDs relative to their neighbors determined, at least in part, which grains became whiskers or hillocks. Based on the models and experiments in this thesis, a clearer picture emerges of the necessary and sufficient conditions for tin whisker and hillock formation in thin films.

Influence of Tool Rotational Speed and Post-Weld Heat Treatments on Friction Stir Welded Reduced Activation Ferritic-Martensitic Steel

NASA Astrophysics Data System (ADS)

Manugula, Vijaya L.; Rajulapati, Koteswararao V.; Reddy, G. Madhusudhan; Mythili, R.; Bhanu Sankara Rao, K.

2017-08-01

The effects of tool rotational speed (200 and 700 rpm) on evolving microstructure during friction stir welding (FSW) of a reduced activation ferritic-martensitic steel (RAFMS) in the stir zone (SZ), thermo-mechanically affected zone (TMAZ), and heat-affected zone (HAZ) have been explored in detail. The influence of post-weld direct tempering (PWDT: 1033 K (760 °C)/ 90 minutes + air cooling) and post-weld normalizing and tempering (PWNT: 1253 K (980 °C)/30 minutes + air cooling + tempering 1033 K (760 °C)/90 minutes + air cooling) treatments on microstructure and mechanical properties has also been assessed. The base metal (BM) microstructure was tempered martensite comprising Cr-rich M23C6 on prior austenite grain and lath boundaries with intra-lath precipitation of V- and Ta-rich MC precipitates. The tool rotational speed exerted profound influence on evolving microstructure in SZ, TMAZ, and HAZ in the as-welded and post-weld heat-treated states. Very high proportion of prior austenitic grains and martensite lath boundaries in SZ and TMAZ in the as-welded state showed lack of strengthening precipitates, though very high hardness was recorded in SZ irrespective of the tool speed. Very fine-needle-like Fe3C precipitates were found at both the rotational speeds in SZ. The Fe3C was dissolved and fresh precipitation of strengthening precipitates occurred on both prior austenite grain and sub-grain boundaries in SZ during PWNT and PWDT. The post-weld direct tempering caused coarsening and coalescence of strengthening precipitates, in both matrix and grain boundary regions of TMAZ and HAZ, which led to inhomogeneous distribution of hardness across the weld joint. The PWNT heat treatment has shown fresh precipitation of M23C6 on lath and grain boundaries and very fine V-rich MC precipitates in the intragranular regions, which is very much similar to that prevailed in BM prior to FSW. Both the PWDT and PWNT treatments caused considerable reduction in the hardness of SZ. In the as-welded state, the 200 rpm joints have shown room temperature impact toughness close to that of BM, whereas 700 rpm joints exhibited very poor impact toughness. The best combination of microstructure and mechanical properties could be obtained by employing low rotational speed of 200 rpm followed by PWNT cycle. The type and size of various precipitates, grain size, and evolving dislocation substructure have been presented and comprehensively discussed.

Microstructure study of ZnO thin films on Si substrate grown by MOCVD

NASA Astrophysics Data System (ADS)

Huang, Jingyun; Ye, Zhizhen; Lu, Huanming; Wang, Lei; Zhao, Binghui; Li, Xianhang

2007-08-01

The microstructure of zinc oxide thin films on silicon substrates grown by metalorganic chemical vapour deposition (MOCVD) was characterized. The cross-sectional bright-field transmission electron microscopy (TEM) image showed that small ZnO columnar grains were embedded into large columnar grains, and the selected-area electron diffraction pattern showed that the ZnO/Si thin films were nearly c-axis oriented. The deviation angle along the ZnO (0 0 0 1) direction with respect to the growth direction of Si (1 0 0) was no more than 5°. The [0 0 0 1]-tilt grain boundaries in ZnO/Si thin films were investigated symmetrically by plan-view high resolution TEM. The boundaries can be classified into three types: low-angle boundaries described as an irregular array of edge dislocations, boundaries of near 30° angle with (1\\,0\\,\\bar{1}\\,0) facet structures and large-angle boundaries with symmetric structure which could be explained by a low Σ coincident site lattice structure mode. The research was useful to us for finding optimized growth conditions to improve ZnO/Si thin film quality.

Conductive paths through polycrystalline BaTiO{sub 3}: Scanning probe microscopy study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ayvazian, Talin; Bersuker, Gennadi; Lingley, Zachary R.

2016-08-15

The microstructural features determining the leakage current through polycrystalline BaTiO{sub 3} films are investigated using Conductive Atomic Force Microscopy. Grain boundaries are found to be the dominant conductive paths compared to the conduction through the grains. Grain boundary currents are observed to reversibly rise with the increase of the applied DC voltages, indicating that the current is controlled by a field-activated charge transport process.

Atomisti modeling of the microstructure and transport properties of lead-free solder alloys

NASA Astrophysics Data System (ADS)

Sellers, Michael S.

Damage mechanics models of lead-free solder joints in nanoelectronics continue to improve, and in doing so begin to utilize quantitative values describing processes at the atomic level, governing phenomena like electromigration and thermomigration. In particular, knowledge of the transport properties of specific microstructures helps continuum level models fully describe these larger-scale damage phenomena via multi-scale analysis. For example, diffusivities for different types of grain boundaries (fast diffusion paths for solvent and solute atoms, and vacancies), and a description of the boundary structure as a function of temperature, are critical in modeling solder microstructure evolution and, consequently, joint behavior under extreme temperature and electric current. Moreover, for damage that develops at larger length scales, surface energies and diffusivities play important roles in characterizing void stability and morphology. Unfortunately, experiments that investigate these kind of damage phenomena in the atomistic realm are often inconsistent or unable to directly quantify important parameters. One case is the particular transport and structural properties of grain boundaries in Sn (the main component in lead-free solder alloys) and their behavior in the presence of Ag and Cu impurities. This information is crucial in determining accurate diffusivity values for the common SnAgCu (SAC) type solder. Although an average grain boundary diffusivity has been reported for polycrystalline Sn in several works, the value for grain boundary width is estimated and specific diffusivities for boundaries known to occur in Sn have not been reported, to say nothing of solute effects on Sn diffusivity and grain boundary structure. Similarly, transport properties of Sn surfaces remain relatively uninvestigated as well. These gaps and inconsistencies in atomistic data must be remedied for micro- and macro-scale modeling to improve. As a complement to experimental work and possessing the ability to fill in the gaps, molecular simulation serves to reinforce experimental predictions and provide insight into the atomistic processes that govern studied phenomena. In the present body of work, we employ molecular statics and dynamics simulations in the characterization and computation of betaSn surface energies and surface diffusivities, the determination of diffusivities and structural properties of specific betaSn grain boundaries, and the investigation of Cu and Ag solute effects on betaSn grain boundaries. In our study of betaSn surfaces, energies for low number Miller index surfaces are computed and the (100) plane is found to have the lowest un-relaxed energy. We then find that two simple hopping mechanisms dominate adatom diffusion transitions on this surface. For each, we determine hopping rates of the adatom and compute its tracer diffusivity. Our work on grain boundaries investigates the self-diffusion properties and structure of several betaSn symmetric tilt grain boundaries using molecular dynamics simulations. We find that larger diffusive widths are exhibited by higher excess potential energy grain boundaries. Diffusivities in the directions parallel to the interface plane are also computed and activation energies are found with the Arrhenius relation. These are shown to agree well with experimental data. Finally, we examine the effect that solute atoms of Ag and Cu have on the microstructure of betaSn. Excess energies of the (101) symmetric tilt betaSn grain boundary are computed as a function of solute concentration at the interface, and we show that Ag lowers the energy at a greater rate than Cu. We also quantify segregation enthalpies and critical solute concentrations (where the excess energy of the boundary is reduced to zero). The effect of solute type on shear stress is also examined, and we show that solute has a strong effect on the stabilization of higher energy grain boundaries under shear stress. We then look at the self-diffusivity of Sn in the (101) symmetric tilt betaSn grain boundary and show that adding both Ag or Cu decrease the grain boundary self-diffusivity of Sn as solute amount in the interface increases. Effects of larger concentrations of Cu in particular are also investigated.

The microstructure of polar ice. Part II: State of the art

NASA Astrophysics Data System (ADS)

Faria, Sérgio H.; Weikusat, Ilka; Azuma, Nobuhiko

2014-04-01

An important feature of natural ice, in addition to the obvious relevance of glaciers and ice sheets for climate-related issues, is its ability to creep on geological time scales and low deviatoric stresses at temperatures very close to its melting point, without losing its polycrystalline character. This fact, together with its strong mechanical anisotropy and other notable properties, makes natural ice an interesting model material for studying the high-temperature creep and recrystallization of rocks in Earth's interior. After having reviewed the major contributions of deep ice coring to the research on natural ice microstructures in Part I of this work (Faria et al., 2014), here in Part II we present an up-to-date view of the modern understanding of natural ice microstructures and the deformation processes that may produce them. In particular, we analyze a large body of evidence that reveals fundamental flaws in the widely accepted tripartite paradigm of polar ice microstructure (also known as the "three-stage model," cf. Part I). These results prove that grain growth in ice sheets is dynamic, in the sense that it occurs during deformation and is markedly affected by the stored strain energy, as well as by air inclusions and other impurities. The strong plastic anisotropy of the ice lattice gives rise to high internal stresses and concentrated strain heterogeneities in the polycrystal, which demand large amounts of strain accommodation. From the microstructural analyses of ice cores, we conclude that the formation of many and diverse subgrain boundaries and the splitting of grains by rotation recrystallization are the most fundamental mechanisms of dynamic recovery and strain accommodation in polar ice. Additionally, in fine-grained, high-impurity ice layers (e.g. cloudy bands), strain may sometimes be accommodated by diffusional flow (at low temperatures and stresses) or microscopic grain boundary sliding via microshear (in anisotropic ice sheared at high temperatures). Grain boundaries bulged by migration recrystallization and subgrain boundaries are endemic and very frequent at almost all depths in ice sheets. Evidence of nucleation of new grains is also observed at various depths, provided that the local concentration of strain energy is high enough (which is not seldom the case). As a substitute for the tripartite paradigm, we propose a novel dynamic recrystallization diagram in the three-dimensional state space of strain rate, temperature, and mean grain size, which summarizes the various competing recrystallization processes that contribute to the evolution of the polar ice microstructure.

The effect of high-pressure torsion on the microstructure and properties of magnesium

NASA Astrophysics Data System (ADS)

Figueiredo, Roberto B.; Sabbaghianrad, Shima; Langdon, Terence G.

2017-05-01

High-pressure torsion provides the opportunity to introduce significant plastic strain at room temperature in magnesium and its alloys. It is now established that this processing operation produces ultrafine-grained structures and changes the properties of these materials. The present paper shows that the mechanism of grain refinement differs from f.c.c. and b.c.c. materials. It is shown that fine grains are formed at the grain boundaries of coarse grains and gradually consume the whole structure. Also, the processed material exhibits unusual mechanical properties due to the activation of grain boundary sliding at room temperature.

Effect of microstructural evolution by isothermal aging on the mechanical properties of 9Cr-1WVTa reduced activation ferritic/martensitic steels

NASA Astrophysics Data System (ADS)

Park, Min-Gu; Lee, Chang-Hoon; Moon, Joonoh; Park, Jun Young; Lee, Tae-Ho; Kang, Namhyun; Chan Kim, Hyoung

2017-03-01

The influence of microstructural changes caused by aging condition on tensile and Charpy impact properties was investigated for reduced activation ferritic-martensitic (RAFM) 9Cr-1WVTa steels having single martensite and a mixed microstructure of martensite and ferrite. For the mixed microstructure of martensite and ferrite, the Charpy impact properties deteriorated in both as-normalized and tempered conditions due to the ferrite and the accompanying M23C6 carbides at the ferrite grain boundaries which act as path and initiation sites for cleavage cracks, respectively. However, aging at 550 °C for 20-100 h recovered gradually the Charpy impact toughness without any distinct drop in strength, as a result of the spheroidization of the coarse M23C6 carbides at the ferrite grain boundaries, which makes crack initiation more difficult.

Orientation Dependence of the Deformation Microstructure of Ta-4%W after Cold-Rolling

NASA Astrophysics Data System (ADS)

Zhang, J.; Ma, G. Q.; Godfrey, A.; Shu, D. Y.; Chen, Q.; Wu, G. L.

2017-07-01

One of the common features of deformed face-centered cubic metals with medium to high stacking fault energy is the formation of geometrically necessary dislocation boundaries. The dislocation boundary arrangements in refractory metals with body-centered cubic crystal structure are, however, less well known. To address this issue a Ta-4%W alloy was cold rolled up to 70% in thickness in the present work. The resulting deformation microstructures were characterized by electron back-scattering diffraction and the dislocation boundary arrangements in each grain were revealed using sample-frame misorientation axis maps calculated using an in-house code. The maps were used to analyze the slip pattern of individual grains after rolling, revealing an orientation dependence of the slip pattern.

Grain Nucleation and Growth in Deformed NiTi Shape Memory Alloys: An In Situ TEM Study

NASA Astrophysics Data System (ADS)

Burow, J.; Frenzel, J.; Somsen, C.; Prokofiev, E.; Valiev, R.; Eggeler, G.

2017-12-01

The present study investigates the evolution of nanocrystalline (NC) and ultrafine-grained (UFG) microstructures in plastically deformed NiTi. Two deformed NiTi alloys were subjected to in situ annealing in a transmission electron microscope (TEM) at 400 and 550 °C: an amorphous material state produced by high-pressure torsion (HPT) and a mostly martensitic partly amorphous alloy produced by wire drawing. In situ annealing experiments were performed to characterize the microstructural evolution from the initial nonequilibrium states toward energetically more favorable microstructures. In general, the formation and evolution of nanocrystalline microstructures are governed by the nucleation of new grains and their subsequent growth. Austenite nuclei which form in HPT and wire-drawn microstructures have sizes close to 10 nm. Grain coarsening occurs in a sporadic, nonuniform manner and depends on the physical and chemical features of the local environment. The mobility of grain boundaries in NiTi is governed by the local interaction of each grain with its microstructural environment. Nanograin growth in thin TEM foils seems to follow similar kinetic laws to those in bulk microstructures. The present study demonstrates the strength of in situ TEM analysis and also highlights aspects which need to be considered when interpreting the results.

Powder metallurgy processing and deformation characteristics of bulk multimodal nickel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Farbaniec, L., E-mail: lfarban1@jhu.edu; Dirras, G., E-mail: dirras@univ-paris13.fr; Krawczynska, A.

2014-08-15

Spark plasma sintering was used to process bulk nickel samples from a blend of three powder types. The resulting multimodal microstructure was made of coarse (average size ∼ 135 μm) spherical microcrystalline entities (the core) surrounded by a fine-grained matrix (average grain size ∼ 1.5 μm) or a thick rim (the shell) distinguishable from the matrix. Tensile tests revealed yield strength of ∼ 470 MPa that was accompanied by limited ductility (∼ 2.8% plastic strain). Microstructure observation after testing showed debonding at interfaces between the matrix and the coarse entities, but in many instances, shallow dimples within the rim weremore » observed indicating local ductile events in the shell. Dislocation emission and annihilation at grain boundaries and twinning at crack tip were the main deformation mechanisms taking place within the fine-grained matrix as revealed by in-situ transmission electron microscopy. Estimation of the stress from loop's curvature and dislocation pile-up indicates that dislocation emission from grain boundaries and grain boundary overcoming largely contributes to the flow stress. - Highlights: • Bulk multi-modal Ni was processed by SPS from a powder blend. • Ultrafine-grained matrix or rim observed around spherical microcrystalline entities • Yield strength (470 MPa) and ductility (2.8% plastic strain) were measured. • Debonding was found at the matrix/microcrystalline entity interfaces. • In-situ TEM showed twinning, dislocation emission and annihilation at grain boundaries.« less

Effect of Microstructural Interfaces on the Mechanical Response of Crystalline Metallic Materials

NASA Astrophysics Data System (ADS)

Aitken, Zachary H.

Advances in nano-scale mechanical testing have brought about progress in the understanding of physical phenomena in materials and a measure of control in the fabrication of novel materials. In contrast to bulk materials that display size-invariant mechanical properties, sub-micron metallic samples show a critical dependence on sample size. The strength of nano-scale single crystalline metals is well-described by a power-law function, sigma ∝ D-n, where D is a critical sample size and n is a experimentally-fit positive exponent. This relationship is attributed to source-driven plasticity and demonstrates a strengthening as the decreasing sample size begins to limit the size and number of dislocation sources. A full understanding of this size-dependence is complicated by the presence of microstructural features such as interfaces that can compete with the dominant dislocation-based deformation mechanisms. In this thesis, the effects of microstructural features such as grain boundaries and anisotropic crystallinity on nano-scale metals are investigated through uniaxial compression testing. We find that nano-sized Cu covered by a hard coating displays a Bauschinger effect and the emergence of this behavior can be explained through a simple dislocation-based analytic model. Al nano-pillars containing a single vertically-oriented coincident site lattice grain boundary are found to show similar deformation to single-crystalline nano-pillars with slip traces passing through the grain boundary. With increasing tilt angle of the grain boundary from the pillar axis, we observe a transition from dislocation-dominated deformation to grain boundary sliding. Crystallites are observed to shear along the grain boundary and molecular dynamics simulations reveal a mechanism of atomic migration that accommodates boundary sliding. We conclude with an analysis of the effects of inherent crystal anisotropy and alloying on the mechanical behavior of the Mg alloy, AZ31. Through comparison to pure Mg, we show that the size effect dominates the strength of samples below 10 microm, that differences in the size effect between hexagonal slip systems is due to the inherent crystal anisotropy, suggesting that the fundamental mechanism of the size effect in these slip systems is the same.

The effect of hydrocarbons on the microstructural evolution in rock salt: a case study on hydrocarbon bearing Ara salt from the South Oman Salt Basin

NASA Astrophysics Data System (ADS)

Schmatz, Joyce; Urai, Janos L.; Wübbeler, Franziska M. M.; Sadler, Marc

2014-05-01

It has been shown that dilatant deformation promotes the incorporation of hydrocarbons into typically low permeable rock salt (Schoenherr et al., 2007). However, there is not much knowledge on subsequent mechanisms related to recrystallization processes, which cause morphological and chemical changes of the carbonic inclusions. This work aims to contribute to an increased understanding of fluid inclusion dynamics related to grain boundary migration recrystallization and hence to facilitate the interpretation of complex microstructures in recrystallized, multiphase salt rocks. In this case study we investigate hydrocarbon-impregnated salt from the Cambrian Ara Group in the South Oman Salt Basin. The samples were cored from cm-m thick anhydrite-salt sequences overlying hydrocarbon bearing carbonate stringers in 3300 m depth. The anhydrite layers consist mainly of fine-grained anhydrite, which contains calcite, dolomite, and olivine inclusions. Solid bitumen and lighter hydrocarbon phases are observed in between the anhydrite grains and along cracks. Anhydrite layers host salt veins, which contain fragments of anhydrite. These fragments do not differ in composition or structure from the host material and the related vein microstructures indicate crack-seal mechanisms. Halite in the salt layers is almost entirely recrystallized with solid inclusions consisting of anhydrite, calcite, dolomite and olivine with hydrocarbon-coatings present inside grains and along grain boundaries. Solid inclusions cause pinning indicated by a decreased recrystallized grain size and by the presence of grains with preserved substructures representing earlier deformation phases. We observe two types of carbonic inclusions: I) solid bitumen coatings along grain boundaries and microcracks, interpreted to be incorporated into the salt in an overpressure state that allowed dilatancy of the salt, and II) less degraded, liquid hydrocarbons along grain boundaries in the vicinity of the anhydrite, interpreted to be incorporated into the salt in a subsequent deformation phase. Type II inclusions usually form arrays of isolated inclusions (liquid hydrocarbons, vapor, and aqueous phases in minor proportions) along grain boundaries of the recrystallized grains, presumably formed in a surface-energy controlled shrinking process from thin fluid films. Here, the contact with mobile grain boundaries promoted necking down and decomposition of multiphase inclusions. We present a model, which describes the dynamic behavior of liquid hydrocarbons in mobile grain boundaries after their enclosure into the salt layers. The model is based on numerous microanalytical methods, such as optical microscopy, fluorescence microscopy, cryo-SEM, and EDX. Schoenherr, J., et al. (2007), Limits to the sealing capacity of rock salt: A case study of the infra-Cambrian Ara Salt from the South Oman salt basin, AAPG Bulletin, 91(11), 1541-1557

Microstructural and Mechanical-Property Manipulation through Rapid Dendrite Growth and Undercooling in an Fe-based Multinary Alloy

PubMed Central

Ruan, Ying; Mohajerani, Amirhossein; Dao, Ming

2016-01-01

Rapid dendrite growth in single- or dual-phase multicomponent alloys can be manipulated to improve the mechanical properties of such metallic materials. Rapid growth of (αFe) dendrites was realized in an undercooled Fe-5Ni-5Mo-5Ge-5Co (wt.%) multinary alloy using the glass fluxing method. The relationship between rapid dendrite growth and the micro-/nano-mechanical properties of the alloy was investigated by analyzing the grain refinement and microstructural evolution resulting from the rapid dendrite growth. It was found that (αFe) dendrites grow sluggishly within a low but wide undercooling range. Once the undercooling exceeds 250 K, the dendritic growth velocity increases steeply until reaching a plateau of 31.8 ms−1. The increase in the alloy Vickers microhardness with increasing dendritic growth velocity results from the hardening effects of increased grain/phase boundaries due to the grain refinement, the more homogeneous distribution of the second phase along the boundaries, and the more uniform distribution of solutes with increased contents inside the grain, as verified also by nanohardness maps. Once the dendritic growth velocity exceeds ~8 ms−1, the rate of Vickers microhardness increase slows down significantly with a further increase in dendritic growth velocity, owing to the microstructural transition of the (αFe) phase from a trunk-dendrite to an equiaxed-grain microstructure. PMID:27539749

Microstructurally Based Prediction of High Strain Failure Modes in Crystalline Solids

DTIC Science & Technology

2016-07-05

SECURITY CLASSIFICATION OF: New three-dimensional dislocation-density based crystalline plasticity formulations was used with grain-boundary (GB...Army Research Office P.O. Box 12211 Research Triangle Park, NC 27709-2211 High strain-rate; failure, crsytalline plasticity , dislocation-density...Solids Report Title New three-dimensional dislocation-density based crystalline plasticity formulations was used with grain-boundary (GB) kinematic

Constraints on strain rate and fabric partitioning in ductilely deformed black quartzites (Badajoz-Córdoba Shear Zone, Iberian Massif)

NASA Astrophysics Data System (ADS)

Puelles, Pablo; Ábalos, Benito; Fernández-Armas, Sergio

2013-04-01

The Badajoz-Córdoba Shear Zone is a is 30-40 km wide and 400 km long, NW-SE trending structure located at the boundary between the Ossa-Morena and Central-Iberian Zones of the Iberian Massif. Two elongated domains can be differentiated inside: the Obejo-Valsequillo domain to the NE and the Ductile Shear Belt (DSB) to the SW. The former exhibits Precambrian to Cambrian volcano-sedimentary rocks unconformably overlaying a Neoproterozoic basement formed by the "Serie Negra". The latter, 5-15 km wide, is composed mainly of metamorphic tectonites including the "Serie Negra" and other units located structurally under it. The petrofabric of "Serie Negra" black quartzites from the DSB is analyzed in this study with the Electron Back-Scattered Diffraction technique (EBSD). Black quartzites represent originally siliceous, chemical-biochemical shallow-water marine deposits, currently composed almost exclusively of quartz and graphite. Macroscopically they exhibit an outstanding planolinear tectonic fabric. Petrographically, coarse- and fine-grained dynamically recrystallized quartz bands alternate. The former contain quartz grains with irregular shapes, mica inclusions and "pinning" grain boundaries. Oriented mica grains and graphite particles constrain irregular quartz grain shapes. Quartz ribbons with chessboard microstructures also occur, indicating recrystallization under elevated temperatures coeval with extreme stretching. Fine-grained recrystallized quartz bands are dominated by quartz grains with straight boundaries, triple junctions, a scarcer evidence of bulging, and a higher concentration of dispersed, minute graphite grains. Quartz lattice-preferred orientation (LPO) patterns permit to identify two well-developed maxima for [c] axes: one close to the Y structural direction and the other one around Z, and -axes girdles normal to Y and Z. Although both [c] axis maxima appear in the coarse- and fine-grained bands, subsets can be isolated with grain cluster orientations around Y and Z. Quartz [c]-axis orientations close to Y predominate in coarser-grained bands, whereas [c]-axes scatter around Z in fine-grained zones. A relationship between microstructure and crystal orientation can thus be unraveled. In both fabric types the asymmetry of the LPOs with respect to the external XYZ reference unravel non-coaxial deformation components. Microstructural and LPO evidences indicate that two intracrystalline quartz deformation modes have operated in the "Serie Negra" black quartzites in parallel domains interleaved at the mm- to cm scale. Unless one of them took place under higher-temperature conditions ({m} slip in the high-T amphibolite-facies) and is a relic feature, both modes should have operated simultaneously. Thus, high-temperature boundary migration and the dispersed inclusion pattern of small mica and graphite grains constrained the pinning grain boundary microstructures, the {m} intracrystalline slip, and the larger size of some quartz crystals. Simultaneously, a larger concentration of disseminated graphite led to formation of finer-grained quartz aggregates (due to grain growth) deformed by the (0001) intracrystalline slip systems, that dominate lower-T quartz plasticity (under greenschist- to amphibolite-facies conditions). Arguably, this intracrystalline slip system partitioning was initially constrained by primary variations in inclusion concentration. Likely, these induced a domainal variation in the rate of plastic strain accommodation that led to the current banded microstructural and fabric organization.

Localizing sources of acoustic emission during the martensitic transformation

NASA Astrophysics Data System (ADS)

Niemann, R.; Kopeček, J.; Heczko, O.; Romberg, J.; Schultz, L.; Fähler, S.; Vives, E.; Mañosa, L.; Planes, A.

2014-06-01

Acoustic avalanches are a general feature of solids under stress, e.g., evoked by external compression or arising from internal processes like martensitic phase transformations. From integral measurements, it is usually concluded that nucleation, phase boundary pinning, or interface incompatibilities during this first-order phase transition all may generate acoustic emission. This paper studies the local sources of acoustic emission to enlight the microscopic mechanisms. From two-dimensional spatially resolved acoustic emission measurement and simultaneous optical observation of the surface, we can identify microstructural events at the phase boundary that lead to acoustic emission. A resolution in the 100-μm range was reached for the location of acoustic emission sources on a coarse-grained Ni-Mn-Ga polycrystal. Both, the acoustic activity and the size distribution of the microstructural transformation events, exhibit power-law behavior. The origin of the acoustic emission are elastically incompatible areas, such as differently oriented martensitic plates that meet each other, lamellae growing up to grain boundaries, and grain boundaries in proximity to transforming grains. Using this result, we propose a model to explain the decrease of the critical exponent under a mechanical stress or magnetic field.

Unraveling irradiation induced grain growth with in situ transmission electron microscopy and coordinated modeling

DOE PAGES

Bufford, D. C.; Abdeljawad, F. F.; Foiles, S. M.; ...

2015-11-09

Here, nanostructuring has been proposed as a method to enhance radiation tolerance, but many metallic systems are rejected due to significant concerns regarding long term grain boundary and interface stability. This work utilized recent advancements in transmission electron microscopy (TEM) to quantitatively characterize the grain size, texture, and individual grain boundary character in a nanocrystalline gold model system before and after in situ TEM ion irradiation with 10 MeV Si. The initial experimental measurements were fed into a mesoscale phase field model, which incorporates the role of irradiation-induced thermal events on boundary properties, to directly compare the observed and simulatedmore » grain growth with varied parameters. The observed microstructure evolution deviated subtly from previously reported normal grain growth in which some boundaries remained essentially static. In broader terms, the combined experimental and modeling techniques presented herein provide future avenues to enhance quantification and prediction of the thermal, mechanical, or radiation stability of grain boundaries in nanostructured crystalline systems.« less

Effects of oxide distributed in grain boundaries on microstructure stability of nanocrystalline metals

NASA Astrophysics Data System (ADS)

Zhou, Kai; Li, Hui; Biao Pang, Jin; Wang, Zhu

2013-06-01

Nanocrystalline copper and zinc prepared by high-pressure compaction method have been studied by positron lifetime spectroscopy associated with X-ray diffraction. For nanocrystalline Cu, mean grain sizes of the samples decrease after being annealed at 900 °C and increase during aging at 180 °C, revealing that the atoms exchange between the two regions. The positron lifetime results indicate that the vacancy clusters formed in the annealing process are unstable and decomposed at the aging time below 6 hours. In addition, the partially oxidized surfaces of the nanoparticles hinder the grain growth during the ageing at 180 °C, and the vacancy clusters inside the disorder regions which are related to Cu2O need longer aging time to decompose. In the case of nanocrystalline Zn, the open volume defect (not larger than divacancy) is dominant according to the high relative intensity for the short positron lifetime (τ1). The oxide (ZnO) inside the grain boundaries has been found having an effect to hinder the decrease of average positron lifetime (τav) during the annealing, which probably indicates that the oxide stabilizes the microstructure of the grain boundaries. For both nanocrystalline copper and zinc, the oxides in grain boundaries enhance the thermal stability of the microstucture, in spite of their different crystal structures. This effect is very important for the nanocrystalline materials using as radiation resistant materials.

Microstructural Effects on Creep-Fatigue Life of Alloy 709

DOE Office of Scientific and Technical Information (OSTI.GOV)

McMurtrey, Michael; Carroll, Laura; Wright, Jill

Creep-fatigue tests were performed on plates of Alloy 709 from various heats and processing conditions, but often with inhomogeneous microstructures. After testing, metallographic analysis was performed and the specimens were generally found to either have a uniform grain size or a bimodal grain size distribution with either isolated or groups (bands) of large grains. Creep-fatigue life was characterized with respect to the length of the grain boundary perpendicular to the stress axis, and it was found that large grains (>400 μm) tended to be detrimental to creep-fatigue life, with the exception of elongated (parallel to the stress axis) grains andmore » some specimens that underwent additional annealing.« less

Superthermostability of nanoscale TIC-reinforced copper alloys manufactured by a two-step ball-milling process

NASA Astrophysics Data System (ADS)

Wang, Fenglin; Li, Yunping; Xu, Xiandong; Koizumi, Yuichiro; Yamanaka, Kenta; Bian, Huakang; Chiba, Akihiko

2015-12-01

A Cu-TiC alloy, with nanoscale TiC particles highly dispersed in the submicron-grained Cu matrix, was manufactured by a self-developed two-step ball-milling process on Cu, Ti and C powders. The thermostability of the composite was evaluated by high-temperature isothermal annealing treatments, with temperatures ranging from 727 to 1273 K. The semicoherent nanoscale TiC particles with Cu matrix, mainly located along the grain boundaries, were found to exhibit the promising trait of blocking grain boundary migrations, which leads to a super-stabilized microstructures up to approximately the melting point of copper (1223 K). Furthermore, the Cu-TiC alloys after annealing at 1323 K showed a slight decrease in Vickers hardness as well as the duplex microstructure due to selective grain growth, which were discussed in terms of hardness contributions from various mechanisms.

Microstructure and Current-Voltage Characteristics of Erbium Oxide Doped Multicomponent Zinc Oxide Varistors

NASA Astrophysics Data System (ADS)

Roy, Samarpita; Kundu Roy, Tapatee; Das, Debdulal

2018-03-01

The present work emphasizes the influence of Er2O3 addition on the microstructure and nonlinear current-voltage characteristics of ZnO based varistors prepared by mixing in a high energy ball mill followed by compaction and sintering at a temperature of 1100 °C for duration ranging from 0.5 to 8 h. Increasing sintering time is found to enhance the size of ZnO grains of the sintered pellets and thereby, degrades the electrical properties. However, Er2O3 addition retards the grain growth of ZnO due to the generation of secondary spinel phases (ErVO4 and Er-rich) at grain boundaries and triple points that restrict the grain boundary migration. Er2O3 modified ZnO varistor sintered at 1100 °C for 0.5 h exhibits considerably improved electrical property with nonlinear exponent and breakdown field of 27 and 3880 V cm-1, respectively.

Relations and interactions between twinning and grain boundaries in hexagonal close-packed structures

NASA Astrophysics Data System (ADS)

Barrett, Christopher Duncan

Improving the formability and crashworthiness of wrought magnesium alloys are the two biggest challenges in current magnesium technology. Magnesium is the best material candidate for enabling required improvements in fuel economy of combustion engines and increases in ranges of electric vehicles. In hexagonal closed-packed (HCP) structures, effects of grain size/morphology and crystallographic texture are particularly important. Prior research has established a general understanding of the dependences of strength and strain anisotropy on grain morphology and texture. Unfortunately, deformation, recrystallization, and grain growth strategies that control the microstructures and textures of cubic metals and alloys have not generally worked for HCPs. For example, in Magnesium, the deformation texture induced by primary forming operations (rolling, extrusion, etc.) is not randomized by recrystallization and may strengthen during grain growth. A strong texture reduces formability during secondary forming (stamping, bending, hemming etc.) Thus, the inability to randomize texture has impeded the implementation of magnesium alloys in engineering applications. When rare earth solutes are added to magnesium alloys, distinct new textures are derived. However, `rare earth texture' derivation remains insufficiently explained. Currently, it is hypothesized that unknown mechanisms of alloy processing are at work, arising from the effects of grain boundary intrinsic defect structures on microstructural evolution. This dissertation is a comprehensive attempt to identify formal methodologies of analyzing the behavior of grain boundaries in magnesium. We focus particularly on twin boundaries and asymmetric tilt grain boundaries using molecular dynamics. We begin by exploring twin nucleation in magnesium single crystals, elucidating effects of heterogeneities on twin nucleation and their relationships with concurrent slip. These efforts highlighted the necessity of imperfections to nucleate {10-12} twins. Subsequent studies encountered the importance of deformation faceting on the high mobility of {10-12} and stabilization of observed twin mode boundaries. Implementation of interfacial defect theory was necessary to decipher the complex mechanisms observed which govern the development of defects in grain boundaries, disconnection pile-up, facet nucleation, interfacial disclination nucleation, disconnection movements, disconnection transformation across interfacial disclinations, cross-faceting, and byproducts of interactions between lattice dislocations and grain boundaries.

Creep deformation of grain boundary in a highly crystalline SiC fibre.

PubMed

Shibayama, Tamaki; Yoshida, Yutaka; Yano, Yasuhide; Takahashi, Heishichiro

2003-01-01

Silicon carbide (SiC) matrix composites reinforced by SiC fibres (SiC/SiC composites) are currently being considered as alternative materials in high Ni alloys for high-temperature applications, such as aerospace components, gas-turbine energy-conversion systems and nuclear fusion reactors, because of their high specific strength and fracture toughness at elevated temperatures compared with monolithic SiC ceramics. It is important to evaluate the creep properties of SiC fibres under tensile loading in order to determine their usefulness as structural components. However, it would be hard to evaluate creep properties by monoaxial tensile properties when we have little knowledge on the microstructure of crept specimens, especially at the grain boundary. Recently, a simple fibre bend stress relaxation (BSR) test was introduced by Morscher and DiCarlo to address this problem. Interpretation of the fracture mechanism at the grain boundary is also essential to allow improvement of the mechanical properties. In this paper, effects of stress applied by BSR test on microstructural evolution in advanced SiC fibres, such as Tyranno-SA including small amounts of Al, are described and discussed along with the results of microstructure analysis on an atomic scale by using advanced microscopy.

Electron back-scattered diffraction and nanoindentation analysis of nanostructured Al tubes processed by multipass tubular-channel angular pressing

NASA Astrophysics Data System (ADS)

Mesbah, Mohsen; Faraji, Ghader; Bushroa, A. R.

2016-03-01

Microstructural evolution and mechanical properties of nanostructured 1060 aluminum alloy tubes processed by tubular-channel angular pressing (TCAP) process were investigated using electron back-scattered diffraction (EBSD), transmission electron microscopy (TEM) and nanoindentation analyzes. EBSD scans revealed a homogeneous ultrafine grained microstructure after the third passes of the TCAP process. Apart from that the mean grain sizes of the TCAP processed tubes were refined to 566 nm, 500 nm and 480 nm respectively after the first, second and third passes. The results showed that after the three TCAP passes, the grain boundaries with a high angle comprised 78% of all the boundaries. This is in comparison to the first pass processed sample that includes approximately 20% HAGBs. The TEM inspection afforded an appreciation of the role of very low-angle misorientation boundaries in the process of refining microstructure. Nanoindentation results showed that hardness was the smallest form of an unprocessed sample while the largest form of the processed sample after the three passes of TCAP indicated the highest resistant of the material. In addition, the module of elasticity of the TCAP processed samples was greater from that of the unprocessed sample.

Softening due to Grain Boundary Cavity Formation and its Competition with Hardening in Helium Implanted Nanocrystalline Tungsten

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cunningham, W. Streit; Gentile, Jonathan M.; El-Atwani, Osman

The unique ability of grain boundaries to act as effective sinks for radiation damage plays a significant role in nanocrystalline materials due to their large interfacial area per unit volume. Leveraging this mechanism in the design of tungsten as a plasma-facing material provides a potential pathway for enhancing its radiation tolerance under fusion-relevant conditions. In this study, we explore the impact of defect microstructures on the mechanical behavior of helium ion implanted nanocrystalline tungsten through nanoindentation. Softening was apparent across all implantation temperatures and attributed to bubble/cavity loaded grain boundaries suppressing the activation barrier for the onset of plasticity viamore » grain boundary mediated dislocation nucleation. An increase in fluence placed cavity induced grain boundary softening in competition with hardening from intragranular defect loop damage, thus signaling a new transition in the mechanical behavior of helium implanted nanocrystalline tungsten.« less

Softening due to Grain Boundary Cavity Formation and its Competition with Hardening in Helium Implanted Nanocrystalline Tungsten

DOE PAGES

Cunningham, W. Streit; Gentile, Jonathan M.; El-Atwani, Osman; ...

2018-02-13

The unique ability of grain boundaries to act as effective sinks for radiation damage plays a significant role in nanocrystalline materials due to their large interfacial area per unit volume. Leveraging this mechanism in the design of tungsten as a plasma-facing material provides a potential pathway for enhancing its radiation tolerance under fusion-relevant conditions. In this study, we explore the impact of defect microstructures on the mechanical behavior of helium ion implanted nanocrystalline tungsten through nanoindentation. Softening was apparent across all implantation temperatures and attributed to bubble/cavity loaded grain boundaries suppressing the activation barrier for the onset of plasticity viamore » grain boundary mediated dislocation nucleation. An increase in fluence placed cavity induced grain boundary softening in competition with hardening from intragranular defect loop damage, thus signaling a new transition in the mechanical behavior of helium implanted nanocrystalline tungsten.« less

A grain boundary damage model for delamination

NASA Astrophysics Data System (ADS)

Messner, M. C.; Beaudoin, A. J.; Dodds, R. H.

2015-07-01

Intergranular failure in metallic materials represents a multiscale damage mechanism: some feature of the material microstructure triggers the separation of grain boundaries on the microscale, but the intergranular fractures develop into long cracks on the macroscale. This work develops a multiscale model of grain boundary damage for modeling intergranular delamination—a failure of one particular family of grain boundaries sharing a common normal direction. The key feature of the model is a physically-consistent and mesh independent, multiscale scheme that homogenizes damage at many grain boundaries on the microscale into a single damage parameter on the macroscale to characterize material failure across a plane. The specific application of the damage framework developed here considers delamination failure in modern Al-Li alloys. However, the framework may be readily applied to other metals or composites and to other non-delamination interface geometries—for example, multiple populations of material interfaces with different geometric characteristics.

Computational and Experimental Studies of Microstructure-Scale Porosity in Metallic Fuels for Improved Gas Swelling Behavior

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mllett, Paul; McDeavitt, Sean; Deo, Chaitanya

This proposal will investigate the stability of bimodal pore size distributions in metallic uranium and uranium-zirconium alloys during sintering and re-sintering annealing treatments. The project will utilize both computational and experimental approaches. The computational approach includes both Molecular Dynamics simulations to determine the self-diffusion coefficients in pure U and U-Zr alloys in single crystals, grain boundaries, and free surfaces, as well as calculations of grain boundary and free surface interfacial energies. Phase-field simulations using MOOSE will be conducted to study pore and grain structure evolution in microstructures with bimodal pore size distributions. Experiments will also be performed to validate themore » simulations, and measure the time-dependent densification of bimodal porous compacts.« less

Microstructural stability of wrought, laser and electron beam glazed NARloy-Z alloy at elevated temperatures

NASA Technical Reports Server (NTRS)

Singh, J.; Jerman, G.; Bhat, B.; Poorman, R.

1993-01-01

Microstructure of wrought, laser, and electron-beam glazed NARloy-Z(Cu-3 wt.% Ag-0.5 wt.% Zr) was investigated for thermal stability at elevated temperatures (539 to 760 C (1,100 to 1,400 F)) up to 94 h. Optical and scanning electron microscopy and electron probe microanalysis were employed for studying microstructural evolution and kinetics of precipitation. Grain boundary precipitation and precipitate free zones (PFZ's) were observed in the wrought alloy after exposing to temperatures above 605 C (1,120 F). The fine-grained microstructure observed in the laser and electron-beam glazed NARloy-Z was much more stable at elevated temperatures. Microstructural changes correlated well with hardness measurements.

Microstructural Evolution of Ti-6Al-4V during High Strain Rate Conditions of Metal Cutting

NASA Technical Reports Server (NTRS)

Dong, Lei; Schneider, Judy

2009-01-01

The microstructural evolution following metal cutting was investigated within the metal chips of Ti-6Al-4V. Metal cutting was used to impose a high strain rate on the order of approx.10(exp 5)/s within the primary shear zone as the metal was removed from the workpiece. The initial microstructure of the parent material (PM) was composed of a bi-modal microstructure with coarse prior grains and equiaxed primary located at the boundaries. After metal cutting, the microstructure of the metal chips showed coarsening of the equiaxed primary grains and lamellar. These metallographic findings suggest that the metal chips experienced high temperatures which remained below the transus temperature.

Microstructure Evolution in Cut Metal Chips of Ti-6Al-4V

NASA Technical Reports Server (NTRS)

Dong, L.; Schneider, J. A.

2008-01-01

The microstructural evolution following metal cutting was investigated within metal chips of Ti-6Al-4V. Metal cutting was used to impose a high strain rate on the order of approx.10(exp 5)/s within the primary shear zone as the metal was removed from the workpiece. The initial microstructure of the parent material (PM) was composed of a bi-modal microstructure with coarse prior beta grains and equiaxed primary alpha located at the boundaries. After metal cutting, the microstructure of the metal chips showed coarsening of the equiaxed primary alpha grains and beta lamellar. These metallographic findings suggest that the metal chips experienced high temperatures which remained below the beta transus temperature.

Atomic scale characterization of white etching area and its adjacent matrix in a martensitic 100Cr6 bearing steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Y.J., E-mail: y.li@mpie.de

Atom probe tomography was employed to characterize the microstructure and C distribution in the white etching area (WEA) of a martensitic 100Cr6 bearing steel subjected to rolling contact fatigue. Different from its surrounding matrix where a plate-like martensitic structure prevails, the WEA exhibits equiaxed grains with a uniform grain size of about 10 nm. Significant C grain boundary enrichment (>7.5at.%) and an overall higher C concentration than the nominal value are observed in the WEA. These results suggest that the formation of WEA results from severe local plastic deformation that causes dissolution of carbides and the redistribution of C. -more » Highlights: •APT has been applied to characterize the microstructure of white etching area (WEA). •Quantitative analyses of C distribution indicate that carbides are dissolved on the WEA. •WEA contains equiaxed grains with a uniform grain size of 10 nm. •C segregation at grain boundaries stabilizes the nanosized grain structure. •Formation of WEA is explained by severe local plastic deformation introduced by cyclic contact loading.« less

Dielectric and magnetic studies of BaTi0.5Fe0.5O3 ceramic materials, synthesized by solid state sintering.

PubMed

Samuvel, K; Ramachandran, K

2015-02-05

A comparative study of the surface morphology, dielectric and magnetic properties of the BaTi0.5Fe0.5O3 (BTFO) ceramics materials. This has been carried out by synthesizing the samples in different routes. BTFO samples have shown single phased 12R type hexagonal structure with R3m, P4mm space group. Interfacial effects on the dielectric properties of the samples have been understood by Cole-Cole plots in complex impedance and modulus formalism. It has been identified that huge dielectric constant (10(3)-10(6)) at lower frequencies is largely contributed by the heterogeneous electronic microstructure at the interfaces of grains. Modulus formalism has identified the effects of both grain and grain boundary microstructure on the dielectric properties, particularly in chemical routed samples. The order of grain boundary resistivity suggests the semiconductor/insulator class of the material. The grain boundary resistivity of the mechanical alloyed samples is remarkably lower than the solid state and chemical routed samples. Few samples have of the samples have exhibited signature of ferromagnetism at the room temperature. Copyright © 2014 Elsevier B.V. All rights reserved.

Subsurface imaging of grain microstructure using picosecond ultrasonics

DOE PAGES

Khafizov, M.; Pakarinen, J.; He, L.; ...

2016-04-21

We report on imaging subsurface grain microstructure using picosecond ultrasonics. This approach relies on elastic anisotropy of crystalline materials where ultrasonic velocity depends on propagation direction relative to the crystal axes. Picosecond duration ultrasonic pulses are generated and detected using ultrashort light pulses. In materials that are transparent or semitransparent to the probe wavelength, the probe monitors GHz Brillouin oscillations. The frequency of these oscillations is related to the ultrasonic velocity and the optical index of refraction. Ultrasonic waves propagating across a grain boundary experience a change in velocity due to a change in crystallographic orientation relative to the ultrasonicmore » propagation direction. This change in velocity is manifested as a change in the Brillouin oscillation frequency. Using the ultrasonic propagation velocity, the depth of the interface can be determined from the location in time of the transition in oscillation frequency. An image of the grain boundary is obtained by scanning the beam along the surface. We demonstrate this volumetric imaging capability using a polycrystalline UO 2 sample. As a result, cross section liftout analysis of the grain boundaries using electron microscopy were used to verify our imaging results.« less

Heterogeneous dislocation loop formation near grain boundaries in a neutron-irradiated commercial FeCrAl alloy

NASA Astrophysics Data System (ADS)

Field, Kevin G.; Briggs, Samuel A.; Hu, Xunxiang; Yamamoto, Yukinori; Howard, Richard H.; Sridharan, Kumar

2017-01-01

FeCrAl alloys are an attractive class of materials for nuclear power applications because of their increased environmental compatibility compared with more traditional nuclear materials. Preliminary studies into the radiation tolerance of FeCrAl alloys under accelerated neutron testing between 300 and 400 °C have shown post-irradiation microstructures containing dislocation loops and a Cr-rich α‧ phase. Although these initial studies established the post-irradiation microstructures, there was little to no focus on understanding the influence of pre-irradiation microstructures on this response. In this study, a well-annealed commercial FeCrAl alloy, Alkrothal 720, was neutron irradiated to 1.8 displacements per atom (dpa) at 382 °C and then the effect of random high-angle grain boundaries on the spatial distribution and size of a〈100〉 dislocation loops, a/2〈111〉 dislocation loops, and black dot damage was analyzed using on-zone scanning transmission electron microscopy. Results showed a clear heterogeneous dislocation loop formation with a/2〈111〉 dislocation loops showing an increased number density and size, black dot damage showing a significant number density decrease, and a〈100〉 dislocation loops exhibiting an increased size in the vicinity of the grain boundary. These results suggest the importance of the pre-irradiation microstructure and, specifically, defect sink density spacing to the radiation tolerance of FeCrAl alloys.

Origin of electrically heterogeneous microstructure in CuO from scanning tunneling spectroscopy study

NASA Astrophysics Data System (ADS)

Sarkar, Sudipta; Jana, Pradip Kumar; Chaudhuri, B. K.

2008-04-01

We report electronic structure of the grains and grain boundaries (GBs) of the high permittivity (κ˜104) ceramic CuO from scanning tunneling spectroscopy (STS) studies. The p-type semiconducting character of the CuO grains and insulating behavior of the corresponding GBs, observed from STS studies, have been explained. This type of electrically inhomogeneous microstructure leads to the formation of barrier layer capacitance elements in CuO and, hence, provides an explanation of the colossal-κ response exhibited by CuO.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bagri, Akbar; Hanson, John P.; Lind, J. P.

We use high-energy X-ray diffraction microscopy (HEDM) to characterize the microstructure of Ni-base alloy 725. HEDM is a non-destructive technique capable of providing three-dimensional reconstructions of grain shapes and orientations in polycrystals. The present analysis yields the grain size distribution in alloy 725 as well as the grain boundary character distribution (GBCD) as a function of lattice misorientation and boundary plane normal orientation. We find that the GBCD of Ni-base alloy 725 is similar to that previously determined in pure Ni and other fcc-base metals. We find an elevated density of Σ9 and Σ3 grain boundaries. We also observe amore » preponderance of grain boundaries along low-index planes, with those along (1 1 1) planes being the most common, even after Σ3 twins have been excluded from the analysis.« less

Grain boundary engineering to control the discontinuous precipitation in multicomponent U10Mo alloy

DOE PAGES

Devaraj, Arun; Kovarik, Libor; Kautz, Elizabeth; ...

2018-03-30

Here, we demonstrate here that locally stabilized structure and compositional segregation at grain boundaries in a complex multicomponent alloy can be modified using high temperature homogenization treatment to influence the kinetics of phase transformations initiating from grain boundaries during subsequent low temperature annealing. Using aberration-corrected scanning transmission electron microscopy and atom probe tomography of a model multicomponent metallic alloy —uranium-10 wt% molybdenum (U-10Mo) a nuclear fuel, that is highly relevant to worldwide nuclear non-proliferation efforts, we demonstrate the ability to change the structure and compositional segregation at grain boundary, which then controls the subsequent discontinuous precipitation kinetics during sub-eutectoid annealing.more » A change in grain boundary from one characterized by segregation of Mo and impurities at grain boundary to a phase boundary with a distinct U 2MoSi 2C wetting phase precipitates introducing Ni and Al rich interphase complexions caused a pronounced reduction in area fraction of subsequent discontinuous precipitation. The broader implication of this work is in highlighting the role of grain boundary structure and composition in metallic alloys on dictating the fate of grain boundary initiated phase transformations like discontinuous precipitation or cellular transformation. This work highlights a new pathway to tune the grain boundary structure and composition to tailor the final microstructure of multicomponent metallic alloys.« less

Grain boundary engineering to control the discontinuous precipitation in multicomponent U10Mo alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Devaraj, Arun; Kovarik, Libor; Kautz, Elizabeth

Here, we demonstrate here that locally stabilized structure and compositional segregation at grain boundaries in a complex multicomponent alloy can be modified using high temperature homogenization treatment to influence the kinetics of phase transformations initiating from grain boundaries during subsequent low temperature annealing. Using aberration-corrected scanning transmission electron microscopy and atom probe tomography of a model multicomponent metallic alloy —uranium-10 wt% molybdenum (U-10Mo) a nuclear fuel, that is highly relevant to worldwide nuclear non-proliferation efforts, we demonstrate the ability to change the structure and compositional segregation at grain boundary, which then controls the subsequent discontinuous precipitation kinetics during sub-eutectoid annealing.more » A change in grain boundary from one characterized by segregation of Mo and impurities at grain boundary to a phase boundary with a distinct U 2MoSi 2C wetting phase precipitates introducing Ni and Al rich interphase complexions caused a pronounced reduction in area fraction of subsequent discontinuous precipitation. The broader implication of this work is in highlighting the role of grain boundary structure and composition in metallic alloys on dictating the fate of grain boundary initiated phase transformations like discontinuous precipitation or cellular transformation. This work highlights a new pathway to tune the grain boundary structure and composition to tailor the final microstructure of multicomponent metallic alloys.« less

Observations of ’Economical’ Fixed Prosthodontic Alloys,

DTIC Science & Technology

1982-01-01

Office) 15. SECURITY CLASS. (of this ,.portj Ia. OS7RI~fl3 ~TATM~T1of5sA. DECLASSIFICATION/OO44GRAUTIV S Unlimited 17. 0137 PI3UT10ON STATEMENT (of the...however, the silver-palladium and silver-indium materials require ~DA~3 47 EOfl4O tO’/SfOBOLTE UNCLASSIFIED 8 2’ 02 R -/ SECURITY CLASSIFICATION OF...ous grain boundary netowrk , whereas those of Salivan revealed large grains, discontinuous grain boundaries and prominent subgrains. Microstructures

Microstructural Evolution during Mid-Crustal Shear Zone Thickening and Thinning, Mount Irene Detachment Zone, Fiordland, New Zealand

NASA Astrophysics Data System (ADS)

Negrini, M.; Smith, S. A. F.; Scott, J.; Rooney, J. S.; Demurtas, M.

2016-12-01

Recent work has shown that ductile shear zones experience cyclic variations in stress and strain rate due to, for example, elastic loading from earthquake slip on brittle faults or the presence of rigid particles and asperities within the shear zone. Such non-steady state flow conditions can promote microstructural changes including a decrease in grain sizes followed by a switch in the main deformation mechanisms. Understanding the microstructural changes that occur during non steady-state deformation is therefore critical in evaluating shear zone rheology. The Mount Irene shear zone formed during Cretaceous extension in the middle crust and was active at temperatures of 600°C and pressures of 6 kbar. The shear zone localized in a basal calcite marble layer typically 3-5 m thick containing hundreds of thin (mm-cm) calc-silicate bands that are now parallel to the shear zone boundaries. The lower boundary of the shear zone preserves meter-scale undulations that cause the shear zone to be squeezed in to regions that are <1.5 m thick. The calc-silicate bands act as "flow markers" and allow individual shear zone layers to be traced continuously through thick and thin regions, implying that the mylonites experienced cyclic variations in stress and strain rate. Calc-mylonite samples collected from the same layer close to the base of the shear zone reveal that layer thinning was accompanied by progressive microstructural changes including intense twinning, stretching and flattening of large calcite porphyroclasts as well as the development of interconnected networks of recrystallized calcite aggregates. EBSD analysis shows that the recrystallized aggregates contain polygonal calcite grains with microstructures (e.g. grain quadruple junctions) similar to those reported for neighbor-switching processes associated with grain boundary sliding and superplasticity. Ongoing and future work will utilize samples from across the full thickness of the shear zone to determine key microstructural changes and deformation mechanisms that accommodated shear zone thinning and thickening during non-steady state deformation.

Mixed conduction and grain boundary effect in lithium niobate under high pressure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Qinglin; Center for High Pressure Science and Technology Advanced Research, Changchun 130012; Liu, Cailong

2015-03-30

The charge transport behavior of lithium niobate has been investigated by in situ impedance measurement up to 40.6 GPa. The Li{sup +} ionic conduction plays a dominant role in the transport process. The relaxation process is described by the Maxwell-Wagner relaxation arising at the interfaces between grains and grain boundaries. The grain boundary microstructure rearranges after the phase transition, which improves the bulk dielectric performance. The theoretical calculations show that the decrease of bulk permittivity with increasing pressure in the Pnma phase is caused by the pressure-induced enhancement of electron localization around O atoms, which limits the polarization of Nb-O electricmore » dipoles.« less

In situ electron backscatter diffraction investigation of recrystallization in a copper wire.

PubMed

Brisset, François; Helbert, Anne-Laure; Baudin, Thierry

2013-08-01

The microstructural evolution of a cold drawn copper wire (reduction area of 38%) during primary recrystallization and grain growth was observed in situ by electron backscatter diffraction. Two thermal treatments were performed, and successive scans were acquired on samples undergoing heating from ambient temperature to a steady state of 200°C or 215°C. During a third in situ annealing, the temperature was continuously increased up to 600°C. Nuclei were observed to grow at the expense of the deformed microstructure. This growth was enhanced by the high stored energy difference between the nuclei and their neighbors (driving energy in recrystallization) and by the presence of high-angle grain boundaries of high mobility. In the early stages of growth, the nuclei twin and the newly created orientations continue to grow to the detriment of the strained copper. At high temperatures, the disappearance of some twins was evidenced by the migration of the incoherent twin boundaries. Thermal grooving of grain boundaries is observed at these high temperatures and affects the high mobile boundaries but tends to preserve the twin boundaries of lower energy. Thus, grooving may contribute to the twin vanishing.

Evidence for Seismic and Aseismic Slip along a Foreland Thrust Fault, Southern Appalachians

NASA Astrophysics Data System (ADS)

Newman, J.; Wells, R. K.; Holyoke, C. W.; Wojtal, S. F.

2013-12-01

Studies of deformation along ancient thrust faults form the basis for much of our fundamental understanding of fault and shear zone processes. These classic studies interpreted meso- and microstructures as formed during aseismic creep. Recent experimental studies, and studies of naturally deformed rocks in seismically active regions, reveal similar microstructures to those observed locally in a carbonate foreland thrust from the southern Appalachians, suggesting that this thrust fault preserves evidence of both seismic and aseismic deformation. The Copper Creek thrust, TN, accommodated 15-20 km displacement, at depths of 4-6 km, as estimated from balanced cross-sections. At the Diggs Gap exposure of the Copper Creek thrust, an approximately 2 cm thick, vein-like shear zone separates shale layers in the hanging wall and footwall. The shear zone is composed of anastomosing layers of ultrafine-grained calcite and/or shale as well as aggregate clasts of ultrafine-grained calcite or shale. The boundary between the shear zone and the hanging wall is sharp, with slickensides along the boundary, parallel to the shear zone movement direction. A 350 μm-thick layer of ultrafine-grained calcite separates the shear zone and the footwall. Fault parallel and perpendicular calcite veins are common in the footwall and increase in density towards the shear zone. Microstructures within the vein-like shear zone that are similar to those observed in experimental studies of unstable slip include: ultrafine-grained calcite (~0.34 μm), nano-aggregate clasts (100-300 nm), injection structures, and vein-wrapped and matrix-wrapped clasts. Not all structures within the shear zone and ultrafine-grained calcite layer suggest seismic slip. Within the footwall veins and calcite aggregate clasts within the shear zone, pores at twin-twin intersections suggest plasticity-induced fracturing as the main mechanism for grain size reduction. Interpenetrating grain boundaries in ultrafine-grained calcite and a lack of a lattice preferred orientation suggest ultrafine-grained calcite deformed by diffusion creep accommodated grain boundary sliding. These structures suggest a strain-rate between 10-15 - 10-11 s-1, using calcite flow laws at temperatures 150-250 °C. Microstructures suggest both seismic and aseismic slip along this ancient fault zone. During periods of aseismic slip, deformation is accommodated by plasticity-induced fracturing and diffusion creep. Calcite veins suggest an increase in pore-fluid pressure, contributing to fluidized and unstable flow, but also providing the calcite that deformed by diffusion creep during aseismic creep.

Nanocrystalline Al7075 + 1 wt % Zr Alloy Prepared Using Mechanical Milling and Spark Plasma Sintering

PubMed Central

Málek, Přemysl; Minárik, Peter; Chráska, Tomáš; Novák, Pavel; Průša, Filip

2017-01-01

The microstructure, phase composition, and microhardness of both gas-atomized and mechanically milled powders of the Al7075 + 1 wt % Zr alloy were investigated. The gas-atomized powder exhibited a cellular microstructure (grain size of a few µm) with layers of intermetallic phases along the cell boundaries. Mechanical milling (400 revolutions per minute (RPM)/8 h) resulted in a grain size reduction to the nanocrystalline range (20 to 100 nm) along with the dissolution of the intermetallic phases. Milling led to an increase in the powder’s microhardness from 97 to 343 HV. Compacts prepared by spark plasma sintering (SPS) exhibited negligible porosity. The grain size of the originally gas-atomized material was retained, but the continuous layers of intermetallic phases were replaced by individual particles. Recrystallization led to a grain size increase to 365 nm in the SPS compact prepared from the originally milled powder. Small precipitates of the Al3Zr phase were observed in the SPS compacts, and they are believed to be responsible for the retainment of the sub-microcrystalline microstructure during SPS. A more intensive precipitation in this SPS compact can be attributed to a faster diffusion due to a high density of dislocations and grain boundaries in the milled powder. PMID:28930192

Effect of Trace Levels of Si on Microstructure and Grain Boundary Segregation in DOP-26 Iridium Alloy

NASA Astrophysics Data System (ADS)

Pierce, Dean; Muralidharan, Govindarajan; Heatherly, Lee; Fox, Ethan

2018-03-01

The thermodynamics and kinetics of Silicon (Si) segregation to grain boundaries in Iridium alloy DOP-26 with added trace levels of Si of 6, 11, 29, and 36 wppm was studied by Auger Electron Spectroscopy. The four alloys were annealed at 1500 or 1535 °C for 19 or 76 hours followed by cooling at three different rates. Si enrichment at the grain boundaries (GB) increased with increasing bulk Si content, with the grain boundary Si enrichment factors ranging from 62 to 344, depending on the bulk Si content and the cooling rate. Grain boundary Si contents increased with decreasing cooling rate in all alloys, indicating that Si GB segregation is influenced by both thermodynamic and kinetic factors in the alloys and temperature ranges of the study. A Langmuir-McLean isotherm-based model was successfully used to predict the temperature dependence of GB Si segregation in DOP-26 alloys with Si additions and estimate the temperature independent free energy of Si segregation to grain boundaries in DOP-26.

On the role of the grain size in the magnetic behavior of sintered permanent magnets

NASA Astrophysics Data System (ADS)

Efthimiadis, K. G.; Ntallis, N.

2018-02-01

In this work the finite elements method is used to simulate, by micromagnetic modeling, the magnetic behavior of sintered anisotropic magnets. Hysteresis loops were simulated for different grain sizes in an oriented multigrain sample. By keeping out other parameters that contribute to the magnetic microstructure, such as the sample size, the grain morphology and the grain boundaries mismatch, it has been found that the grain size affects the magnetic properties only if the grains are exchange-decoupled. In this case, as the grain size decreases, a decrease in the nucleation field of a reverse magnetic domain is observed and an increase in the coercive field due to the pinning of the magnetic domain walls at the grain boundaries.

Microstructure design for fast oxygen conduction

DOE PAGES

Aidhy, Dilpuneet S.; Weber, William J.

2015-11-11

Research from the last decade has shown that in designing fast oxygen conducting materials for electrochemical applications has largely shifted to microstructural features, in contrast to material-bulk. In particular, understanding oxygen energetics in heterointerface materials is currently at the forefront, where interfacial tensile strain is being considered as the key parameter in lowering oxygen migration barriers. Nanocrystalline materials with high densities of grain boundaries have also gathered interest that could possibly allow leverage over excess volume at grain boundaries, providing fast oxygen diffusion channels similar to those previously observed in metals. In addition, near-interface phase transformations and misfit dislocations aremore » other microstructural phenomenon/features that are being explored to provide faster diffusion. In this review, the current understanding on oxygen energetics, i.e., thermodynamics and kinetics, originating from these microstructural features is discussed. Moreover, our experimental observations, theoretical predictions and novel atomistic mechanisms relevant to oxygen transport are highlighted. In addition, the interaction of dopants with oxygen vacancies in the presence of these new microstructural features, and their future role in the design of future fast-ion conductors, is outlined.« less

TA [B] Predicting Microstructure-Creep Resistance Correlation in High Temperature Alloys over Multiple Time Scales

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tomar, Vikas

2017-03-06

DoE-NETL partnered with Purdue University to predict the creep and associated microstructure evolution of tungsten-based refractory alloys. Researchers use grain boundary (GB) diagrams, a new concept, to establish time-dependent creep resistance and associated microstructure evolution of grain boundaries/intergranular films GB/IGF controlled creep as a function of load, environment, and temperature. The goal was to conduct a systematic study that includes the development of a theoretical framework, multiscale modeling, and experimental validation using W-based body-centered-cubic alloys, doped/alloyed with one or two of the following elements: nickel, palladium, cobalt, iron, and copper—typical refractory alloys. Prior work has already established and validated amore » basic theory for W-based binary and ternary alloys; the study conducted under this project extended this proven work. Based on interface diagrams phase field models were developed to predict long term microstructural evolution. In order to validate the models nanoindentation creep data was used to elucidate the role played by the interface properties in predicting long term creep strength and microstructure evolution.« less

Micro-mechanisms of Surface Defects Induced on Aluminum Alloys during Plastic Deformation at Elevated Temperatures

NASA Astrophysics Data System (ADS)

Gali, Olufisayo A.

Near-surface deformed layers developed on aluminum alloys significantly influence the corrosion and tribological behavior as well as reduce the surface quality of the rolled aluminum. The evolution of the near-surface microstructures induced on magnesium containing aluminum alloys during thermomechanical processing has been investigated with the aim generating an understanding of the influence of individual forming parameters on its evolution and examine the microstructure of the roll coating induced on the mating steel roll through material transfer during rolling. The micro-mechanisms related to the various features of near-surface microstructure developed during tribological conditions of the simulated hot rolling process were identified. Thermomechanical processing experiments were performed with the aid of hot rolling (operating temperature: 550 to 460 °C, 4, 10 and 20 rolling pass schedules) and hot forming (operating temperature: 350 to 545 °C, strain rate: 4 x 10-2 s-1) tribo-simulators. The surface, near-surface features and material transfer induced during the elevated temperature plastic deformation were examined and characterized employing optical interferometry, SEM/EDS, FIB and TEM. Near-surface features characterized on the rolled aluminum alloys included; cracks, fractured intermetallic particles, aluminum nano-particles, oxide decorated grain boundaries, rolled-in oxides, shingles and blisters. These features were related to various individual rolling parameters which included, the work roll roughness, which induced the formation of shingles, rolling marks and were responsible for the redistribution of surface oxide and the enhancements of the depth of the near-surface damage. The enhanced stresses and strains experienced during rolling were related to the formation and propagation of cracks, the nanocrystalline structure of the near-surface layers and aluminum nano-particles. The mechanism of the evolution of the near-surface microstructure were determined to include grain boundary sliding which induced the cracks at the surface and subsurface of the alloy, magnesium diffusion to free surfaces, crack propagation from shear stresses and the shear strains inducing the nanocrystalline grain structure, the formation of shingles by the shear deformation of micro-wedges induced by the work roll grooves, and the deformation of this oxide covered micro-wedges inducing the rolled-in oxides. Magnesium diffusion to free surfaces was identified as inducing crack healing due to the formation of MgO within cracks and was responsible for the oxide decorated grain boundaries. An examination of the roll coating revealed a complex layered microstructure that was induced through tribo-chemical and mechanical entrapment mechanisms. The microstructure of the roll coating suggested that the work roll material and the rolled aluminum alloy were essential in determining its composition and structure. Subsequent hot forming processes revealed the rich oxide-layer of the near-surface microstructure was beneficial for reducing the coefficient of friction during tribological contact with the steel die. Damage to the microstructure include cracks induced from grain boundary sliding of near-surface grains and the formation of oxide fibres within cracks of the near-surface deformed layers.

Grain boundary diffusion of Dy films prepared by magnetron sputtering for sintered Nd–Fe–B magnets

NASA Astrophysics Data System (ADS)

Chen, W.; Luo, J. M.; Guan, Y. W.; Huang, Y. L.; Chen, M.; Hou, Y. H.

2018-05-01

Dy films, deposited on the surface of sintered Nd–Fe–B magnets by magnetron sputtering, were employed for grain boundary diffusion source. High coercivity sintered Nd–Fe–B magnets were successfully prepared. Effects of sputtering power and grain boundary diffusion processes (GBDP) on the microstructure and magnetic properties were investigated in detail. The dense and uniform Dy films were beneficial to prepare high coercivity magnets by GBDP. The maximum coercivity value of 1189 kA m‑1 could be shown, which was an amplification of 22.3%, compared with that of as-prepared Nd–Fe–B magnet. Furthermore, the improved remanence and maximum energy product were also achieved through tuning grain boundary diffusion processes. Our results demonstrated that the formation of (Nd, Dy)2Fe14B shell surrounding Nd2Fe14B grains and fine, uniform and continuous intergranular RE-rich phases jointly contribute to the improved coercivity.

Deformation mechanisms and grain size evolution in the Bohemian granulites - a computational study

NASA Astrophysics Data System (ADS)

Maierova, Petra; Lexa, Ondrej; Jeřábek, Petr; Franěk, Jan; Schulmann, Karel

2015-04-01

A dominant deformation mechanism in crustal rocks (e.g., dislocation and diffusion creep, grain boundary sliding, solution-precipitation) depends on many parameters such as temperature, major minerals, differential stress, strain rate and grain size. An exemplary sequence of deformation mechanisms was identified in the largest felsic granulite massifs in the southern Moldanubian domain (Bohemian Massif, central European Variscides). These massifs were interpreted to result from collision-related forced diapiric ascent of lower crust and its subsequent lateral spreading at mid-crustal levels. Three types of microstructures were distinguished. The oldest relict microstructure (S1) with large grains (>1000 μm) of feldspar deformed probably by dislocation creep at peak HT eclogite facies conditions. Subsequently at HP granulite-facies conditions, chemically- and deformation- induced recrystallization of feldspar porphyroclasts led to development of a fine-grained microstructure (S2, ~50 μm grain size) indicating deformation via diffusion creep, probably assisted by melt-enhanced grain-boundary sliding. This microstructure was associated with flow in the lower crust and/or its diapiric ascent. The latest microstructure (S3, ~100 μm grain size) is related to the final lateral spreading of retrograde granulites, and shows deformation by dislocation creep at amphibolite-facies conditions. The S2-S3 switch and coarsening was interpreted to be related with a significant decrease in strain rate. From this microstructural sequence it appears that it is the grain size that is critically linked with specific mechanical behavior of these rocks. Thus in this study, we focused on the interplay between grain size and deformation with the aim to numerically simulate and reinterpret the observed microstructural sequence. We tested several different mathematical descriptions of the grain size evolution, each of which gave qualitatively different results. We selected the two most elaborated and at the same time the most promising descriptions: thermodynamics-based models with and without Zener pinning. For conditions compatible with the S1 and S2 microstructures (~800 °C and strain rate ~10-13 s-1), the calculated stable grain sizes are ~30 μm and >300 μm in the models with and without Zener pinning, respectively. This is in agreement with the contrasting grain sizes associated with S1 and S2 microstructures implying that mainly chemically induced recrystallization of S1 feldspar porphyroclasts must had played a fundamental role in the transition into the diffusion creep. The model with pinning also explains only minor changes of mean grain size associated with S2 microstructure. The S2-S3 switch from the diffusion to dislocation creep is difficult to explain when assuming reasonable temperature and strain rate (or stress). However, a simple incorporation of the effect of melt solidification into the model with pinning can mimic this observed switch. Besides the above mentioned simple models with prescribed temperature and strain rate, we implemented the grain size evolution laws into in a 2D thermo-mechanical model setup, where stress, strain rate and temperature evolve in a more natural manner. This setup simulates a collisional evolution of an orogenic root with anomalous lower crust. The lower-crustal material is a source region for diapirs and it deforms via a combination of dislocation and grain-size-sensitive creeps. We tested the influence of selected parameters in the flow laws and in the grain-size evolution laws on the shape and other characteristics of the growing diapirs. The outputs of our simulations were then compared with the geological record from the Moldanubian granulite massifs.

Effect of Composition and Deformation on Coarse-Grained Austenite Transformation in Nb-Mo Microalloyed Steels

NASA Astrophysics Data System (ADS)

Isasti, N.; Jorge-Badiola, D.; Taheri, M. L.; López, B.; Uranga, P.

2011-12-01

Thermomechanical processing of microalloyed steels containing niobium can be performed to obtain deformed austenite prior to transformation. Accelerated cooling can be employed to refine the final microstructure and, consequently, to improve both strength and toughness. This general rule is fulfilled if the transformation occurs on a quite homogeneous austenite microstructure. Nevertheless, the presence of coarse austenite grains before transformation in different industrial processes is a usual source of concern, and regarding toughness, the coarsest high-angle boundary units would determine its final value. Sets of deformation dilatometry tests were carried out using three 0.06 pct Nb microalloyed steels to evaluate the effect of Mo alloying additions (0, 0.16, and 0.31 pct Mo) on final transformation from both recrystallized and unrecrystallized coarse-grained austenite. Continuous cooling transformation (CCT) diagrams were created, and detailed microstructural characterization was achieved through the use of optical microscopy (OM), field emission gun scanning electron microscopy (FEGSEM), and electron backscattered diffraction (EBSD). The resultant microstructures ranged from polygonal ferrite (PF) and pearlite (P) at slow cooling ranges to bainitic ferrite (BF) accompanied by martensite (M) for fast cooling rates. Plastic deformation of the parent austenite accelerated both ferrite and bainite transformation, moving the CCT curves to higher temperatures and shorter times. However, an increase in the final heterogeneity was observed when BF packets were formed, creating coarse high-angle grain boundary units.

Simulation of xenon, uranium vacancy and interstitial diffusion and grain boundary segregation in UO 2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Andersson, Anders D.; Tonks, Michael R.; Casillas, Luis

2014-10-31

In light water reactor fuel, gaseous fission products segregate to grain boundaries, resulting in the nucleation and growth of large intergranular fission gas bubbles. Based on the mechanisms established from density functional theory (DFT) and empirical potential calculations 1, continuum models for diffusion of xenon (Xe), uranium (U) vacancies and U interstitials in UO 2 have been derived for both intrinsic conditions and under irradiation. Segregation of Xe to grain boundaries is described by combining the bulk diffusion model with a model for the interaction between Xe atoms and three different grain boundaries in UO 2 ( Σ5 tilt, Σ5more » twist and a high angle random boundary),as derived from atomistic calculations. All models are implemented in the MARMOT phase field code, which is used to calculate effective Xe and U diffusivities as well as redistribution for a few simple microstructures.« less

Microstructure and dielectric properties of (Nb + In) co-doped rutile TiO2 ceramics

NASA Astrophysics Data System (ADS)

Li, Jinglei; Li, Fei; Zhuang, Yongyong; Jin, Li; Wang, Linghang; Wei, Xiaoyong; Xu, Zhuo; Zhang, Shujun

2014-08-01

The (Nb + In) co-doped TiO2 ceramics recently attracted considerable attention due to their colossal dielectric permittivity (CP) (˜100,000) and low dielectric loss (˜0.05). In this research, the 0.5 mol. % In-only, 0.5 mol. % Nb-only, and 0.5-7 mol. % (Nb + In) co-doped TiO2 ceramics were synthesized by standard conventional solid-state reaction method. Microstructure studies showed that all samples were in pure rutile phase. The Nb and In ions were homogeneously distributed in the grain and grain boundary. Impedance spectroscopy and I-V behavior analysis demonstrated that the ceramics may compose of semiconducting grains and insulating grain boundaries. The high conductivity of grain was associated with the reduction of Ti4+ ions to Ti3+ ions, while the migration of oxygen vacancy may account for the conductivity of grain boundary. The effects of annealing treatment and bias filed on electrical properties were investigated for co-doped TiO2 ceramics, where the electric behaviors of samples were found to be susceptible to the annealing treatment and bias field. The internal-barrier-layer-capacitance mechanism was used to explain the CP phenomenon, the effect of annealing treatment and nonlinear I-V behavior for co-doped rutile TiO2 ceramics. Compared with CaCu3Ti4O12 ceramics, the high activation energy of co-doped rutile TiO2 (3.05 eV for grain boundary) was thought to be responsible for the low dielectric loss.

EBSD Study on Grain Boundary and Microtexture Evolutions During Friction Stir Processing of A413 Cast Aluminum Alloy

NASA Astrophysics Data System (ADS)

Shamanian, Morteza; Mostaan, Hossein; Safari, Mehdi; Szpunar, Jerzy A.

2016-07-01

The as-cast Al alloys contain heterogeneous distributions of non-deforming particles due to non-equilibrium solidification effects. Therefore, these alloys have poor tribological and mechanical behaviors. It is well known that using friction stir processing (FSP), very fine microstructure is created in the as-cast Al alloys, while their wear resistance can be improved. In this research work, FSP is used to locally refine a surface layer of the coarse as-cast microstructure of cast A413 Al alloy. The main objective of this study is to investigate the effect of FSP on microstructure and microtexture evolutions in A413 cast Al alloy. The grain boundary character distribution, grain structure, and microtexture evolutions in as-cast and friction stir processed A413 Al alloy are analyzed by electron back scatter diffraction technique. It is found that with the FSP, the fraction of low ∑boundary such as ∑3, 7, and 9 are increased. The obtained results show that there are no deformation texture components in the structure of friction stir processed samples. However, some of the main recrystallization texture components such as BR and cubeND are formed during FSP which indicate the occurrence of dynamic recrystallization phenomenon due to the severe plastic deformation induced by the rotation of tool.

Literature survey on oxidations and fatigue lives at elevated temperatures

NASA Technical Reports Server (NTRS)

Liu, H. W.; Oshida, Y.

1984-01-01

Nickel-base superalloys are the most complex and the most widely used for high temperature applications such as aircraft engine components. The desirable properties of nickel-base superalloys at high temperatures are tensile strength, thermomechanical fatigue resistance, low thermal expansion, as well as oxidation resistance. At elevated temperature, fatigue cracks are often initiated by grain boundary oxidation, and fatigue cracks often propagate along grain boundaries, where the oxidation rate is higher. Oxidation takes place at the interface between metal and gas. Properties of the metal substrate, the gaseous environment, as well as the oxides formed all interact to make the oxidation behavior of nickel-base superalloys extremely complicated. The important topics include general oxidation, selective oxidation, internal oxidation, grain boundary oxidation, multilayer oxide structure, accelerated oxidation under stress, stress-generation during oxidation, composition and substrate microstructural changes due to prolonged oxidation, fatigue crack initiation at oxidized grain boundaries and the oxidation accelerated fatigue crack propagation along grain boundaries.

Rotation-induced grain growth and stagnation in phase-field crystal models.

PubMed

Bjerre, Mathias; Tarp, Jens M; Angheluta, Luiza; Mathiesen, Joachim

2013-08-01

We consider grain growth and stagnation in polycrystalline microstructures. From the phase-field crystal modeling of the coarsening dynamics, we identify a transition from a grain-growth stagnation upon deep quenching below the melting temperature T(m) to a continuous coarsening at shallower quenching near T(m). The grain evolution is mediated by local grain rotations. In the deep quenching regime, the grain assembly typically reaches a metastable state where the kinetic barrier for recrystallization across boundaries is too large and grain rotation with subsequent coalescence or boundary motion is infeasible. For quenching near T(m), we find that the grain growth depends on the average rate of grain rotation, and follows a power-law behavior with time, with a scaling exponent that depends on the quenching depth.

Microstructure, Texture and Mechanical Properties of Titanium Grade 2 Processed by ECAP (Route C)

NASA Astrophysics Data System (ADS)

Wroński, M.; Wierzbanowski, K.; Wojtas, D.; Szyfner, E.; Valiev, R. Z.; Kawałko, J.; Berent, K.; Sztwiertnia, K.

2018-03-01

In the present work the properties of titanium grade 2 after ECAP processing with original route and regimes (route C, channel angle Φ= 120°, deformation temperature 300 °C, number of passes up to 8) were examined. Texture development and microstructure parameters after ECAP processing and after recrystallization were determined using electron back scatter diffraction and analysed. A significant increase of the mechanical strength accompanied by some increase of ductility was observed in the deformed samples. The kernel average misorientation and average grain orientation spread were strongly increased after deformation, which confirms the material refinement and fragmentation. The proportion of low angle boundaries increased after four ECAP passes, but after four consecutive passes high angle grain boundaries became predominant. No deformation twins were observed after four and eight ECAP passes. The material recrystallized after deformation retained a fine grain microstructure. The textures of deformed and recrystallized samples were determined. It was found that texture after 8 passes is more homogeneous that that after 4 passes, which partly explains higher ductility of this first sample.

Role of Y-Al Oxides During Extended Recovery Process of a Ferritic ODS Alloy

NASA Astrophysics Data System (ADS)

Capdevila, C.; Pimentel, G.; Aranda, M. M.; Rementeria, R.; Dawson, K.; Urones-Garrote, E.; Tatlock, G. J.; Miller, M. K.

2015-08-01

The microstructural stability of Y-Al oxides during the recrystallization of Fe-Cr-Al oxide dispersion strengthened alloy is studied in this work. The goal is to determine the specific distribution pattern of oxides depending where they are located: in the matrix or at the grain boundaries. It was concluded that those located at the grain boundaries yielded a faster coarsening than the ones in the matrix, although no significant differences in composition and/or crystal structure were observed. However, the recrystallization heat treatment leads to the dissolution of the Y2O3 and its combination with Al to form the YAlO3 perovskite oxide particles process, mainly located at the grain boundaries. Finally, atom probe tomography analysis revealed a significant Ti build-up at the grain boundaries that might affect subsequent migration during recrystallization.

Multiscale simulation of xenon diffusion and grain boundary segregation in UO₂

DOE PAGES

Andersson, David A.; Tonks, Michael R.; Casillas, Luis; ...

2015-07-01

In light water reactor fuel, gaseous fission products segregate to grain boundaries, resulting in the nucleation and growth of large intergranular fission gas bubbles. The segregation rate is controlled by diffusion of fission gas atoms through the grains and interaction with the boundaries. Based on the mechanisms established from earlier density functional theory (DFT) and empirical potential calculations, diffusion models for xenon (Xe), uranium (U) vacancies and U interstitials in UO₂ have been derived for both intrinsic (no irradiation) and irradiation conditions. Segregation of Xe to grain boundaries is described by combining the bulk diffusion model with a model formore » the interaction between Xe atoms and three different grain boundaries in UO₂ (Σ5 tilt, Σ5 twist and a high angle random boundary), as derived from atomistic calculations. The present model does not attempt to capture nucleation or growth of fission gas bubbles at the grain boundaries. The point defect and Xe diffusion and segregation models are implemented in the MARMOT phase field code, which is used to calculate effective Xe and U diffusivities as well as to simulate Xe redistribution for a few simple microstructures.« less

Grain Refinement Kinetics in a Low Alloyed Cu–Cr–Zr Alloy Subjected to Large Strain Deformation

PubMed Central

Morozova, Anna; Borodin, Elijah; Bratov, Vladimir; Zherebtsov, Sergey; Kaibyshev, Rustam

2017-01-01

This paper investigates the microstructural evolution and grain refinement kinetics of a solution-treated Cu–0.1Cr–0.06Zr alloy during equal channel angular pressing (ECAP) at a temperature of 673 K via route BC. The microstructural change during plastic deformation was accompanied by the formation of the microband and an increase in the misorientations of strain-induced subboundaries. We argue that continuous dynamic recrystallization refined the initially coarse grains, and discuss the dynamic recrystallization kinetics in terms of grain/subgrain boundary triple junction evolution. A modified Johnson–Mehl–Avrami–Kolmogorov relationship with a strain exponent of about 1.49 is used to express the strain dependence of the triple junctions of high-angle boundaries. Severe plastic deformation by ECAP led to substantial strengthening of the Cu–0.1Cr–0.06Zr alloy. The yield strength increased from 60 MPa in the initial state to 445 MPa after a total strain level of 12. PMID:29210990

Influence of minor combined addition of Cr and Pr on microstructure, mechanical properties and corrosion behaviors of an ultrahigh strength Al-Zn-Mg-Cu-Zr alloy.

PubMed

Wang, Ming; Huang, Lanping; Chen, Kanghua; Liu, Wensheng

2018-01-01

This work focuses on controlling grain boundary structure in an ultra-high strength Al-8.6Zn-2.5Mg-2.2Cu-0.16Zr (wt.%) alloy by the combined addition of trace Cr (0.1wt.%) and Pr (0.14wt.%), and evaluating mechanical properties and localized corrosion behaviors of the alloy in the peak aged condition. The introduction of trace Cr and Pr leads to the formation of nanoscale Cr, Pr-containing Al 3 Zr and Zr-containing PrCr 2 Al 20 dispersoids which can obviously inhibit the recrystallization and sub-grain growth of the super-high strength Al-Zn-Mg-Cu alloys, and retain the deformation-recovery microstructure dominated by low-angle grain boundaries. The nearly ellipsoidal dispersoids with a size of 10-35nm are discretely distributed and precipitate free zones are hardly formed in low-angle grain boundaries. This new alloy composition exhibits better combined properties, higher resistance to stress corrosion, exfoliation corrosion and inter-granular corrosion with the undamaged strength, ductility and fracture toughness. Copyright © 2017 Elsevier Ltd. All rights reserved.

Microstructure evolution of a ZrC coating layer in TRISO particles during high-temperature annealing

NASA Astrophysics Data System (ADS)

Kim, Daejong; Chun, Young Bum; Ko, Myeong Jin; Lee, Hyeon-Geun; Cho, Moon-Sung; Park, Ji Yeon; Kim, Weon-Ju

2016-10-01

The influence of high-temperature annealing on the microstructure of zirconium carbide (ZrC) was investigated in relation to its application as a coating layer of a nuclear fuel in a very high temperature gas cooled reactor. ZrC was deposited as a constituent coating layer of TRISO coated particles by a fluidized bed chemical vapor deposition method using a ZrCl4-CH4-Ar-H2 system. The grain growth of ZrC during high-temperature annealing was strongly influenced by the co-deposition of free carbon. Sub-stoichiometric ZrC coatings have experienced a significant grain growth during high-temperature annealing at 1800 °C and 1900 °C for 1 h. On the other hand, a dual phase of stoichiometric ZrC and free carbon experienced little grain growth. It was revealed that the free carbon of the as-deposited ZrC was primarily distributed within the ZrC grains but was redistributed to the grain boundaries after annealing. Consequently, carbon at the grain boundary retarded the grain growth of ZrC. Electron backscatter diffraction (EBSD) results showed that as-deposited ZrC had (001) a preferred orientation that kept its favored direction after significant grain growth during annealing. The hardness slightly decreased as the grain growth progressed.

Modelling grain growth in the framework of Rational Extended Thermodynamics

NASA Astrophysics Data System (ADS)

Kertsch, Lukas; Helm, Dirk

2016-05-01

Grain growth is a significant phenomenon for the thermomechanical processing of metals. Since the mobility of the grain boundaries is thermally activated and energy stored in the grain boundaries is released during their motion, a mutual interaction with the process conditions occurs. To model such phenomena, a thermodynamic framework for the representation of thermomechanical coupling phenomena in metals including a microstructure description is required. For this purpose, Rational Extended Thermodynamics appears to be a useful tool. We apply an entropy principle to derive a thermodynamically consistent model for grain coarsening due to the growth and shrinkage of individual grains. Despite the rather different approaches applied, we obtain a grain growth model which is similar to existing ones and can be regarded as a thermodynamic extension of that by Hillert (1965) to more general systems. To demonstrate the applicability of the model, we compare our simulation results to grain growth experiments in pure copper by different authors, which we are able to reproduce very accurately. Finally, we study the implications of the energy release due to grain growth on the energy balance. The present unified approach combining a microstructure description and continuum mechanics is ready to be further used to develop more elaborate material models for complex thermo-chemo-mechanical coupling phenomena.

Hydrogen segregation to inclined Σ3 < 110 >twin grain boundaries in nickel

DOE PAGES

O’Brien, Christopher J.; Foiles, Stephen M.

2016-08-04

Low-mobility twin grain boundaries dominate the microstructure of grain boundary-engineered materials and are critical to understanding their plastic deformation behaviour. The presence of solutes, such as hydrogen, has a profound effect on the thermodynamic stability of the grain boundaries. This work examines the case of a Σ3 grain boundary at inclinations from 0° ≤ Φ ≤ 90°. The angle Φ corresponds to the rotation of the Σ3 (1 1 1) < 1 1 0 > (coherent) into the Σ3 (1 1 2) < 1 1 0 > (lateral) twin boundary. To this end, atomistic models of inclined grain boundaries, utilisingmore » empirical potentials, are used to elucidate the finite-temperature boundary structure while grand canonical Monte Carlo models are applied to determine the degree of hydrogen segregation. In order to understand the boundary structure and segregation behaviour of hydrogen, the structural unit description of inclined twin grain boundaries is found to provide insight into explaining the observed variation of excess enthalpy and excess hydrogen concentration on inclination angle, but the explanatory power is limited by how the enthalpy of segregation is affected by hydrogen concentration. At higher concentrations, the grain boundaries undergo a defaceting transition. In order to develop a more complete mesoscale model of the interfacial behaviour, an analytical model of boundary energy and hydrogen segregation that relies on modelling the boundary as arrays of discrete 1/3 < 1 1 1 > disconnections is constructed. Lastly, the complex interaction of boundary reconstruction and concentration-dependent segregation behaviour exhibited by inclined twin grain boundaries limits the range of applicability of such an analytical model and illustrates the fundamental limitations for a structural unit model description of segregation in lower stacking fault energy materials.« less

Strength of Rocks Affected by Deformation Enhanced Grain Growth

NASA Astrophysics Data System (ADS)

Kellermann Slotemaker, A.; de Bresser, H.; Spiers, C.

2005-12-01

One way of looking into the possibility of long-term strength changes in the lithosphere is to study transient effects resulting from modifications of the microstructure of rocks. It is generally accepted that mechanical weakening may occur due to progressive grain size refinement resulting from dynamic recrystallization. A decrease in grain size may induce a switch from creep controlled by grain size insensitive dislocation mechanisms to creep governed by grain size sensitive (GSS) mechanisms involving diffusion and grain boundary sliding processes. This switch forms a well-known scenario to explain localization in the lithosphere. However, fine-grained rocks in localized deformation zones are prone to grain coarsening due to surface energy driven grain boundary migration (SED-GBM). This might harden the rock, affecting its role in localizing strain in the long term. The question has arisen if grain growth by SED-GBM in a rock deforming in the GSS creep field can be significantly affected by strain. The broad aim of this study is to shed more light onto this. We have experimentally investigated the microstructural and strength evolution of fine-grained (~0.6 μm) synthetic forsterite and Fe-bearing olivine aggregates that coarsen in grain size while deforming by GSS creep at elevated pressure (600 MPa) and temperature (850-1000 °C). The materials were prepared by `sol-gel' method and contained 0.3-0.5 wt% water and 5-10 vol% enstatite. We performed i) static heat treatment tests of various time durations involving hot isostatic pressing (HIP), and ii) heat treatment tests starting with HIP and continuing with deformation up to 45% axial strain at strain rates in the range 4x10-7 - 1x10-4 s-1. Microstructures were characterized by analyzing full grain size distributions and textures using SEM/EBSD. In addition to the experiments, we studied microstructural evolution in simple two-dimensional numerical models, combining deformation and SED-GBM by means of the modeling package ELLE. Synthetic olivine samples that were heat treated without straining showed only minor grain growth. Presumably, the second phase (enstatite) and/or porosity remaining in the starting material after densification slowed down or inhibited SED-GBM in the static situation. In contrast, samples heat treated and deformed for time durations similar to those of the static tests demonstrated, at identical temperature, an increase in grain size with increasing strain up to a value twice that of the static counterpart. This grain coarsening was associated with continuous hardening of the material, witnessed by the stress-strain curves. A random lattice preferred orientation combined with a low stress sensitivity (n~2) suggested dominant GSS creep controlled by grain boundary sliding. A dynamic grain growth model involving an increase in the fraction of non-hexagonal grains, related to grain neighbor switching, appears applicable to the observed grain growth that is held responsible for the hardening. The ELLE numerical modeling demonstrated that a combination of SED-GBM and geometrical deformation of a 2D grain aggregate can indeed result in enhanced grain growth compared to static grain growth tests. The fraction of non-hexagonal grains was found to remain more or less constant during static grain growth but increased during deformation. We suggest that the application of the dynamic grain growth model to the long-term microstructural evolution of fine-grained lithospheric shear zones can further improve our understanding of the transient or permanent character of strain localizations and related rheological behavior.

The effect of sheet processing on the microstructure, tensile, and creep behavior of INCONEL alloy 718

NASA Astrophysics Data System (ADS)

Boehlert, C. J.; Dickmann, D. S.; Eisinger, Ny. N. C.

2006-01-01

The grain size, grain boundary character distribution (GBCD), creep, and tensile behavior of INCONEL alloy 718 (IN 718) were characterized to identify processing-microstructure-property relationships. The alloy was sequentially cold rolled (CR) to 0, 10, 20, 30, 40, 60, and 80 pct followed by annealing at temperatures between 954 °C and 1050 °C and the traditional aging schedule used for this alloy. In addition, this alloy can be superplastically formed (IN 718SPF) to a significantly finer grain size and the corresponding microstructure and mechanical behavior were evaluated. The creep behavior was evaluated in the applied stress (σ a ) range of 300 to 758 MPa and the temperature range of 638 °C to 670 °C. Constant-load tensile creep experiments were used to measure the values of the steady-state creep rate and the consecutive load reduction method was used to determine the values of backstress (σ0). The values for the effective stress exponent and activation energy suggested that the transition between the rate-controlling creep mechanisms was dependent on effective stresses (σ e =σ a σ0) and the transition occurred at σ e ≅ 135 MPa. The 10 to 40 pct CR samples exhibited the greatest 650 °C strength, while IN 718SPF exhibited the greatest room-temperature (RT) tensile strength (>1550 MPa) and ductility (ɛ f >16 pct). After the 954 °C annealing treatment, the 20 pct CR and 30 pct CR microstructures exhibited the most attractive combination of elevated-temperature tensile and creep strength, while the most severely cold-rolled materials exhibited the poorest elevated-temperature properties. After the 1050 °C annealing treatment, the IN 718SPF material exhibited the greatest backstress and best creep resistance. Electron backscattered diffraction was performed to identify the GBCD as a function of CR and annealing. The data indicated that annealing above 1010 °C increased the grain size and resulted in a greater fraction of twin boundaries, which in turn increased the fraction of coincident site lattice boundaries. This result is discussed in light of the potential to grain boundary engineer this alloy.

Stress Rupture Fracture Model and Microstructure Evolution for Waspaloy

NASA Astrophysics Data System (ADS)

Yao, Zhihao; Zhang, Maicang; Dong, Jianxin

2013-07-01

Stress rupture behavior and microstructure evolution of nickel-based superalloy Waspaloy specimens from tenon teeth of an as-received 60,000-hour service-exposed gas turbine disk were studied between 923 K and 1088 K (650 °C and 815 °C) under initial applied stresses varying from 150 to 840 MPa. Good microstructure stability and performance were verified for this turbine disk prior to stress rupture testing. Microstructure instability, such as the coarsening and dissolution of γ' precipitates at the varying test conditions, was observed to be increased with temperature and reduced stress. Little microstructure variation was observed at 923 K (650 °C). Only secondary γ' instability occurred at 973 K (700 °C). Four fracture mechanisms were obtained. Transgranular creep fracture was exhibited up to 923 K (650 °C) and at high stress. A mixed mode of transgranular and intergranular creep fracture occurred with reduced stress as a transition to intergranular creep fracture (ICF) at low stress. ICF was dominated by grain boundary sliding at low temperature and by the nucleation and growth of grain boundary cavities due to microstructure instability at high temperature. The fracture mechanism map and microstructure-related fracture model were constructed. Residual lifetime was also evaluated by the Larson-Miller parameter method.

Viscous constitutive relations of solid-liquid composites in terms of grain boundary contiguity: 1. Grain boundary diffusion control model

NASA Astrophysics Data System (ADS)

Takei, Yasuko; Holtzman, Benjamin K.

2009-06-01

Viscous constitutive relations of partially molten rocks deforming in the regime of grain boundary (GB) diffusion creep are derived theoretically on the basis of microstructural processes at the grain scale. The viscous constitutive relation developed in this study is based on contiguity as an internal state variable, which enables us to take into account the detailed effects of grain-scale melt distribution observed in experiments. Compared to the elasticities derived previously for the same microstructural model, the viscosities are much more sensitive to the presence of melt and variations in contiguity. As explored in this series of three companion papers, this "contiguity" model predicts that a very small amount of melt (ϕ < 0.01) significantly reduces the bulk and shear viscosities. Furthermore, a large anisotropy in viscosity is produced by anisotropy in contiguity, which occurs in deforming partially molten rocks. These results have important implications for deformation and melt extraction at small melt fractions, as well as for shear-induced melt segregation. The viscous and elastic constitutive relations derived in terms of contiguity bridge microscopic grain-scale and macroscopic continuum properties. These constitutive relations are essential for investigating melt migration dynamics in a forward sense on the basis of the basic equations of two-phase dynamics and in an inverse sense on the basis of seismological observations.

Microstructure evolution and dislocation behaviour in high chromium, fully ferritic steels strengthened by intermetallic Laves phases.

PubMed

Lopez Barrilao, Jennifer; Kuhn, Bernd; Wessel, Egbert

2018-05-01

In the present study a stainless, high strength, ferritic (non-martensitic) steel was analysed regarding microstructure and particle evolution. The preceding hot-rolling process of the steel results in the formation of sub-grain structures, which disappear over time at high temperature. Besides that the formation of particle-free zones was observed. The pronounced formation of these zones preferentially appears close to high angle grain boundaries and is considered to be responsible for long-term material failure under creep conditions. The reasons for this are lacking particle hardening and thus a concentration and accumulation of deformation in the particle free areas close to the grain boundaries. Accordingly in-depth investigations were performed by electron microscopy to analyse dislocation behaviour and its possible effect on the mechanical response of these weak areas. Copyright © 2018 Elsevier Ltd. All rights reserved.

Deformation-Induced Dynamic Precipitation and Resulting Microstructure in a Mg-Zn-Ca Alloy

NASA Astrophysics Data System (ADS)

Du, Yuzhou; Zheng, Mingyi; Jiang, Bailing; Zhou, Kesong

2018-05-01

The microstructure of an Mg-Zn-Ca extrusion was investigated by transmission electron microscopy, and the interaction between dynamic precipitation and dynamic recrystallization was analyzed. The results showed that dynamic precipitation significantly affected the microstructure of the as-extruded Mg-Zn-Ca alloy. The pinning effects of precipitates on dislocations effectively prohibited dynamic recrystallization processes, while the grain boundary precipitate Ca2Mg6Zn3, inhibited the growth of dynamically recrystallized grains. Consequently, a bimodal microstructure with fine dynamically recrystallized (DRXed) grains and elongated deformed regions was obtained for the Mg-Zn-Ca extrusion. High-resolution transmission electron microscopy indicated that the intragranular precipitate MgZn2 had a crystal orientation relationship with α-Mg in the form of (0002)Mg//(10-13)MgZn2 and [1-100]Mg//[1-210]MgZn2, which was beneficial for strength improvement.

Strain Characterization and Microstructure Evolution Under Deformation in 2060 Alloy

NASA Astrophysics Data System (ADS)

Jin, X.; Zhang, G. D.; Zhao, Y. F.; Xue, F.

2018-05-01

A new method of DIC combined with EBSD is developed for the characterization of strain and microstructure evolution during bending. The traditional microhardness point and DIC methods are used to study the microstructure evolution in 2060 alloy during bending; the interested area suffers under tensile stress, the microstructure evolution is collected by SEM, EBSD, digital image correlation (DIC) method during bending. The results shows that the DIC method can both realize the strain tensor characterization of the interested area, and can also express the local strain tensor in the micro-area even more. The degree of grain division in the process of deformation is related to the strain in this region; the grains have larger strain of small angle grain boundary (SLGBs), which results in a new micro-organizational structure. The misorientation is smaller with larger strain degree while the misorientation is larger with smaller strain.

Mechanism of Martensitic to Equiaxed Microstructure Evolution during Hot Deformation of a Near-Alpha Ti Alloy

NASA Astrophysics Data System (ADS)

Shams, Seyed Amir Arsalan; Mirdamadi, Shamsoddin; Abbasi, Seyed Mahdi; Kim, Daehwan; Lee, Chong Soo

2017-06-01

In this study, mechanisms of microstructural evolution during hot deformation of Ti-1100 were investigated by EBSD analysis. Misorientation angle distribution of initial microstructure showed that diffusionless martensitic phase transformation in Ti-1100 obeys Burgers orientation relationship, and most of the high-angle-grain boundaries consist of angles of 60 and 63 deg. Calculated activation energy of hot deformation ( 338 kJ/mol) and EBSD grain boundary maps revealed that continuous dynamic recrystallization (CDRX) is the dominant mechanism during hot compression at 1073 K (800 °C) and strain rate of 0.005 s-1. At a temperature range of 1073 K to 1173 K (800 °C to 900 °C), not only the array of variants lying perpendicular to compression axis but also CDRX contributes to flow softening. Increasing the rolling temperature from 1123 K to 1273 K (850 °C to 1000 °C) brought about changes in spheroidization mechanism from CDRX to conventional boundary splitting and termination migration correlated with the higher volume fraction of beta phase at higher temperatures.

Impurity distribution and microstructure of Ga-doped ZnO films grown by molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Kvit, A. V.; Yankovich, A. B.; Avrutin, V.; Liu, H.; Izyumskaya, N.; Özgür, Ü.; Morkoç, H.; Voyles, P. M.

2012-12-01

We report microstructural characterization of heavily Ga-doped ZnO (GZO) thin films on GaN and sapphire by aberration-corrected scanning transmission electron microscopy. Growth under oxygen-rich and metal-rich growth conditions leads to changes in the GZO polarity and different extended defects. For GZO layers on sapphire, the primary extended defects are voids, inversion domain boundaries, and low-angle grain boundaries. Ga doping of ZnO grown under metal-rich conditions causes a switch from pure oxygen polarity to mixed oxygen and zinc polarity in small domains. Electron energy loss spectroscopy and energy dispersive spectroscopy spectrum imaging show that Ga is homogeneous, but other residual impurities tend to accumulate at the GZO surface and at extended defects. GZO grown on GaN on c-plane sapphire has Zn polarity and no voids. There are misfit dislocations at the interfaces between GZO and an undoped ZnO buffer layer and at the buffer/GaN interface. Low-angle grain boundaries are the only threading microstructural defects. The potential effects of different extended defects and impurity distributions on free carrier scattering are discussed.

Modelling of Microstructure Changes in Hot Deformed Materials Using Cellular Automata

NASA Astrophysics Data System (ADS)

Kuc, Dariusz; Gawąd, Jerzy

2011-01-01

The paper is focused on application of multi-scale 2D method. Model approach consists of Cellular Automata (CA) model of microstructure development and the finite element code to solve thermo-mechanical problem. Dynamic recrystallization phenomenon is taken into account in 2D CA model which takes advantage of explicit representation of microstructure, including individual grains and grain boundaries. Flow stress is the main material parameter in mechanical part of FE and is calculated on the basis of average dislocation density obtained from CA model. The results attained from the model were validated with the experimental data. In the present study, austenitic steel X3CrNi18-10 was investigated. The examination of microstructure for the initial and final microstructures was carried out, using light microscopy and transmission electron microscopy.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Valderrama, Billy; He, Lingfeng; Henderson, Hunter B.

Fission products, such as krypton (Kr), are known to be insoluble within UO 2, segregating towards grain boundaries, eventually leading to a lowering of the thermal conductivity and fuel swelling. Recent computational studies have identified that differences in grain boundary structure have a significant effect on the segregation behavior of fission products. However, experimental work supporting these simulations is lacking. Atom probe tomography was used to measure the Kr distribution across grain boundaries in UO 2. Polycrystalline depleted-UO 2 samples was irradiated with 0.7 and 1.8 MeV Kr-ions and annealed to 1000ºC, 1300ºC, and 1600°C for 1 hour to producemore » a Kr-bubble dominated microstructure. The results of this work indicate a strong dependence of Kr concentration as a function of grain boundary structure. Temperature also influences grain boundary chemistry with greater Kr concentration evident at higher temperatures, resulting in a reduced Kr concentration in the bulk. While Kr migration is active at elevated temperatures, no changes in grain size or texture were observed in the irradiated UO 2 samples.« less

The relationship between structure and magnetic properties in ultra-fine grained/nanostructured FePd alloys

NASA Astrophysics Data System (ADS)

Okumura, Hideyuki

In this study, the magnetic behavior including coercivity and the magnetic phase transition (ferromagnetic ↔ paramagnetic) and related phenomena were qualitatively and quantitatively investigated in ultra-fine grained/nanostructured FePd permanent magnet alloys, in relation to the microstructure and defect structure, and the results were compared with bulk FePd. Most of the alloy specimens investigated were in the form of epoxybonded magnets or isostatically-pressed pellets, formed from powders which were produced with high energy ball milling. Some results of thin films and ribbons produced with sputtering and melt-spinning, respectively, are also included in this thesis. Characterization of the materials was performed by using X-ray diffraction techniques with texture measurement, transmission electron microscopy with Lorentz microscopy, scanning electron microscopy with EDS analysis, optical microscopy and vibrating sample magnetometry. X-ray line broadening analysis was utilized for the quantitative characterization of the nanoscale microstructure, and it was found that the Cauchy-Gaussian profile assumption best describes the broadening data. Enhanced coercivities ˜10 times those of the bulk FePd obtained using conventional heat treatments were explained as the result of statistical (stochastic) unpinning of interaction domain walls out of the potential well at the grain boundary, and there is also an additional effect ascribed to an increase of the magnetocrystalline anisotropy, which is mainly due to the metastable c/a ratio of the nanostructured ordered phase and possibly to stress anisotropy. At the same time, there is also a decrease of the coercivity for smaller grain sizes because of the "magnetically soft" grain boundary phase. A semi-quantitative theoretical model is proposed, which includes the effect of exchange coupling between the ordered grains. The so-called Kronmuller analysis based on the wall pinning model was self-consistent, supporting the notion that wall pinning by grain boundary is the dominant mechanism controlling the coercivity in the nanostructured aggregates in which the magnetic structure is comprised of interaction domains. Furthermore, conventionally structure-insensitive, intrinsic properties such as the saturation magnetization and Curie temperature were found to become structure-sensitive in these materials. The results were semi-quantitatively explained by consideration of the extraordinary microstructure and defect structure involving the high and complex strain fields, metastable tetragonalities, nonequilibrium grain boundaries, extremely high surface-to-volume ratios and perturbed coordination spheres. The possible change in the atomic bond character particularly around grain boundaries is also briefly discussed. It seems that there is a significant fluctuation in exchange couplings at the grain boundary volume, causing the variation of the saturation magnetization, while for the variation of the Curie temperature the powder surface instead of the grain boundary is more important. A modified localized moment model and thus Hund's rules seem applicable to the FePd alloy systems, and the spin density fluctuations seem small in the FePd alloys.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rodgers, Theron M.; Madison, Jonathan D.; Tikare, Veena

Additive manufacturing (AM) is of tremendous interest given its ability to realize complex, non-traditional geometries in engineered structural materials. But, microstructures generated from AM processes can be equally, if not more, complex than their conventionally processed counterparts. While some microstructural features observed in AM may also occur in more traditional solidification processes, the introduction of spatially and temporally mobile heat sources can result in significant microstructural heterogeneity. While grain size and shape in metal AM structures are understood to be highly dependent on both local and global temperature profiles, the exact form of this relation is not well understood. Wemore » implement an idealized molten zone and temperature-dependent grain boundary mobility in a kinetic Monte Carlo model to predict three-dimensional grain structure in additively manufactured metals. In order to demonstrate the flexibility of the model, synthetic microstructures are generated under conditions mimicking relatively diverse experimental results present in the literature. Simulated microstructures are then qualitatively and quantitatively compared to their experimental complements and are shown to be in good agreement.« less

A Cosserat crystal plasticity and phase field theory for grain boundary migration

NASA Astrophysics Data System (ADS)

Ask, Anna; Forest, Samuel; Appolaire, Benoit; Ammar, Kais; Salman, Oguz Umut

2018-06-01

The microstructure evolution due to thermomechanical treatment of metals can largely be described by viscoplastic deformation, nucleation and grain growth. These processes take place over different length and time scales which present significant challenges when formulating simulation models. In particular, no overall unified field framework exists to model concurrent viscoplastic deformation and recrystallization and grain growth in metal polycrystals. In this work a thermodynamically consistent diffuse interface framework incorporating crystal viscoplasticity and grain boundary migration is elaborated. The Kobayashi-Warren-Carter (KWC) phase field model is extended to incorporate the full mechanical coupling with material and lattice rotations and evolution of dislocation densities. The Cosserat crystal plasticity theory is shown to be the appropriate framework to formulate the coupling between phase field and mechanics with proper distinction between bulk and grain boundary behaviour.

Subsurface Grain Morphology Reconstruction by Differential Aperture X-ray Microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eisenlohr, Philip; Shanthraj, Pratheek; Vande Kieft, Brendan R.

A multistep, non-destructive grain morphology reconstruction methodology that is applicable to near-surface volumes is developed and tested on synthetic grain structures. This approach probes the subsurface crystal orientation using differential aperture x-ray microscopy on a sparse grid across the microstructure volume of interest. Resulting orientation data are clustered according to proximity in physical and orientation space and used as seed points for an initial Voronoi tessellation to (crudely) approximate the grain morphology. Curvature-driven grain boundary relaxation, simulated by means of the Voronoi implicit interface method, progressively improves the reconstruction accuracy. The similarity between bulk and readily accessible surface reconstruction errormore » provides an objective termination criterion for boundary relaxation.« less

Microstructure, microtexture and precipitation in the ultrafine-grained surface layer of an Al-Zn-Mg-Cu alloy processed by sliding friction treatment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Yanxia

2017-01-15

Precipitate redistribution and texture evolution are usually two concurrent aspects accompanying grain refinement induced by various surface treatment. However, the detailed precipitate redistribution characteristics and process, as well as crystallographic texture in the surface refined grain layer, are still far from full understanding. In this study, we focused on the microstructural and crystallographic features of the sliding friction treatment (SFT) induced surface deformation layer in a 7050 aluminum alloy. With the combination of transmission electron microscopy (TEM) and high angle angular dark field scanning TEM (HAADF-STEM) observations, a surface ultrafine grain (UFG) layer composed of both equiaxed and lamellar ultrafinemore » grains and decorated by high density of coarse grain boundary precipitates (GBPs) were revealed. Further precession electron diffraction (PED) assisted orientation mapping unraveled that high angle grain boundaries rather than low angle grain boundaries are the most favorable nucleation sites for GBPs. The prominent precipitate redistribution can be divided into three successive and interrelated stages, i.e. the mechanically induced precipitate dissolution, solute diffusion and reprecipitation. The quantitative prediction based on pipe diffusion along dislocations and grain boundary diffusion proved the distribution feasibility of GBPs around UFGs. Based on PED and electron backscatter diffraction (EBSD) analyses, the crystallographic texture of the surface UFG layer was identified as a shear texture composed of major rotated cube texture (001) 〈110〉 and minor (111) 〈112〉, while that of the adjoining lamellar coarse grained matrix was pure brass. The SFT induced surface severe shear deformation is responsible for texture evolution. - Highlights: •The surface ultrafine grain layer in a 7050 aluminum alloy was focused. •Precipitate redistribution and texture evolution were discussed. •The quantitative prediction proved the distribution feasibility of GBPs. •Precession electron diffraction orientation mapping showed a shear texture.« less

Heterogeneous dislocation loop formation near grain boundaries in a neutron-irradiated commercial FeCrAl alloy

DOE PAGES

Field, Kevin G.; Briggs, Samuel A.; Hu, Xunxiang; ...

2016-11-01

FeCrAl alloys are an attractive materials class for nuclear power applications due to their increased environmental compatibility over more traditional nuclear materials. Preliminary studies into the radiation tolerance of FeCrAl alloys under accelerated neutron testing between 300-400 °C have shown post-irradiation microstructures containing dislocation loops and Cr-rich ' phase. Although these initial works established the post-irradiation microstructures, little to no focus was applied towards the influence of pre-irradiation microstructures on this response. Here, a well annealed commercial FeCrAl alloy, Alkrothal 720, was neutron irradiated to 1.8 dpa at 382 °C and then the role of random high angle grain boundariesmore » on the spatial distribution and size of dislocation loops, dislocation loops, and black dot damage was analyzed using on-zone scanning transmission electron microscopy. Results showed a clear heterogeneous dislocation loop formation with dislocation loops showing an increased number density and size, black dot damage showing a significant number density decrease, and an increased size of dislocation loops in the vicinity directly adjacent to the grain boundary. Lastly, these results suggest the importance of the pre-irradiation microstructure on the radiation tolerance of FeCrAl alloys.« less

Microstructural changes in Beta-silicon nitride grains upon crystallizing the grain-boundary glass

NASA Technical Reports Server (NTRS)

Lee, William E.; Hilmas, Gregory E.; Lange, F. F. (Editor)

1991-01-01

Crystallizing the grain boundary glass of a liquid phase sintered Si3N4 ceramic for 2 h or less at 1500 C led to formation of gamma Y2Si2O7. After 5 h at 1500 C, the gamma Y2Si2O7 had transformed to beta Y2Si2O7 with a concurrent dramatic increase in dislocation density within beta Si3N4 grains. Reasons for the increased dislocation density is discussed. Annealing for 20 h at 1500 C reduced dislocation densities to the levels found in as-sintered materials.

Effect of Aging Isothermal Time on the Microstructure and Room-Temperature Impact Toughness of Fe-24.8Mn-7.3Al-1.2C Austenitic Steel with κ-Carbides Precipitation

NASA Astrophysics Data System (ADS)

Feng, Yifan; Song, Renbo; Pei, Zhongzheng; Song, Renfeng; Dou, Guoyu

2018-03-01

The microstructure and impact toughness of the as-cast Fe-24.8Mn-7.3Al-1.2C austenitic steel after solution treatment and subsequent aging treatment were investigated in the present work. Research on the κ-carbides precipitation behavior was carried out by transmission electron microscope. The results show that nano-sized coherent κ-carbides were obtained in the as-solutionized steel after aging treatment, which produced precipitation hardening. After being aging treated at 550 °C for 1 h, the steel with regular hexagonal grain structure exhibited a good combination of yield strength ( 574 MPa) and room-temperature impact toughness ( 168 J). In the present steel, the typical cube-on-cube orientation relationship between austenite and κ-carbides was observed. However, due to the long aging isothermal time and high C content, the coarse intergranular κ'-carbide was formed and grew along the austenite grain boundary, which caused this orientation relationship to be destroyed and a dramatical increase of the coherency strain energy at grain boundary. Furthermore, serious embrittlement of grain boundaries caused that cleavage cracks trend to propagate along the grain boundaries. Accordingly, the room-temperature impact toughness decreased sharply. After aging isothermal time prolonging to 13 h, the Charpy V-notch impact toughness was only 5 J and fracture mode turned to fully brittle fracture accompanied with flat facets, shear cracks and well-developed secondary crack.

The Influence of Milling and Spark Plasma Sintering on the Microstructure and Properties of the Al7075 Alloy

PubMed Central

Málek, Přemysl; Minárik, Peter; Novák, Pavel; Průša, Filip

2018-01-01

The compact samples of an Al7075 alloy were prepared by a combination of gas atomization, high energy milling, and spark plasma sintering. The predominantly cellular morphology observed in gas atomized powder particles was completely changed by mechanical milling. The continuous-like intermetallic phases present along intercellular boundaries were destroyed; nevertheless, a small amount of Mg(Zn,Cu,Al)2 phase was observed also in the milled powder. Milling resulted in a severe plastic deformation of the material and led to a reduction of grain size from several µm into the nanocrystalline region. The combination of these microstructural characteristics resulted in abnormally high microhardness values exceeding 300 HV. Consolidation through spark plasma sintering (SPS) resulted in bulk samples with negligible porosity. The heat exposition during SPS led to precipitation of intermetallic phases from the non-equilibrium microstructure of both gas atomized and milled powders. SPS of the milled powder resulted in a recrystallization of the severely deformed structure. An ultra-fine grained structure (grain size close to 500 nm) with grains divided primarily by high-angle boundaries was formed. A simultaneous release of stored deformation energy and an increase in the grain size caused a drop of microhardness to values close to 150 HV. This value was retained even after annealing at 425 °C. PMID:29614046

Microstructural analysis of biodegradable Mg-0.9Ca-1.2Zr alloy

NASA Astrophysics Data System (ADS)

Istrate, B.; Munteanu, C.; Geanta, V.; Baltatu, S.; Focsaneanu, S.; Earar, K.

2016-08-01

Magnesium alloys have applications in aerospace and medical applications as biodegradable orthopedic implants. Alloying with biocompatible elements, such as calcium or zirconium contribute to refining the the microstructure and improves corrosion resistance with the formation of an eutectic compound - Mg2Ca at boundary alpha-Mg grains. The purpose of this paper is to present the microstructure throw optical and scanning electron methods and phase and constituents identification with X-ray analysis. The results showed the presence of alpha-Mg grains with formation of a mechanical compound - Mg2Ca and appearance of alpha- Zr phase relatively uniformly distributed in nests.

Crystalline orientation dependent photoresponse and heterogeneous behaviors of grain boundaries in perovskite solar cells

NASA Astrophysics Data System (ADS)

Jiang, Chuanpeng; Zhang, Pengpeng

2018-02-01

Using photoconductive atomic force microscopy and Kelvin probe force microscopy, we characterize the local electrical properties of grains and grain boundaries of organic-inorganic hybrid perovskite (CH3NH3PbI3) thin films on top of a poly(3,4-ethylenedioxythiophene)-polystyrene sulfonate (PEDOT:PSS)/ITO substrate. Three discrete photoconductivity levels are identified among perovskite grains, likely corresponding to the crystal orientation of each grain. Local J-V curves recorded on these grains further suggest an anti-correlation behavior between the short circuit current (JSC) and open circuit voltage (VOC). This phenomenon can be attributed to diffusion-limited surface recombination at the non-selective perovskite-tip contact, where a higher carrier mobility established in the perovskite grain results in an enhanced surface recombination and thus a lower VOC. In addition, the photoresponse of perovskite films displays a pronounced heterogeneity across the grain boundaries, with the boundaries formed between grains of the same photoconductivity level displaying even enhanced photocurrent and open circuit voltage compared to those of the adjacent grain interiors. These observations highlight the significance of controlling the microstructure of perovskite thin films, which will be a necessary route for further improving the efficiency of perovskite solar cells.

Effect of Heat Treatments on Microstructures and Tensile Properties of Cu-3 wt%Ag-0.5 wt%Zr Alloy

NASA Astrophysics Data System (ADS)

Chen, Gang; Wang, ChuanJie; Zhang, Ying; Yi, Cen; Zhang, Peng

2018-03-01

The microstructures and tensile properties of Cu-3 wt%Ag-0.5 wt%Zr alloy sheets under different aging treatments are investigated in this research. As one kind of precipitate, Ag nanoparticles with coherent orientation relationship with matrix precipitate. However, after the peak-age point, most of Ag nanoparticles grow into short rod shape with the interface translating to semi-coherent, which leads to the lower strength of over-aging sample. The yield strength is estimated by considering solid solute, grain boundary and precipitation strengthening mechanisms. The result shows that the Ag precipitates provide the main strengthening role. Then a constitutive equation representing the evolution of dislocation density with plastic strain is built by considering work-hardening behavior coming from shearable and non-shearable precipitates which is mainly the particles containing Zr. The flow stress contributed by shearable particle hardening is higher than that of non-shearable one. Due to the coarsening of grain boundary precipitates and low rate of damage accumulation of these non-shearable particles, the micro-cracks nucleate easily at grain boundary which leads to intergranular fracture.

Effects of Stress Relaxation Aging with Electrical Pulses on Microstructures and Properties of 2219 Aluminum Alloy

PubMed Central

Tan, Jingsheng; Zhan, Lihua; Zhang, Jiao; Yang, Zhan; Ma, Ziyao

2016-01-01

To realize the high-efficiency and high-performance manufacture of complex high-web panels, this paper introduced electric pulse current (EPC) into the stress relaxation aging forming process of 2219 aluminum alloy and systematically studied the effects of EPC, stress, and aging time upon the microstructure and properties of 2219 aluminum alloy. It is discovered that: (a) EPC greatly enhanced the mechanical properties after stress relaxation aging and reduced the sensitivity of the yield strength for the initial stress under the aging system of 165 °C/11 h; (b) compared with general aging, stress relaxation aging instead delayed the aging process of 2219 aluminum alloy and greatly increased the peak strength value; (c) EPC accelerated the aging precipitation behavior of 2219 aluminum alloy and reduced transgranular and grain-boundary energy difference, thus leading to a more diffused distribution of the transgranular precipitated phase and the absence of a significant precipitation-free zone (PFZ) and grain-boundary stable phase in the grain boundary, further improving the mechanical properties of the alloy. PMID:28773660

Localization of ductile deformation in lithosphere and rocks: the role of grain boundary sliding

NASA Astrophysics Data System (ADS)

Dimanov, Alexandre; Rahanel, Jean; Bornert, Michel; Bourcier, Mathieu; Gaye, Ag; Heripre, Eva; Ludwig, Wolfgang

2017-04-01

Ductile strain of the lithosphere localizes in multi-scale shear zones, ranging from km to mm scales. The resulting mylonites/ultramylonites present microstructural signatures of several concomitant deformation mechanisms. Besides cataclastic features, crystal plasticity dominates in volume, but grain boundary sliding and diffusive/solution mass transport act along interfaces. Considering solely the inherited natural microstructures does not make clear the chronology of appearance and the interactions between these mechanisms. Therefore, inference of the overall mylonitic rheology seems illusory. We have therefore realized over the last decade a systematic rheological characterization of the high temperature flow of various synthetic anorthite - diopside mixtures. The data clearly suggest Newtonian type of rheology as best adapted to the materials representative of the lower crust mylonites. However, the post mortem microstructures undoubtedly evidenced the coexistence of both crystal plasticity and grain boundary sliding processes. Yet, the specific roles of each mechanism in the localization process remained unclear. In order to clarify these aspects we realized a multi-scale micromechanical in situ investigation of the ductile deformation of synthetic rock-salt. The mechanical tests were combined with in-situ optical microscopy, scanning electron microscopy and X-ray tomography (MCT). Digital image correlation (DIC) techniques allowed for measurements and characterization of the multi-scale organization of 2D and 3D full strain fields. Macroscopic and mesoscopic shear bands appear at the sample and microstructure scales, respectively. DIC evidenced the development of discrete slip bands within individual grains, and hence of dominant crystal plasticity. Combination of DIC and EBSD allowed for identification of active slip systems. Conversely, DIC allowed for the identification and the precise quantification of minor activity (< 5% contribution) of grain boundary sliding (GBS). Most importantly, GBS is continuously operating along with crystal slip plasticity, which indicates that in spite of being a secondary mechanism it is a necessary one. GBS seems to accommodate very efficiently for plastic strain incompatibilities between neighboring grains. Our finding is strengthened by finite element (FE) modeling of the viscoplastic behavior of rock-salt, which appears inadequate in detail if solely based on crystal plasticity. Moreover, the local GBS appears to i) trigger the formation of localized shear bands at the microstructure scale, and ii) allow for homogenization of ductile strain throughout the whole specimen. Our major conclusions are that crystal plasticity and GBS are not really dissociable. They are co-operative mechanisms that accommodate each other depending on microstructure and loading conditions. Minor GBS is always necessary in order to accommodate for the pronounced plastic anisotropy of minerals. Conversely, localized minor crystal plasticity is necessary to accommodate dominant GBS. Finally, GBS is directly involved in the initial development of localized ductile strain at the aggregate scale. But, GBS might take over as the dominant mechanism within fine grained mylonites and contribute to the large scale shear zone localization.

Application of ASTAR(TM)/Precession Electron Diffraction Technique to Quantitatively Study Defects in Nanocrystalline Metallic Materials

NASA Astrophysics Data System (ADS)

Ghamarian, Iman

Nanocrystalline metallic materials have the potential to exhibit outstanding performance which leads to their usage in challenging applications such as coatings and biomedical implant devices. To optimize the performance of nanocrystalline metallic materials according to the desired applications, it is important to have a decent understanding of the structure, processing and properties of these materials. Various efforts have been made to correlate microstructure and properties of nanocrystalline metallic materials. Based on these research activities, it is noticed that microstructure and defects (e.g., dislocations and grain boundaries) play a key role in the behavior of these materials. Therefore, it is of great importance to establish methods to quantitatively study microstructures, defects and their interactions in nanocrystalline metallic materials. Since the mechanisms controlling the properties of nanocrystalline metallic materials occur at a very small length scale, it is fairly difficult to study them. Unfortunately, most of the characterization techniques used to explore these materials do not have the high enough spatial resolution required for the characterization of these materials. For instance, by applying complex profile-fitting algorithms to X-ray diffraction patterns, it is possible to get an estimation of the average grain size and the average dislocation density within a relatively large area. However, these average values are not enough for developing meticulous phenomenological models which are able to correlate microstructure and properties of nanocrystalline metallic materials. As another example, electron backscatter diffraction technique also cannot be used widely in the characterization of these materials due to problems such as relative poor spatial resolution (which is 90 nm) and the degradation of Kikuchi diffraction patterns in severely deformed nano-size grain metallic materials. In this study, ASTAR(TM)/precession electron diffraction is introduced as a relatively new orientation microscopy technique to characterize defects (e.g., geometrically necessary dislocations and grain boundaries) in challenging nanocrystalline metallic materials. The capability of this characterization technique to quantitatively determine the dislocation density distributions of geometrically necessary dislocations in severely deformed metallic materials is assessed. Based on the developed method, it is possible to determine the distributions and accumulations of dislocations with respect to the nearest grain boundaries and triple junctions. Also, the competency of this technique to study the grain boundary character distributions of nanocrystalline metallic materials is presented.

Microstructural analysis of the thermal annealing of ice-Ih using EBSD

NASA Astrophysics Data System (ADS)

Hidas, Károly; Tommasi, Andréa; Mainprice, David; Chauve, Thomas; Barou, Fabrice; Montagnat, Maurine

2017-04-01

Rocks deformed in the middle crust and deeper in the Earth typically remain at high temperature for extended time spans after the cessation of deformation. This results in annealing of the deformation microstructure by a series of thermally activated, diffusion-based processes, namely: recovery and static recrystallization, which may also modify the crystal preferred orientation (CPO) or texture. Understanding the effects of annealing on the microstructure and CPO is therefore of utmost importance for the interpretation of the microstructures and for the estimation of the anisotropy of physical properties of lower crustal and mantle rocks. Ice-Ih -the typical form of water ice on the Earth's surface, with hexagonal crystal symmetry- deforms essentially by glide of dislocations on the basal plane [1], thus it has high viscoplastic anisotropy, which induces strong heterogeneity of stresses and strains at both the intra- and intergranular scales [2-3]. This behavior makes ice-Ih an excellent analog material for silicate minerals that compose the Earth. In situ observations of the evolution of the microstructures and CPO during annealing enable the study of the interplay between the various physical processes involved in annealing (recovery, nucleation, grain growth). They also allow the analysis of the impact of the preexisting deformation microstructures on the microstructural and CPO evolution during annealing. Here we studied the evolution of the microstructure of ice-Ih during static recrystallization by stepwise annealing experiments. We alternated thermal annealing and electron backscatter diffraction (EBSD) analyses on polycrystalline columnar ice-Ih pre-deformed in uniaxial compression at temperature of -7 °C to strains of 3.0-5.2. Annealing experiments were carried out at -5 °C and -2 °C up to a maximum of 3.25 days, typically in 5-6 steps. EBSD crystal orientation maps obtained after each annealing step permit the description of microstructural changes. Decrease in average intragranular misorientation at the sample scale and modification of the misorientation across subgrain boundaries provide evidence for recovery from the earliest stages of annealing. This evolution is similar for all studied samples irrespective of their initial strain or annealing temperature. After an incubation period up to 2 hours, recovery is accompanied by recrystallization (nucleation and grain boundary migration). Grain growth proceeds at the expense of domains with high intra-granular misorientations and its kinetics fits the parabolic growth law. Deformation-induced microstructures (tilt boundaries and kink bands) are stable features during early stages of static recrystallization and locally slow down grain boundary migration, pinning grain growth. REFERENCES 1. Duval, P., Ashby, M.F., Anderman, I., 1983. Rate-controlling processes in the creep of polycrystalline ice. Journal of Physical Chemistry 87, 4066-4074. 2. Grennerat, F., Montagnat, M., Castelnau, O., Vacher, P., Moulinec, H., Suquet, P., Duval, P., 2012. Experimental characterization of the intragranular strain field in columnar ice during transient creep. Acta Materialia 60, 3655-3666. 3. Chauve, T., Montagnat, M., Vacher, P., 2015. Strain field evolution during dynamic recrystallization nucleation: A case study on ice. Acta Materialia 101, 116-124. Funding: Research leading to these results was funded by the EU-FP7 Marie Curie postdoctoral grant PIEF-GA-2012-327226 to K.H.

The shear response of copper bicrystals with Σ11 symmetric and asymmetric tilt grain boundaries by molecular dynamics simulation

NASA Astrophysics Data System (ADS)

Zhang, Liang; Lu, Cheng; Tieu, Kiet; Zhao, Xing; Pei, Linqing

2015-04-01

Grain boundaries (GBs) are important microstructure features and can significantly affect the properties of nanocrystalline materials. Molecular dynamics simulation was carried out in this study to investigate the shear response and deformation mechanisms of symmetric and asymmetric Σ11<1 1 0> tilt GBs in copper bicrystals. Different deformation mechanisms were reported, depending on GB inclination angles and equilibrium GB structures, including GB migration coupled to shear deformation, GB sliding caused by local atomic shuffling, and dislocation nucleation from GB. The simulation showed that migrating Σ11(1 1 3) GB under shear can be regarded as sliding of GB dislocations and their combination along the boundary plane. A non-planar structure with dissociated intrinsic stacking faults was prevalent in Σ11 asymmetric GBs of Cu. This type of structure can significantly increase the ductility of bicrystal models under shear deformation. A grain boundary can be a source of dislocation and migrate itself at different stress levels. The intrinsic free volume involved in the grain boundary area was correlated with dislocation nucleation and GB sliding, while the dislocation nucleation mechanism can be different for a grain boundary due to its different equilibrium structures.Grain boundaries (GBs) are important microstructure features and can significantly affect the properties of nanocrystalline materials. Molecular dynamics simulation was carried out in this study to investigate the shear response and deformation mechanisms of symmetric and asymmetric Σ11<1 1 0> tilt GBs in copper bicrystals. Different deformation mechanisms were reported, depending on GB inclination angles and equilibrium GB structures, including GB migration coupled to shear deformation, GB sliding caused by local atomic shuffling, and dislocation nucleation from GB. The simulation showed that migrating Σ11(1 1 3) GB under shear can be regarded as sliding of GB dislocations and their combination along the boundary plane. A non-planar structure with dissociated intrinsic stacking faults was prevalent in Σ11 asymmetric GBs of Cu. This type of structure can significantly increase the ductility of bicrystal models under shear deformation. A grain boundary can be a source of dislocation and migrate itself at different stress levels. The intrinsic free volume involved in the grain boundary area was correlated with dislocation nucleation and GB sliding, while the dislocation nucleation mechanism can be different for a grain boundary due to its different equilibrium structures. Electronic supplementary information (ESI) available: Movies show the evolution of different grain boundaries under shear deformation: S-0, S-54.74, S-70.53-A, S-70.53-B, S-90. See DOI: 10.1039/c4nr07496c

Grain boundary diffusion behaviors in hot-deformed Nd2Fe14B magnets by PrNd-Cu low eutectic alloys

NASA Astrophysics Data System (ADS)

Tang, Xu; Chen, Renjie; Li, Ming; Jin, Chaoxiang; Yin, Wenzong; Lee, Don; Yan, Aru

2018-01-01

High coercivity of hot-deformed Nd2Fe14B magnets was obtained by grain boundary diffusion. Comparable squareness and similar magnetic properties for samples diffusing from side and pole surfaces show little discrepancies if quantities of the infiltrated PrNd-Cu low eutectic alloys is enough to obtain sufficient diffusion. However, the microstructures and higher characteristic peak ratios show preferable orientation of grains near surfaces of the sample diffused from side surfaces than that from pole surfaces. Amorphous Nd-rich phases and crystal Fe-rich phases were both observed in the diffused magnets. The enhancement of coercivity is considered to be resulted from grain boundary optimization and magnetic isolation which is caused by the thickened nonmagnetic intergranular phases.

Simulation of metal additive manufacturing microstructures using kinetic Monte Carlo

DOE PAGES

Rodgers, Theron M.; Madison, Jonathan D.; Tikare, Veena

2017-04-19

Additive manufacturing (AM) is of tremendous interest given its ability to realize complex, non-traditional geometries in engineered structural materials. But, microstructures generated from AM processes can be equally, if not more, complex than their conventionally processed counterparts. While some microstructural features observed in AM may also occur in more traditional solidification processes, the introduction of spatially and temporally mobile heat sources can result in significant microstructural heterogeneity. While grain size and shape in metal AM structures are understood to be highly dependent on both local and global temperature profiles, the exact form of this relation is not well understood. Wemore » implement an idealized molten zone and temperature-dependent grain boundary mobility in a kinetic Monte Carlo model to predict three-dimensional grain structure in additively manufactured metals. In order to demonstrate the flexibility of the model, synthetic microstructures are generated under conditions mimicking relatively diverse experimental results present in the literature. Simulated microstructures are then qualitatively and quantitatively compared to their experimental complements and are shown to be in good agreement.« less

Role of Y-Al oxides during extended recovery process of a ferritic ODS alloy

DOE PAGES

Capdevila, C.; Pimentel, G.; Aranda, M. M.; ...

2015-08-04

The microstructural stability of Y-Al oxides during the recrystallization of Fe-Cr-Al oxide dispersion strengthened alloy is studied in this work. The goal is to determine the specific distribution pattern of oxides depending where they are located: in the matrix or at the grain boundaries. It was concluded that those located at the grain boundaries yielded a faster coarsening than the ones in the matrix, although no significant differences in composition and/or crystal structure were observed. However, the recrystallization heat treatment leads to the dissolution of the Y 2O 3 and its combination with Al to form the YAlO 3 perovskitemore » oxide particles process, mainly located at the grain boundaries. Lastly, atom probe tomography analysis revealed a significant Ti build-up at the grain boundaries that might affect subsequent migration during recrystallization.« less

Investigation of Parent Austenite Grains from Martensite Structure Using EBSD in a Wear Resistant Steel

PubMed Central

Gyhlesten Back, Jessica; Engberg, Göran

2017-01-01

Crystallographic reconstruction of parent austenite grain boundaries from the martensitic microstructure in a wear resistant steel was carried out using electron backscattered diffraction (EBSD). The present study mainly aims to investigate the parent austenite grains from the martensitic structure in an as-rolled (reference) steel sample and samples obtained by quenching at different cooling rates with corresponding dilatometry. Subsequently, this study is to correlate the nearest cooling rate by the dilatometer which yields a similar orientation relationship and substructure as the reference sample. The Kurdjumov-Sachs orientation relationship was used to reconstruct the parent austenite grain boundaries from the martensite boundaries in both reference and dilatometric samples using EBSD crystallographic data. The parent austenite grain boundaries were successfully evaluated from the EBSD data and the corresponding grain sizes were measured. The parent austenite grain boundaries of the reference sample match the sample quenched at 100 °C/s (CR100). Also the martensite substructures and crystallographic textures are similar in these two samples. The results from hardness measurements show that the reference sample exhibits higher hardness than the CR100 sample due to the presence of carbides in the reference sample. PMID:28772813

Investigation of Parent Austenite Grains from Martensite Structure Using EBSD in a Wear Resistant Steel.

PubMed

Gyhlesten Back, Jessica; Engberg, Göran

2017-04-26

Crystallographic reconstruction of parent austenite grain boundaries from the martensitic microstructure in a wear resistant steel was carried out using electron backscattered diffraction (EBSD). The present study mainly aims to investigate the parent austenite grains from the martensitic structure in an as-rolled (reference) steel sample and samples obtained by quenching at different cooling rates with corresponding dilatometry. Subsequently, this study is to correlate the nearest cooling rate by the dilatometer which yields a similar orientation relationship and substructure as the reference sample. The Kurdjumov-Sachs orientation relationship was used to reconstruct the parent austenite grain boundaries from the martensite boundaries in both reference and dilatometric samples using EBSD crystallographic data. The parent austenite grain boundaries were successfully evaluated from the EBSD data and the corresponding grain sizes were measured. The parent austenite grain boundaries of the reference sample match the sample quenched at 100 °C/s (CR100). Also the martensite substructures and crystallographic textures are similar in these two samples. The results from hardness measurements show that the reference sample exhibits higher hardness than the CR100 sample due to the presence of carbides in the reference sample.

Abnormal grain growth in AISI 304L stainless steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shirdel, M., E-mail: mshirdel1989@ut.ac.ir; Mirzadeh, H., E-mail: hmirzadeh@ut.ac.ir; Advanced Metalforming and Thermomechanical Processing Laboratory, School of Metallurgy and Materials Engineering, University of Tehran, Tehran

2014-11-15

The microstructural evolution during abnormal grain growth (secondary recrystallization) in 304L stainless steel was studied in a wide range of annealing temperatures and times. At relatively low temperatures, the grain growth mode was identified as normal. However, at homologous temperatures between 0.65 (850 °C) and 0.7 (900 °C), the observed transition in grain growth mode from normal to abnormal, which was also evident from the bimodality in grain size distribution histograms, was detected to be caused by the dissolution/coarsening of carbides. The microstructural features such as dispersed carbides were characterized by optical metallography, X-ray diffraction, scanning electron microscopy, energy dispersivemore » X-ray analysis, and microhardness. Continued annealing to a long time led to the completion of secondary recrystallization and the subsequent reappearance of normal growth mode. Another instance of abnormal grain growth was observed at homologous temperatures higher than 0.8, which may be attributed to the grain boundary faceting/defaceting phenomenon. It was also found that when the size of abnormal grains reached a critical value, their size will not change too much and the grain growth behavior becomes practically stagnant. - Highlights: • Abnormal grain growth (secondary recrystallization) in AISI 304L stainless steel • Exaggerated grain growth due to dissolution/coarsening of carbides • The enrichment of carbide particles by titanium • Abnormal grain growth due to grain boundary faceting at very high temperatures • The stagnancy of abnormal grain growth by annealing beyond a critical time.« less

Grain boundary modification to suppress lithium penetration through garnet-type solid electrolyte

NASA Astrophysics Data System (ADS)

Hongahally Basappa, Rajendra; Ito, Tomoko; Morimura, Takao; Bekarevich, Raman; Mitsuishi, Kazutaka; Yamada, Hirotoshi

2017-09-01

Garnet-type solid electrolytes are one of key materials to enable practical usage of lithium metal anode for high-energy-density batteries. However, it suffers from lithium growth in pellets on charging, which causes short circuit. In this study, grain boundaries of Li6.5La3Zr1.5Ta0.5O12 (LLZT) pellets are modified with Li2CO3 and LiOH to investigate the influence of the microstructure of grain boundaries on lithium growth and to study the mechanism of the lithium growth. In spite of similar properties (relative density of ca. 96% and total ionic conductivity of 7 × 10-4 S cm-1 at 25 °C), the obtained pellets exhibit different tolerance on the short circuit. The LLZT pellets prepared from LiOH-modified LLZT powders exhibit rather high critical current density of 0.6 mA cm-2, at which short circuit occurs. On the other hand, the LLZT pellets without grain boundary modification short-circuited at 0.15 mA cm-2. Microstructural analyses by means of SEM, STEM and EIS suggest that lithium grows through interconnected open voids, and reveal that surface layers such as Li2CO3 and LiOH are not only plug voids but also facilitate the sintering of LLZT to suppress the lithium growth. The results indicate a strategy towards short-circuit-free lithium metal batteries.

Dynamic Recrystallization of the Constituent γ Phase and Mechanical Properties of Ti-43Al-9V-0.2Y Alloy Sheet.

PubMed

Zhang, Yu; Wang, Xiaopeng; Kong, Fantao; Chen, Yuyong

2017-09-15

A crack-free Ti-43Al-9V-0.2Y alloy sheet was successfully fabricated via hot-pack rolling at 1200 °C. After hot-rolling, the β/γ lamellar microstructure of the as-forged TiAl alloy was completely converted into a homogeneous duplex microstructure with an average γ grain size of 10.5 μm. The dynamic recrystallization (DRX) of the γ phase was systematically investigated. A recrystallization fraction of 62.5% was obtained for the γ phase in the TiAl alloy sheet, when a threshold value of 0.8° was applied to the distribution of grain orientation spread (GOS) values. The high strain rate and high stress associated with hot-rolling are conducive for discontinuous dynamic recrystallization (DDRX) and continuous dynamic recrystallization (CDRX), respectively. A certain high-angle boundary (HAGB: θ = 89° ± 3°<100>), which is associated with DDRX, occurs in both the recrystallized and deformed γ grains. The twin boundaries play an important role in the DDRX of the γ phase. Additionally, the sub-structures and sub-boundaries originating from low-angle boundaries in the deformed grains also indicate that CDRX occurs. The mechanical properties of the alloy sheet were determined at both room and elevated temperatures. At 750 °C, the alloy sheet exhibited excellent elongation (53%), corresponding to a failure strength of 467 MPa.

Static Grain Growth in Contact Metamorphic Calcite: A Cathodoluminescence Study.

NASA Astrophysics Data System (ADS)

Vogt, B.; Heilbronner, R.; Herwegh, M.; Ramseyer, K.

2009-04-01

In the Adamello contact aureole, monomineralic mesozoic limestones were investigated in terms of grain size evolution and compared to results on numerical modeling performed by Elle. The sampled area shows no deformation and therefore represents an appropriate natural laboratory for the study of static grain growth (Herwegh & Berger, 2003). For this purpose, samples were collected at different distances to the contact to the pluton, covering a temperature range between 270 to 630°C. In these marbles, the grain sizes increase with temperature from 5 µm to about 1 cm as one approaches the contact (Herwegh & Berger, 2003). In some samples, photomicrographs show domains of variable cathodoluminescence (CL) intensities, which are interpreted to represent growth zonations. Microstructures show grains that contain cores and in some samples even several growth stages. The cores are usually not centered and the zones not concentric. They may be in touch with grain boundaries. These zonation patterns are consistent within a given aggregate but differ among the samples even if they come from the same location. Relative CL intensities depend on the Mn/Fe ratio. We assume that changes in trace amounts of Mn/Fe must have occurred during the grain size evolution, preserving local geochemical trends and their variations with time. Changes in Mn/Fe ratios can either be explained by (a) locally derived fluids (e.g. hydration reactions of sheet silicate rich marbles in the vicinity) or (b) by the infiltration of the calcite aggregates by externally derived (magmatic?) fluids. At the present stage, we prefer a regional change in fluid composition (b) because the growth zonations only occur at distances of 750-1250 m from the pluton contact (350-450°C). Closer to the contact, neither zonations nor cores were found. At larger distances, CL intensities differ from grain to grain, revealing diagenetic CL patterns that were incompletely recrystallized by grain growth. The role of infiltration of magmatic fluids is also manifest in the vicinity of dikes, where intense zonation patterns are prominent in the marbles. The software Elle was developed to simulate microstructural evolution in rocks. The numerical model with the title "Grain boundary sweeping" was performed by M. Jessell and was found on http://www.materialsknowledge.org/elle. It displays the grain size evolution and the development of growth zonations during grain boundary migration of a 2D foam structure. This simulation was chosen because the driving force is the minimization of isotropic surface energies. It will be compared to the natural microstructures. At the last stage of the simulation the average grain and core sizes have increased. All, even the smallest grains, show growth zonations. Grains can be divided into two groups: (a) initially larger grains, increasing their grain size and maintaining their core size and (b) initially smaller grains with decreasing grain and decreasing core size. Group (a) grains show large areas swept by grain boundaries into the direction of small grains. Grain boundaries between large grains move more slowly. Their cores do not touch any grain boundaries. Cores of group (b) grains are in contact with the grain boundary network and are on the way to be consumed. In the numerical model and in the natural example similar features can be observed: The cores are not necessarily centered, the zonations are not necessarily concentric and some of the cores touch the grain boundary network. In the simulation, grain boundary migration velocity between large grains is smaller than between a large and a small grain. From this we would predict that - given enough time - a well sorted grain size distribution of increased grain size could be generated. But since many small grains occur we infer that this equilibrium has not been obtained. Analytical results of some natural samples that could be analyzed up to now indicate a relatively well sorted grain size distribution suggesting a more mature state of static grain growth. In comparison to the simulation, grain and core boundaries in the marbles are not always straight. For lobate grain boundaries the surface area has not been minimized in respect to the grain size. An explanation for this might be grain boundary pinning or a local dynamic overprint. Some cores and growth zones in the investigated calcites show a continuous change in luminescence. This is interpreted to be an effect of late diffusion within the grain and/or a continuous change of fluid composition and supply. The absence of zonation in samples close to the contact might be explained by fast grain growth due to high temperatures and/or fast fluid transport. Possibly, this is combined with an enhanced component of volume diffusion. Thus concentration variations of Mn/Fe are diminished and not visible in form of a growth zonation. Herwegh M, Berger A (2003) Differences in grain growth of calcite: a field-based modeling approach. Contr. Min. Pet. 145: 600-611

Improvement in plasma illumination properties of ultrananocrystalline diamond films by grain boundary engineering

NASA Astrophysics Data System (ADS)

Sankaran, K. J.; Srinivasu, K.; Chen, H. C.; Dong, C. L.; Leou, K. C.; Lee, C. Y.; Tai, N. H.; Lin, I. N.

2013-08-01

Microstructural evolution of ultrananocrystalline diamond (UNCD) films as a function of substrate temperature (TS) and/or by introducing H2 in Ar/CH4 plasma is investigated. Variation of the sp2 and sp3 carbon content is analyzed using UV-Raman and near-edge X-ray absorption fine structure spectra. Morphological and microstructural studies confirm that films deposited using Ar/CH4 plasma at low TS consist of a random distribution of spherically shaped ultra-nano diamond grains with distinct sp2-bonded grain boundaries, which are attributed to the adherence of CH radicals to the nano-sized diamond clusters. By increasing TS, adhering efficiency of CH radicals to the diamond lattice drops and trans-polyacetylene (t-PA) encapsulating the nano-sized diamond grains break, whereas the addition of 1.5% H2 in Ar/CH4 plasma at low TS induces atomic hydrogen that preferentially etches out the t-PA attached to ultra-nano diamond grains. Both cases make the sp3-diamond phase less passivated. This leads to C2 radicals attaching to the diamond lattice promoting elongated clustered grains along with a complicated defect structure. Such a grain growth model is highly correlated to explain the technologically important functional property, namely, plasma illumination (PI) of UNCD films. Superior PI properties, viz. low threshold field of 0.21 V/μm with a high PI current density of 4.10 mA/cm2 (at an applied field of 0.25 V/μm) and high γ-coefficient (0.2604) are observed for the UNCD films possessing ultra-nano grains with a large fraction of grain boundary phases. The grain boundary component consists of a large amount of sp2-carbon phases that possibly form interconnected paths for facilitating the transport of electrons and the electron field emission process that markedly enhance PI properties.

DOE Office of Scientific and Technical Information (OSTI.GOV)

O’Brien, Christopher J.; Foiles, Stephen M.

Low-mobility twin grain boundaries dominate the microstructure of grain boundary-engineered materials and are critical to understanding their plastic deformation behaviour. The presence of solutes, such as hydrogen, has a profound effect on the thermodynamic stability of the grain boundaries. This work examines the case of a Σ3 grain boundary at inclinations from 0° ≤ Φ ≤ 90°. The angle Φ corresponds to the rotation of the Σ3 (1 1 1) < 1 1 0 > (coherent) into the Σ3 (1 1 2) < 1 1 0 > (lateral) twin boundary. To this end, atomistic models of inclined grain boundaries, utilisingmore » empirical potentials, are used to elucidate the finite-temperature boundary structure while grand canonical Monte Carlo models are applied to determine the degree of hydrogen segregation. In order to understand the boundary structure and segregation behaviour of hydrogen, the structural unit description of inclined twin grain boundaries is found to provide insight into explaining the observed variation of excess enthalpy and excess hydrogen concentration on inclination angle, but the explanatory power is limited by how the enthalpy of segregation is affected by hydrogen concentration. At higher concentrations, the grain boundaries undergo a defaceting transition. In order to develop a more complete mesoscale model of the interfacial behaviour, an analytical model of boundary energy and hydrogen segregation that relies on modelling the boundary as arrays of discrete 1/3 < 1 1 1 > disconnections is constructed. Lastly, the complex interaction of boundary reconstruction and concentration-dependent segregation behaviour exhibited by inclined twin grain boundaries limits the range of applicability of such an analytical model and illustrates the fundamental limitations for a structural unit model description of segregation in lower stacking fault energy materials.« less

Relationships between microstructure and mechanical properties of Ti-5Al-5Mo-5V-3Cr-1Zr alloy

NASA Astrophysics Data System (ADS)

Li, Z. Y.; Wu, G. Q.; Huang, Z.

2018-03-01

Through a statistical, quantitative analysis on microstructure of Ti-5Al-5Mo-5V-3Cr-1Zr (Ti55531) alloy, the relationships between microstructure and mechanical properties and heat treatment temperatures were investigated. The results show that in Widmanstätten structure, the size of β grain is greatly increased with increasing annealing temperature. Static toughness is related to grain boundary alpha phase discontinuity, the tensile strength is related to acicular alpha phase interface length and acicular alpha phase proportion. In duplex microstructure, the tensile strength is related to the equiaxed alpha proportion. Elongation, static toughness and crack forming work are related to the equiaxed alpha proportion and negatively related to secondary phase proportion. The microstructure can be described quantitatively and the mechanical properties can be predicted by analysis of microstructure.

Microstructure and mechanical properties of Al-3Fe alloy processed by equal channel angular extrusion

NASA Astrophysics Data System (ADS)

Fuxiao, Yu; Fang, Liu; Dazhi, Zhao; Toth, Laszlo S.

2014-08-01

Al-Fe alloys are attractive for applications at temperatures beyond those normally associated with the conventional aluminum alloys. Under proper solidification condition, a full eutectic microstructure can be generated in Al-Fe alloys at Fe concentration well in excess of the eutectic composition of 1.8 wt.% Fe. The microstructure in this case is characterized by the metastable regular eutectic Al-Al6Fe fibers of nano-scale in diameter, instead of the equilibrium eutectic Al-Al3Fe phase. In this study, the microstructure and mechanical properties of the Al-3Fe alloy with metastable Al6Fe particles deformed by equal channel angular extrusion were investigated. Severe plastic deformation results in a microstructure consisting of submicron equiaxed Al grains with a uniform distribution of submicron Al6Fe particles on the grain boundaries. The room temperature tensile properties of the alloy with this microstructure will be presented.

Deformation Behavior and Microstructure Evolution of As-Cast 42CrMo Alloy in Isothermal and Non-isothermal Compression

NASA Astrophysics Data System (ADS)

Qin, Fangcheng; Li, Yongtang; Qi, Huiping; Lv, Zhenhua

2016-11-01

The isothermal and non-isothermal multi-pass compression tests of centrifugal casting 42CrMo steel were conducted on a Gleeble-3500 thermal simulation machine. The effects of compression passes and finishing temperatures on deformation behavior and microstructure evolution were investigated. It is found that the microstructure is homogeneous with equiaxed grains, and the flow stress does not show significant change with the increase in passes, while the peak softening coefficient increases first and then decreases during inter-pass. Moreover, the dominant mechanisms of controlled temperature and accumulated static recrystallization for grain refinement and its homogeneous distribution are found after 5 passes deformation. As the finishing temperature increases, the flow stress decreases gradually, but the dynamic recrystallization accelerates and softening effect increases, resulting in the larger grain size and homogeneous microstructure. The microhardness decreases sharply because the sufficient softening occurs in microstructure. When the finishing temperature is 890 °C, the carbide particles are precipitated in the vicinity of the grain boundaries, thus inhibiting the dislocation motion. Thus, the higher finishing temperature (≥970 °C) for centrifugal casting 42CrMo alloy should be avoided in non-isothermal multi-pass deformation, which is beneficial to grain refinement and properties improvement.

Thermal Microstructural Stability of AZ31 Magnesium after Severe Plastic Deformation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Young, John P.; Askari, Hesam A.; Hovanski, Yuri

2015-03-01

Both equal channel angular pressing and friction stir processing have the ability to refine the grain size of twin roll cast AZ31 magnesium and potentially improve its superplastic properties. This work used isochronal and isothermal heat treatments to investigate the microstructural stability of twin roll cast, equal channel angular pressed and friction stir processed AZ31 magnesium. For both heat treatment conditions, it was found that the twin roll casted and equal channel angular pressed materials were more stable than the friction stir processed material. Calculations of the grain growth kinetics showed that severe plastic deformation processing decreased the activation energymore » for grain boundary motion with the equal channel angular pressed material having the greatest Q value of the severely plastically deformed materials and that increasing the tool travel speed of the friction stir processed material improved microstructural stability. The Hollomon-Jaffe parameter was found to be an accurate means of identifying the annealing conditions that will result in substantial grain growth and loss of potential superplastic properties in the severely plastically deformed materials. In addition, Humphreys’s model of cellular microstructural stability accurately predicted the relative microstructural stability of the severely plastically deformed materials and with some modification, closely predicted the maximum grain size ratio achieved by the severely plastically deformed materials.« less

Subgrain Rotation Recrystallization During Shearing: Insights From Full-Field Numerical Simulations of Halite Polycrystals

NASA Astrophysics Data System (ADS)

Gomez-Rivas, E.; Griera, A.; Llorens, M.-G.; Bons, P. D.; Lebensohn, R. A.; Piazolo, S.

2017-11-01

We present, for the first time, results of full-field numerical simulations of subgrain rotation recrystallization of halite polycrystals during simple shear deformation. The series of simulations show how microstructures are controlled by the competition between (i) grain size reduction by creep by dislocation glide and (ii) intracrystalline recovery encompassing subgrain coarsening by coalescence through rotation and alignment of the lattices of neighboring subgrains. A strong grain size reduction develops in models without intracrystalline recovery, as a result of the formation of high-angle grain boundaries when local misorientations exceed 15°. The activation of subgrain coarsening associated with recovery decreases the stored strain energy and results in grains with low intracrystalline heterogeneities. However, this type of recrystallization does not significantly modify crystal preferred orientations. Lattice orientation and grain boundary maps reveal that this full-field modeling approach is able to successfully reproduce the evolution of dry halite microstructures from laboratory deformation experiments, thus opening new opportunities in this field of research. We demonstrate how the mean subgrain boundary misorientations can be used to estimate the strain accommodated by dislocation glide using a universal scaling exponent of about 2/3, as predicted by theoretical models. In addition, this strain gauge can be potentially applied to estimate the intensity of intracrystalline recovery, associated with temperature, using quantitative crystallographic analyses in areas with strain gradients.

A phase quantification method based on EBSD data for a continuously cooled microalloyed steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, H.; Wynne, B.P.; Palmiere, E.J., E-mail: e.j

2017-01-15

Mechanical properties of steels depend on the phase constitutions of the final microstructures which can be related to the processing parameters. Therefore, accurate quantification of different phases is necessary to investigate the relationships between processing parameters, final microstructures and mechanical properties. Point counting on micrographs observed by optical or scanning electron microscopy is widely used as a phase quantification method, and different phases are discriminated according to their morphological characteristics. However, it is difficult to differentiate some of the phase constituents with similar morphology. Differently, for EBSD based phase quantification methods, besides morphological characteristics, other parameters derived from the orientationmore » information can also be used for discrimination. In this research, a phase quantification method based on EBSD data in the unit of grains was proposed to identify and quantify the complex phase constitutions of a microalloyed steel subjected to accelerated coolings. Characteristics of polygonal ferrite/quasi-polygonal ferrite, acicular ferrite and bainitic ferrite on grain averaged misorientation angles, aspect ratios, high angle grain boundary fractions and grain sizes were analysed and used to develop the identification criteria for each phase. Comparing the results obtained by this EBSD based method and point counting, it was found that this EBSD based method can provide accurate and reliable phase quantification results for microstructures with relatively slow cooling rates. - Highlights: •A phase quantification method based on EBSD data in the unit of grains was proposed. •The critical grain area above which GAM angles are valid parameters was obtained. •Grain size and grain boundary misorientation were used to identify acicular ferrite. •High cooling rates deteriorate the accuracy of this EBSD based method.« less

Microstructural Evolution During Cold Rolling and Subsequent Annealing in Low-Carbon Steel with Different Initial Microstructures

NASA Astrophysics Data System (ADS)

Ogawa, Toshio; Dannoshita, Hiroyuki; Maruoka, Kuniaki; Ushioda, Kohsaku

2017-08-01

Microstructural evolution during cold rolling and subsequent annealing of low-carbon steel with different initial microstructures was investigated from the perspective of the competitive phenomenon between recrystallization of ferrite and reverse phase transformation from ferrite to austenite. Three kinds of hot-rolled sheet specimens were prepared. Specimen P consisted of ferrite and pearlite, specimen B consisted of bainite, and specimen M consisted of martensite. The progress of recovery and recrystallization of ferrite during annealing was more rapid in specimen M than that in specimens P and B. In particular, the recrystallized ferrite grains in specimen M were fine and equiaxed. The progress of ferrite-to-austenite phase transformation during intercritical annealing was more rapid in specimen M than in specimens P and B. In all specimens, the austenite nucleation sites were mainly at high-angle grain boundaries, such as those between recrystallized ferrite grains. The austenite distribution was the most uniform in specimen M. Thus, we concluded that fine equiaxed recrystallized ferrite grains were formed in specimen M, leading to a uniform distribution of austenite.

Subsurface Grain Morphology Reconstruction by Differential Aperture X-ray Microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eisenlohr, Philip; Shanthraj, Pratheek; Vande Kieft, Brendan R.

A multistep, non-destructive grain morphology reconstruction methodology that is applicable to near-surface volumes is developed and tested on synthetic grain structures. This approach probes the subsurface crystal orientation using differential aperture X-ray microscopy (DAXM) on a sparse grid across the microstructure volume of interest. Resulting orientation data is clustered according to proximity in physical and orientation space and used as seed points for an initial Voronoi tessellation to (crudely) approximate the grain morphology. Curvature-driven grain boundary relaxation, simulated by means of the Voronoi Implicit Interface Method (VIIM), progressively improves the reconstruction accuracy. The similarity between bulk and readily accessible surfacemore » reconstruction error provides an objective termination criterion for boundary relaxation.« less

Microstructure and electrical properties of CaCu{sub 3}Ti{sub 4}O{sub 12} ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shao, S. F.; Zhang, J. L.; Zheng, P.

2006-04-15

CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) ceramics are prepared by the conventional solid-state reaction method under various sintering temperatures from 1000 to 1120 deg. C at an interval of 10 deg. C. Microstructures and crystalline structures are examined by scanning electronic microscopy and x-ray diffraction, respectively. Dielectric properties and complex impedances are investigated within the frequency range of 40 Hz-110 MHz over the temperature region from room temperature to 350 deg. C. It has been disclosed that the microstructures can be categorized into three different types: type A (with the small but uniform grain sizes), type B (with the bimodal distributionmore » of grain sizes) and type C (with the large and uniform grain sizes), respectively. The largeness of low-frequency dielectric permittivity at room temperature is closely related to the microstructure. Ceramics with different types of microstructures show the diverse temperature-dependent behaviors of electrical properties. However, the existence of some common characteristics is also found among them. For all of the ceramics, a Debye-type relaxation emerges in the frequency range of 100 Hz-100 kHz at high measuring temperatures, which has the larger dielectric dispersion strength than the one known in the frequency range above 100 kHz. Thus, the high-temperature dielectric dispersion exhibits a large low-frequency response and two Debye-type relaxations. Furthermore, all of the ceramics show three semicircles in the complex impedance plane. These semicircles are considered to represent individually different electrical mechanisms, among which the one in the low-frequency range arises most probably from the contribution of the domain boundaries, and the other two are ascribed to the contributions of the domains and the grain boundaries, respectively.« less

Microstructural study of the polymorphic transformation in pentacene thin films.

PubMed

Murakami, Yosuke; Tomiya, Shigetaka; Koshitani, Naoki; Kudo, Yoshihiro; Satori, Kotaro; Itabashi, Masao; Kobayashi, Norihito; Nomoto, Kazumasa

2009-10-02

We have observed, by high-resolution cross-sectional transmission electron microscopy, the first direct evidence of polymorphic transformation in pentacene thin films deposited on silicon oxide substrates. Polymorphic transformation from the thin-film phase to the bulk phase occurred preferentially near polycrystalline grain boundaries, which exhibit concave surfaces. This process is thought to be driven by compressive stress caused by the grain boundaries. In addition to this stress, lattice mismatch between the two phases also results in structural defect formation.

A Microstructure-Based Constitutive Model for Superplastic Forming

NASA Astrophysics Data System (ADS)

Jafari Nedoushan, Reza; Farzin, Mahmoud; Mashayekhi, Mohammad; Banabic, Dorel

2012-11-01

A constitutive model is proposed for simulations of hot metal forming processes. This model is constructed based on dominant mechanisms that take part in hot forming and includes intergranular deformation, grain boundary sliding, and grain boundary diffusion. A Taylor type polycrystalline model is used to predict intergranular deformation. Previous works on grain boundary sliding and grain boundary diffusion are extended to drive three-dimensional macro stress-strain rate relationships for each mechanism. In these relationships, the effect of grain size is also taken into account. The proposed model is first used to simulate step strain-rate tests and the results are compared with experimental data. It is shown that the model can be used to predict flow stresses for various grain sizes and strain rates. The yield locus is then predicted for multiaxial stress states, and it is observed that it is very close to the von Mises yield criterion. It is also shown that the proposed model can be directly used to simulate hot forming processes. Bulge forming process and gas pressure tray forming are simulated, and the results are compared with experimental data.

Mechanisms of grain refinement in aluminum alloys in the process of severe plastic deformation

NASA Astrophysics Data System (ADS)

Kaibyshev, R. O.; Mazurina, I. A.; Gromov, D. A.

2006-01-01

A study of the mechanisms of grain refinement in the process of severe plastic deformation of two aluminum alloys, i.e., 2219 bearing nanometric particles of Al3Zr and low-alloy Al-3% Cu, is described. The alloys are deformed by the method of equal channel angular pressing at 250°C to a maximum strain degree of about 12. The angles of (sub)grain boundaries in alloy 2219 are determined with the help of transmission electron microscopy by the method of Kikuchi lines. The evolution of the microstructure in alloy Al-3% Cu is studied with the help of grain-boundary maps obtained by the method of electron back-scattered diffraction.

Microstructures and dielectric properties of CaCu3Ti4O12 ceramics via combustion method

NASA Astrophysics Data System (ADS)

Yuan, W. X.; Li, Z. J.

2012-01-01

CaCu3Ti4O12 (CCTO) powder was synthesized by the combustion method. The effect of sintering temperature was studied on dielectric properties of the prepared ceramic samples. They have the dielectric constant of ~31 000 and 80 000 for the grain size of 0.3 and 30-100 μm. It is unusual for CCTO with a grain size of 0.3 μm to have a dielectric constant of ~31 000. Their giant dielectric constant could be explained by a two-step internal-barrier-layer-capacitor model, associated with grain boundaries and domain boundaries. The existence of domain boundaries helped to explain the contradiction of the dielectric mechanisms between polycrystalline and single-crystal CCTO.

Effect of Mn and Cr additions on kinetics of recrystallization and parameters of grain-boundary relaxation of Al-4.9Mg alloy

NASA Astrophysics Data System (ADS)

Mikhailovskaya, A. V.; Golovin, I. S.; Zaitseva, A. A.; Portnoi, V. K.; Dröttboom, P.; Cifre, J.

2013-03-01

Methods of microstructural analysis, measurements of hardness, and temperature and time dependences of internal friction (TDIF and TDIF(iso), respectively) have been used to study recrystallization in cold-rolled alloys and grain-boundary relaxation in annealed alloys. A complex analysis of the effect of additions of transition metals (Mn, Cr) on the magnitude of the activation energy of the background of the internal friction in deformed and annealed states and on the activation parameters of grain-boundary relaxation has been performed. Methods of amplitude dependences of internal friction (ADIF) have been used to determine the critical amplitude that corresponds to the beginning of microplastic deformation in the alloys at different temperatures.

Observations of grain boundary structures and inclusions in the NEEM ice core by combination of light and scanning electron microscopy

NASA Astrophysics Data System (ADS)

Shigeyama, Wataru; Nagatsuka, Naoko; Homma, Tomoyuki; Takata, Morimasa; Goto-Azuma, Kumiko; Weikusat, Ilka; Drury, Martyn R.; Kuiper, Ernst-Jan N.; Pennock, Gill M.; Mateiu, Ramona V.; Azuma, Nobuhiko; Dahl-Jensen, Dorthe

2017-04-01

Dynamics of ice sheets is governed by the flow of the ice and this flow results from the internal deformation of the ice aggregate. The deformation properties of the ice are known to be dependent on several factors, such as microstructure (e.g. crystal grain size and orientation) and impurities. It is well known that ice from glacial periods in ice sheets has a high impurity concentration, and the deformation is reported to be faster than that of non-glacial ice (Faria et al., 2014). However, the mechanisms of the deformation are still not well understood. For a better understanding of ice sheet dynamics, it is a prerequisite to elucidate deformation mechanisms of such impurity-rich ice. The microstructure of a material is a factor that influences mechanical properties and is also an indicator of the dominant deformation mechanisms. The effects of impurities on the deformation and the microstructure depend on chemical compositions, states (viz. insoluble inclusions or soluble ions) and locations of the impurities in the crystal lattice. Therefore, in order to better understand the deformation mechanisms in ice, investigation of relationship between the microstructure and characteristics of the impurities is important. We examined the relationship between grain boundaries and inclusions. Light microscopy (LM) is commonly used to map grain boundary structures on a large area of the ice samples (up to 10 × 10 cm); however, observation of small inclusions < 1 µm is limited due to the spatial resolution of LM. For observations of small impurities in ice cores, scanning electron microscopy (SEM) is useful although limited area (1 × 1 cm) can be examined, and sublimation/surface diffusion on ice in the SEM could move the impurities from their original locations. In order to examine the relationship between the grain boundary and the inclusions, we have combined LM and SEM. We first mapped large areas of the ice samples with LM, and then chose several smaller areas within the mapped area for SEM observations. Energy dispersive X-ray spectroscopy (EDS) was also performed during SEM observations to characterize the chemical composition. Our approach was applied to NEEM glacial ice (1548 m depth, 19.2 kyr BP). The initial results show inclusions observed by LM formed aggregates of sub-micrometer-sized particles, whose main constituents were silicates. Reference Faria, S. H., I. Weikusat and N. Azuma (2014). The microstructure of polar ice. Part II: State of the art, Journal of Structural Geology 61: 21-49.

Microstructural Effects on SCC Initiation PWR Primary Water Cold-Worked Alloy 600

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhai, Ziqing; Toloczko, Mychailo B.; Bruemmer, Stephen M.

SCC initiation behavior of one mill annealed alloy 600 plate heat was investigated in simulated PWR primary water under constant load at yield stress with in-situ direct current potential drop (DCPD) monitoring for crack initiation. Twelve specimens were tested at similar cold work levels among which three showed much shorter SCC initiation times (<400 hrs) than the others (>1200 hrs). Post-test examinations revealed that these three specimens all feature an inhomogeneous microstructure where the primary crack always nucleated along the boundary of large elongated grains protruding normally into the gauge. In contrast, such microstructure was either not observed or didmore » not extend deep enough into the gauge in the other specimens exhibiting ~3-6X longer initiation times. In order to better understand the role of this microstructural inhomogeneity in SCC initiation, high-resolution microscopy was performed to compare carbide morphology and strain distribution between the long grains and normal grains, and their potential effects on SCC initiation are discussed in this paper.« less

Evolution of hardness, microstructure, and strain rate sensitivity in a Zn-22% Al eutectoid alloy processed by high-pressure torsion

NASA Astrophysics Data System (ADS)

Kawasaki, Megumi; Lee, Han-Joo; Choi, In-Chul; Jang, Jae-il; Ahn, Byungmin; Langdon, Terence G.

2014-08-01

Severe plastic deformation (SPD) is an attractive processing method for refining microstructures of metallic materials to give ultrafine grain sizes within the submicrometer to even the nanometer levels. Experiments were conducted to discuss the evolution of hardness, microstructure and strain rate sensitivity, m, in a Zn-22% Al eutectoid alloy processed by high- pressure torsion (HPT). The data from microhardness and nanoindentation hardness measurements revealed that there is a significant weakening in the Zn-Al alloy during HPT despite extensive grain refinement. Excellent room-temperature (RT) plasticity was observed in the alloy after HPT from nanoindentation creep in terms of an increased value of m. The microstructural changes with increasing numbers of HPT turns show a strong correlation with the change in the m value. Moerover, the excellent RT plasticity in the alloy is discussed in terms of the enhanced level of grain boundary sliding and the evolution of microsturucture.

Multiscale Characterization of Microstructure in Near-Surface Regions of a 16MnCr5 Gear Wheel After Cyclic Loading

NASA Astrophysics Data System (ADS)

Medghalchi, Setareh; Jamebozorgi, Vahid; Bala Krishnan, Arjun; Vincent, Smobin; Salomon, Steffen; Basir Parsa, Alireza; Pfetzing, Janine; Kostka, Aleksander; Li, Yujiao; Eggeler, Gunther; Li, Tong

2018-05-01

The dependence of the microstructure on the degree of deformation in near-surface regions of a 16MnCr5 gear wheel after 2.1 × 106 loading cycles has been investigated by x-ray diffraction analysis, transmission electron microscopy, and atom probe tomography. Retained austenite and large martensite plates, along with elongated lamella-like cementite, were present in a less deformed region. Comparatively, the heavily deformed region consisted of a nanocrystalline structure with carbon segregation up to 2 at.% at grain boundaries. Spheroid-shaped cementite, formed at the grain boundaries and triple junctions of the nanosized grains, was enriched with Cr and Mn but depleted with Si. Such partitioning of Cr, Mn, and Si was not observed in the elongated cementite formed in the less deformed zone. This implies that rolling contact loading induced severe plastic deformation as well as a pronounced annealing effect in the active contact region of the toothed gear during cyclic loading.

High Temperature Deformation of Twin-Roll Cast Al-Mn-Based Alloys after Equal Channel Angular Pressing.

PubMed

Málek, Přemysl; Šlapáková Poková, Michaela; Cieslar, Miroslav

2015-11-12

Twin roll cast Al-Mn- and Al-Mn-Zr-based alloys were subjected to four passes of equal channel angular pressing. The resulting grain size of 400 nm contributes to a significant strengthening at room temperature. This microstructure is not fully stable at elevated temperatures and recrystallization and vast grain growth occur at temperatures between 350 and 450 °C. The onset of these microstructure changes depends on chemical and phase composition. Better stability is observed in the Al-Mn-Zr-based alloy. High temperature tensile tests reveal that equal channel angular pressing results in a softening of all studied materials at high temperatures. This can be explained by an active role of grain boundaries in the deformation process. The maximum values of ductility and strain rate sensitivity parameter m found in the Al-Mn-Zr-based alloy are below the bottom limit of superplasticity (155%, m = 0.25). However, some features typical for superplastic behavior were observed-the strain rate dependence of the parameter m , the strengthening with increasing grain size, and the fracture by diffuse necking. Grain boundary sliding is believed to contribute partially to the overall strain in specimens where the grain size remained in the microcrystalline range.

High Temperature Deformation of Twin-Roll Cast Al-Mn-Based Alloys after Equal Channel Angular Pressing

PubMed Central

Málek, Přemysl; Šlapáková Poková, Michaela; Cieslar, Miroslav

2015-01-01

Twin roll cast Al-Mn- and Al-Mn-Zr-based alloys were subjected to four passes of equal channel angular pressing. The resulting grain size of 400 nm contributes to a significant strengthening at room temperature. This microstructure is not fully stable at elevated temperatures and recrystallization and vast grain growth occur at temperatures between 350 and 450 °C. The onset of these microstructure changes depends on chemical and phase composition. Better stability is observed in the Al-Mn-Zr-based alloy. High temperature tensile tests reveal that equal channel angular pressing results in a softening of all studied materials at high temperatures. This can be explained by an active role of grain boundaries in the deformation process. The maximum values of ductility and strain rate sensitivity parameter m found in the Al-Mn-Zr-based alloy are below the bottom limit of superplasticity (155%, m = 0.25). However, some features typical for superplastic behavior were observed—the strain rate dependence of the parameter m, the strengthening with increasing grain size, and the fracture by diffuse necking. Grain boundary sliding is believed to contribute partially to the overall strain in specimens where the grain size remained in the microcrystalline range. PMID:28793667

Effect of Heat Treatment on Microstructure and Mechanical Properties of Inconel 625 Alloy Fabricated by Pulsed Plasma Arc Deposition

NASA Astrophysics Data System (ADS)

Xu, Fujia; Lv, Yaohui; Liu, Yuxin; Xu, Binshi; He, Peng

Pulsed plasma arc deposition (PPAD) was successfully used to fabricate the Ni-based superalloy Inconel 625 samples. The effects of three heat treatment technologies on microstructure and mechanical properties of the as-deposited material were investigated. It was found that the as-deposited structure exhibited homogenous cellular dendrite structure, which grew epitaxially along the deposition direction. Moreover, some intermetallic phases including Laves phase and MC carbides were precipitated in the interdendritic region as a result of Nb segregation. Compared with the as-deposited microstructure, the direct aged (DA) microstructure changed little except the precipitation of hardening phases γ' and γ" (Ni3Nb), which enhanced the hardness and tensile strength. But the plastic property was inferior due to the existence of brittle Laves phase. After solution and aging heat treatment (STA), a large amount of Laves particles in the interdendritic regions were dissolved, resulting in the reduction of Nb segregation and the precipitation of needle-like δ (Ni3Nb) in the interdendritic regions and grain boundaries. The hardness and tensile strength were improved without sacrificing the ductility. By homogenization and STA heat treatment (HSTA), Laves particles were dissolved into the matrix completely and resulted in recrystallized large grains with bands of annealing twins. The primary MC particles and remaining phase still appeared in the matrix and grain boundaries. Compared with the as-deposited sample, the mechanical properties decreased severely as a result of the grain growth coarsening. The failure modes of all the tensile specimens were analyzed with fractography.

Rheological stratification of the Hormuz Salt Formation in Iran - microstructural study of the dirty and pure rock salts from the Kuh-e-Namak (Dashti) salt diapir

NASA Astrophysics Data System (ADS)

Závada, Prokop; Desbois, Guillaume; Urai, Janos; Schulmann, Karel; Rahmati, Mahmoud; Lexa, Ondrej; Wollenberg, Uwe

2014-05-01

Significant viscosity contrasts displayed in flow structures of a mountain namakier (Kuh-e-Namak - Dashti), between 'weak' terrestrial debris bearing rock salt types and 'strong' pure rock salt types are questioned for deformation mechanisms using detailed quantitative microstructural study including crystallographic preferred orientation (CPO) mapping of halite grains. While the solid impurity rich ("dirty") rock salts contain disaggregated siltstone and dolomite interlayers, "clean" salts (debris free) reveal microscopic hematite and remnants of abundant fluid inclusions in non-recrystallized cores of porphyroclasts. Although flow in both, the recrystallized dirty and clean salt types is accommodated by combined mechanisms of pressure-solution creep (PS), grain boundary sliding (GBS) and dislocation creep accommodated grain boundary migration (GBM), their viscosity contrasts are explained by significantly slower rates of intergranular diffusion and piling up of dislocations at hematite inclusions in clean salt types. Porphyroclasts of clean salts deform by semi-brittle and plastic mechanisms with intra-crystalline damage being induced also by fluid inclusions that explode in the crystals at high fluid pressures. Boudins of clean salt types with coarse grained and original sedimentary microstructure suggest that clean rock salts are associated with dislocation creep dominated power law flow in the source layer and the diapiric stem. Rheological contrasts between both rock salt classes apply in general for the variegated and terrestrial debris rich ("dirty") Lower Hormuz and the "clean" rock salt forming the Upper Hormuz, respectively, and suggest that large strain rate gradients likely exist along horizons of mobilized salt types of different composition and microstructure.

Effects of Laves phase particles on recovery and recrystallization behaviors of Nb-containing FeCrAl alloys

DOE PAGES

Sun, Zhiqian; Edmondson, Philip D.; Yamamoto, Yukinori

2017-11-15

The microstructures and mechanical properties of deformed and annealed Nb-containing FeCrAl alloys were investigated. Fine dispersion of Fe 2Nb-type Laves phase particles was observed in the bcc-Fe matrix after applying a thermomechanical treatment, especially along grain/subgrain boundaries, which effectively stabilized the recovered and recrystallized microstructures compared with the Nb-free FeCrAl alloy. The stability of recovered areas increased with Nb content up to 1 wt%. The recrystallized grain structure in Nb-containing FeCrAl alloys consisted of elongated grains along the rolling direction with a weak texture when annealed below 1100 °C. An abnormal relationship between recrystallized grain size and annealing temperature wasmore » found. Microstructural inhomogeneity in the deformed and annealed states was explained based on the Taylor factor. Annealed Nb-containing FeCrAl alloys showed a good combination of strength and ductility, which is desirable for their application as fuel cladding in light-water reactors.« less

Strengthening and toughening mechanisms in low-c microalloyed martensitic steel as influenced by austenite conditioning

NASA Astrophysics Data System (ADS)

Kennett, Shane C.

Three low-carbon ASTM A514 microalloyed steels were used to assess the effects of austenite conditioning on the microstructure and mechanical properties of martensite. A range of prior austenite grain sizes with and without thermomechanical processing were produced in a Gleeble RTM 3500 and direct-quenched. Samples in the as-quenched, low temperature tempered, and high temperature tempered conditions were studied. The microstructure was characterized with scanning electron microscopy, electron backscattered diffraction, transmission electron microscopy, and x-ray diffraction. The uniaxial tensile properties and Charpy V-notch properties were measured and compared with the microstructural features (prior austenite grain size, packet size, block size, lath boundaries, and dislocation density). For the equiaxed prior austenite grain conditions, prior austenite grain size refinement decreases the packet size, decreases the block size, and increases the dislocation density of as-quenched martensite. However, after high temperature tempering the dislocation density decreases with prior austenite grain size refinement. Thermomechanical processing increases the low angle substructure, increases the dislocation density, and decreases the block size of as-quenched martensite. The dislocation density increase and block size refinement is sensitive to the austenite grain size before ausforming. The larger prior austenite grain size conditions have a larger increase in dislocation density, but the small prior austenite grain size conditions have the largest refinement in block size. Additionally, for the large prior austenite grain size conditions, the packet size increases with thermomechanical processing. The strength of martensite is often related to an effective grain size or carbon concentration. For the current work, it was concluded that the strength of martensite is primarily controlled by the dislocation density and dislocation substructure; which is related to a grain size and carbon concentration. In the microyielding regime, the strength and work hardening is related to the motion of unpinned dislocation segments. However, with tensile strain, a dislocation cell structure is developed and the flow strength (greater than 1% offset) is controlled by the dislocation density following a Taylor hardening model, thereby ruling out any grain size effects on the flow strength. Additionally, it is proposed that lath boundaries contribute to strength. It is shown that the strength differences associated with thermomechanically processed steels can be fully accounted for by dislocation density differences and the effect of lath boundaries. The low temperature ductile to brittle transition of martensite is controlled by the martensite block size, packet size, and prior austenite grain size. However, the effect of block size is likely small in comparison. The ductile to brittle transition temperature is best correlated to the inverse square root of the martensite packet size because large crack deflections are typical at packet boundaries.

Analysis of stress corrosion cracking in alloy 718 following commercial reactor exposure

DOE PAGES

Leonard, Keith J.; Gussev, Maxim N.; Stevens, Jacqueline N.; ...

2015-08-24

Alloy 718 is generally considered a highly corrosion-resistant material but can still be susceptible to stress corrosion cracking (SCC). The combination of factors leading to SCC susceptibility in the alloy is not always clear enough. In this paper, alloy 718 leaf spring (LS) materials that suffered stress corrosion damage during two 24-month cycles in pressurized water reactor service, operated to >45 MWd/mtU burn-up, was investigated. Compared to archival samples fabricated through the same processing conditions, little microstructural and property changes occurred in the material with in-service irradiation, contrary to high dose rate laboratory-based experiments reported in literature. Though the lackmore » of delta phase formation along grain boundaries would suggest a more SCC resistant microstructure, grain boundary cracking in the material was extensive. Crack propagation routes were explored through focused ion beam milling of specimens near the crack tip for transmission electron microscopy as well as in polished plan view and cross-sectional samples for electron backscatter diffraction analysis. It has been shown in this study that cracks propagated mainly along random high-angle grain boundaries, with the material around cracks displaying a high local density of dislocations. The slip lines were produced through the local deformation of the leaf spring material above their yield strength. Also, the cause for local SCC appears to be related to oxidation of both slip lines and grain boundaries, which under the high in-service stresses resulted in crack development in the material.« less

Dynamic Recrystallization of the Constituent γ Phase and Mechanical Properties of Ti-43Al-9V-0.2Y Alloy Sheet

PubMed Central

Zhang, Yu; Wang, Xiaopeng; Kong, Fantao

2017-01-01

A crack-free Ti-43Al-9V-0.2Y alloy sheet was successfully fabricated via hot-pack rolling at 1200 °C. After hot-rolling, the β/γ lamellar microstructure of the as-forged TiAl alloy was completely converted into a homogeneous duplex microstructure with an average γ grain size of 10.5 μm. The dynamic recrystallization (DRX) of the γ phase was systematically investigated. A recrystallization fraction of 62.5% was obtained for the γ phase in the TiAl alloy sheet, when a threshold value of 0.8° was applied to the distribution of grain orientation spread (GOS) values. The high strain rate and high stress associated with hot-rolling are conducive for discontinuous dynamic recrystallization (DDRX) and continuous dynamic recrystallization (CDRX), respectively. A certain high-angle boundary (HAGB: θ = 89° ± 3°<100>), which is associated with DDRX, occurs in both the recrystallized and deformed γ grains. The twin boundaries play an important role in the DDRX of the γ phase. Additionally, the sub-structures and sub-boundaries originating from low-angle boundaries in the deformed grains also indicate that CDRX occurs. The mechanical properties of the alloy sheet were determined at both room and elevated temperatures. At 750 °C, the alloy sheet exhibited excellent elongation (53%), corresponding to a failure strength of 467 MPa. PMID:28914797

Influence of Yb{sub 2}O{sub 3} on electrical and microstructural characteristics of CaCu{sub 3}Ti{sub 4}O{sub 12} ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

He, Kai; State Key Laboratory of Electronic Thin Films and Integrated Devices, University of Electronic Science and Technology of China, Chengdu 610054; Luo, Yun

2015-09-15

Graphical abstract: Some Yb atoms entered in the lattice of CCTO substituted the Ca sites, the rest of Yb atoms concentrated at grain boundaries decreased the grain size. The dielectric constant was decreased by Yb doping. The dielectric loss of the CCTO could be greatly reduced at low frequency. - Highlights: • Yb atoms may take the place of Ca sites and concentrate at grain boundaries. • Tiny second phase corresponding to Yb may decrease the grain size. • Decrease of the grain size leads to the decrease of dielectric constant. • Yb doping could decrease the dielectric loss ofmore » CCTO. - Abstract: This paper focuses on the remarkable effects of Yb{sub 2}O{sub 3} doping on the microstructure and dielectric characteristics of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO). Samples were prepared by the solid phase reaction method and sintered in air at 1030 °C for 12 h. X-ray diffraction and X-ray photoelectron spectroscopy studies confirm that the primary phase is CCTO. Some Yb{sup 3+} ions may substitute into the Ca site at the center or zenith sites of the CCTO lattice hexahedron, while the rest of the Yb atoms may concentrate at grain boundaries. The grain size of Yb{sub 2}O{sub 3}-doped CCTO ceramics were examined by scanning electron microscopy and demonstrate sharp grain size reduction with Yb{sub 2}O{sub 3} doping. From dielectric property measurements, the Yb{sub 2}O{sub 3} doping reduces the dielectric constant of CCTO, and the dielectric loss is also reduced.« less

Microstructural Evolution during DPRM Process of Semisolid Ledeburitic D2 Tool Steel

PubMed Central

Mohammed, M. N.; Omar, M. Z.; Syarif, J.; Sajuri, Z.; Salleh, M. S.; Alhawari, K. S.

2013-01-01

Semisolid metal processing is a relatively new technology that offers several advantages over liquid processing and solid processing because of the unique behaviour and characteristic microstructure of metals in this state. With the aim of finding a minimum process chain for the manufacture of high-quality production at minimal cost for forming, the microstructural evolution of the ledeburitic AISI D2 tool steel in the semisolid state was studied experimentally. The potential of the direct partial remelting (DPRM) process for the production of AISI D2 with a uniform globular microstructure was revealed. The liquid fraction was determined using differential scanning calorimetry. The microstructures of the samples were investigated using an optical microscope and a scanning electron microscope equipped with an energy dispersive spectroscopy analyser, while X-ray phase analysis was performed to identify the phase evolution and the type of carbides. Mechanical characterisation was completed by hardness measurements. The typical microstructure after DPRM consists of metastable austenite which was located particularly in the globular grains (average grain size about 50 μm), while the remaining interspaces were filled by precipitated eutectic carbides on the grain boundaries and lamellar network. PMID:24223510

Microstructural evolution during DPRM process of semisolid ledeburitic D2 tool steel.

PubMed

Mohammed, M N; Omar, M Z; Syarif, J; Sajuri, Z; Salleh, M S; Alhawari, K S

2013-01-01

Semisolid metal processing is a relatively new technology that offers several advantages over liquid processing and solid processing because of the unique behaviour and characteristic microstructure of metals in this state. With the aim of finding a minimum process chain for the manufacture of high-quality production at minimal cost for forming, the microstructural evolution of the ledeburitic AISI D2 tool steel in the semisolid state was studied experimentally. The potential of the direct partial remelting (DPRM) process for the production of AISI D2 with a uniform globular microstructure was revealed. The liquid fraction was determined using differential scanning calorimetry. The microstructures of the samples were investigated using an optical microscope and a scanning electron microscope equipped with an energy dispersive spectroscopy analyser, while X-ray phase analysis was performed to identify the phase evolution and the type of carbides. Mechanical characterisation was completed by hardness measurements. The typical microstructure after DPRM consists of metastable austenite which was located particularly in the globular grains (average grain size about 50 μ m), while the remaining interspaces were filled by precipitated eutectic carbides on the grain boundaries and lamellar network.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Taheri, M; Teslich, N; Lu, J P

An in situ method for studying the role of laser energy on the microstructural evolution of polycrystalline Si is presented. By monitoring both laser energy and microstructural evolution simultaneously in the dynamic transmission electron microscope, information on grain size and defect concentration can be correlated directly with processing conditions. This proof of principle study provides fundamental scientific information on the crystallization process that has technological importance for the development of thin film transistors. In conclusion, we successfully developed a method for studying UV laser processing of Si films in situ on nanosecond time scales, with ultimate implications for TFT applicationmore » improvements. In addition to grain size distribution as a function of laser energy density, we found that grain size scaled with laser energy in general. We showed that nanosecond time resolution allowed us to see the nucleation and growth front during processing, which will help further the understanding of microstructural evolution of poly-Si films for electronic applications. Future studies, coupled with high resolution TEM, will be performed to study grain boundary migration, intergranular defects, and grain size distribution with respect to laser energy and adsorption depth.« less

MARMOT simulations of Xe segregation to grain boundaries in UO2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Andersson, Anders D.; Tonks, Michael; Casillas, Luis

2012-06-20

Diffusion of Xe and U in UO{sub 2} is controlled by vacancy mechanisms and under irradiation the formation of mobile vacancy clusters is important. We derive continuum thermodynamic and diffusion models for Xe and U in UO{sub 2} based on the vacancy and cluster diffusion mechanisms established from recent density functional theory (DFT) calculations. Segregation of defects to grain boundaries in UO{sub 2} is described by combining the diffusion model with models of the interaction between Xe atoms and vacancies with grain boundaries derived from separate atomistic calculations. The diffusion and segregation models are implemented in the MOOSE/MARMOT (MBM) finitemore » element (FEM) framework and we simulate Xe redistribution for a few simple microstructures. In this report we focus on segregation to grain boundaries. The U or vacancy diffusion model as well as the coupled diffusion of vacancies and Xe have also been implemented, but results are not included in this report.« less

Microstructural defects in He-irradiated polycrystalline α-SiC at 1000 °C

NASA Astrophysics Data System (ADS)

Han, Wentuo; Li, Bingsheng

2018-06-01

In order to investigate the effect of the high-temperature irradiation on microstructural evolutions of the polycrystalline SiC, an ion irradiation at 1000 °C with the 500 keV He2+ was imposed to the α-SiC. The platelets, He bubbles, dislocation loops, and particularly, their interaction with the stacking fault and grain boundaries were focused on and characterized by the cross-sectional transmission electron microscopy (XTEM). The platelets expectably exhibit a dominant plane of (0001), while planes of (01-10) and (10-16) are also found. Inside the platelet, the over-pressurized bubbles exist and remarkably cause a strong-strain zone surrounding the platelet. The disparate roles between the grain boundaries and stacking faults in interacting with the bubbles and loops are found. The results are compared with the previous weighty findings and discussed.

Microstructural evolution and precipitation behavior in heat affected zone of Inconel 625 and AISI 904L dissimilar welds

NASA Astrophysics Data System (ADS)

Senthur Prabu, S.; Devendranath Ramkumar, K.; Arivazhagan, N.

2017-11-01

In the present investigation an attempt has been made to join the dissimilar combination of Inconel 625 super alloy and super austenitic stainless steel (AISI 904L) using manual multi-pass continuous current gas tungsten arc (CCGTA) welding processes. Two different filler wires such as ERNiCrMo-4 and ERNiCrCoMo-1 have been used to compare the metallurgical properties of these welded joints. Both optical microscopy and scanning electron microscopy techniques were adopted to disseminate the microstructure traits of these weldments. Formation of secondary phases at the HAZ and weld interface of AISI 904L was witnessed while using the ERNiCrCoMo-1 filler, along with Solidification Grain Boundary (SGB) and Migrated Grain Boundary (MGB) were also observed at the weld zone.

Study of the Microstructure and Cracking Mechanisms of Hastelloy X Produced by Laser Powder Bed Fusion.

PubMed

Marchese, Giulio; Basile, Gloria; Bassini, Emilio; Aversa, Alberta; Lombardi, Mariangela; Ugues, Daniele; Fino, Paolo; Biamino, Sara

2018-01-11

Hastelloy X (HX) is a Ni-based superalloy which suffers from high crack susceptibility during the laser powder bed fusion (LPBF) process. In this work, the microstructure of as-built HX samples was rigorously investigated to understand the main mechanisms leading to crack formation. The microstructural features of as-built HX samples consisted of very fine dendrite architectures with dimensions typically less than 1 µm, coupled with the formation of sub-micrometric carbides, the largest ones were mainly distributed along the interdendritic regions and grain boundaries. From the microstructural analyses, it appeared that the formation of intergranular carbides provided weaker zones, which combined with high thermal residual stresses resulted in hot cracks formation along the grain boundaries. The carbides were extracted from the austenitic matrix and characterized by combining different techniques, showing the formation of various types of Mo-rich carbides, classified as M₆C, M 12 C and M n C m type. The first two types of carbides are typically found in HX alloy, whereas the last one is a metastable carbide probably generated by the very high cooling rates of the process.

Microstructural characterization of dissimilar welds between Incoloy 800H and 321 Austenitic Stainless Steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sayiram, G., E-mail: sayiram.g@vit.ac.in; Arivazhagan, N.

2015-04-15

In this work, the microstructural character of dissimilar welds between Incoloy 800H and 321 Stainless Steel has been discussed. The microscopic examination of the base metals, fusion zones and interfaces was characterized using an optical microscope and scanning electron microscopy. The results revealed precipitates of Ti (C, N) in the austenitic matrix along the grain boundaries of the base metals. Migration of grain boundaries in the Inconel 82 weld metal was very extensive when compared to Inconel 617 weldment. Epitaxial growth was observed in the 617 weldment which increases the strength and ductility of the weld metal. Unmixed zone nearmore » the fusion line between 321 Stainless Steel and Inconel 82 weld metal was identified. From the results, it has been concluded that Inconel 617 filler metal is a preferable choice for the joint between Incoloy 800H and 321 Stainless Steel. - Highlights: • Failure mechanisms produced by dissimilar welding of Incoloy 800H to AISI 321SS • Influence of filler wire on microstructure properties • Contemplative comparisons of metallurgical aspects of these weldments • Microstructure and chemical studies including metallography, SEM–EDS • EDS-line scan study at interface.« less

Study of the Microstructure and Cracking Mechanisms of Hastelloy X Produced by Laser Powder Bed Fusion

PubMed Central

Basile, Gloria; Bassini, Emilio; Ugues, Daniele; Fino, Paolo

2018-01-01

Hastelloy X (HX) is a Ni-based superalloy which suffers from high crack susceptibility during the laser powder bed fusion (LPBF) process. In this work, the microstructure of as-built HX samples was rigorously investigated to understand the main mechanisms leading to crack formation. The microstructural features of as-built HX samples consisted of very fine dendrite architectures with dimensions typically less than 1 µm, coupled with the formation of sub-micrometric carbides, the largest ones were mainly distributed along the interdendritic regions and grain boundaries. From the microstructural analyses, it appeared that the formation of intergranular carbides provided weaker zones, which combined with high thermal residual stresses resulted in hot cracks formation along the grain boundaries. The carbides were extracted from the austenitic matrix and characterized by combining different techniques, showing the formation of various types of Mo-rich carbides, classified as M6C, M12C and MnCm type. The first two types of carbides are typically found in HX alloy, whereas the last one is a metastable carbide probably generated by the very high cooling rates of the process. PMID:29324658

Effect of arsenic content and quenching temperature on solidification microstructure and arsenic distribution in iron-arsenic alloys

NASA Astrophysics Data System (ADS)

Xin, Wen-bin; Song, Bo; Huang, Chuan-gen; Song, Ming-ming; Song, Gao-yang

2015-07-01

The solidification microstructure, grain boundary segregation of soluble arsenic, and characteristics of arsenic-rich phases were systematically investigated in Fe-As alloys with different arsenic contents and quenching temperatures. The results show that the solidification microstructures of Fe-0.5wt%As alloys consist of irregular ferrite, while the solidification microstructures of Fe-4wt%As and Fe-10wt%As alloys present the typical dendritic morphology, which becomes finer with increasing arsenic content and quenching temperature. In Fe-0.5wt%As alloys quenched from 1600 and 1200°C, the grain boundary segregation of arsenic is detected by transmission electron microscopy. In Fe-4wt%As and Fe-10wt%As alloys quenched from 1600 and 1420°C, a fully divorced eutectic morphology is observed, and the eutectic Fe2As phase distributes discontinuously in the interdendritic regions. In contrast, the eutectic morphology of Fe-10wt%As alloy quenched from 1200°C is fibrous and forms a continuous network structure. Furthermore, the area fraction of the eutectic Fe2As phase in Fe-4wt%As and Fe-10wt%As alloys increases with increasing arsenic content and decreasing quenching temperature.

In-situ Indentation and Correlated Precession Electron Diffraction Analysis of a Polycrystalline Cu Thin Film

NASA Astrophysics Data System (ADS)

Guo, Qianying; Thompson, Gregory B.

2018-04-01

In-situ TEM nanoindentation of a polycrystalline Cu film was cross-correlated with precession electron diffraction (PED) to quantify the microstructural evolution. The use of PED is shown to clearly reveal features, such as grain size, that are easily masked by diffraction contrast created by the deformation. Using PED, the accompanying grain refinement and change in texture as well as the preservation of specific grain boundary structures, including a ∑3 boundary, under the indent impression were quantified. The nucleation of dislocations, evident in low-angle grain boundary formations, was also observed under the indent. PED quantification of texture gradients created by the indentation process linked well to bend contours observed in the bright-field images. Finally, PED enabled generating a local orientation spread map that gave an approximate estimation of the spatial distribution of strain created by the indentation impression.

Nanoscale phase transition behavior of shape memory alloys — closed form solution of 1D effective modelling

NASA Astrophysics Data System (ADS)

Li, M. P.; Sun, Q. P.

2018-01-01

We investigate the roles of grain size (lg) and grain boundary thickness (lb) on the stress-induced phase transition (PT) behaviors of nanocrystalline shape memory alloys (SMAs) by using a Core-shell type "crystallite-amorphous composite" model. A non-dimensionalized length scale lbarg(=lg /lb) is identified as the governing parameter which is indicative of the energy competition between the crystallite and the grain boundary. Closed form analytical solutions of a reduced effective 1D model with embedded microstructure length scales of lg and lb are presented in this paper. It is shown that, with lbarg reduction, the energy of the elastic non-transformable grain boundary will gradually become dominant in the phase transition process, and eventually bring fundamental changes of the deformation behaviors: breakdown of two-phase coexistence and vanishing of superelastic hysteresis. The predictions are supported by experimental data of nanocrystalline NiTi SMAs.

Crystallographic texture in oxide-dispersion-strengthened alloys

NASA Technical Reports Server (NTRS)

Whittenberger, J. D.

1982-01-01

Crystallographic and elastic moduli data are presented which document the degree of texture in several oxide dispersion-strengthened (ODS) nickel-base alloys. The existence of strong crystallographic textures in such multicrystalline alloys is considered important, since the small angle grain boundaries may be partially responsible for creep threshold stresses. Gleiter (1979) has shown that ideal, low energy boundaries will act as vacancy sources only when the applied stress is greater than a threshold stress, while large angle grain boundaries will emit vacancies at all stress levels. The continued operation of a net vacancy in an ODS alloy must be avoided, since it will lead to a localized disruption of the microstructure.

The Influence of Impurities and Metallic Capping Layers on the Microstructure of Copper Interconnects

NASA Astrophysics Data System (ADS)

Rizzolo, Michael

As copper interconnects have scaled to ever smaller dimensions on semiconductor devices, the microstructure has become increasingly detrimental for performance and reliability. Small grains persist in interconnects despite annealing at high temperatures, leading to higher line resistance and more frequent electromigration-induced failures. Conventionally, it was believed that impurities from the electrodeposition pinned grain growth, but limitations in analytical techniques meant the effect was inferred rather than observed. Recent advances in analytical techniques, however, have enabled this work to quantify impurity content, location, and diffusion in relation to microstructural changes in electroplated copper. Surface segregation of impurities during the initial burst of grain growth was investigated. After no surface segregation was observed, a microfluidic plating cell was constructed to plate multilayer films with regions of intentionally high and low impurity concentrations to determine if grain growth could be pinned by the presence of impurities; it was not. An alternate mechanism for grain boundary pinning based on the texture of the seed layer is proposed, supported by time-resolved transmission electron microscopy and transmission electron backscatter diffraction data. The suggested model posits that the seed in narrow features has no preferred orientation, which results in rapid nucleation of subsurface grains in trench regions prior to recrystallization from the overburden down. These rapidly growing grains are able to block off several trenches from the larger overburden grains, inhibiting grain growth in narrow features. With this knowledge in hand, metallic capping layers were employed to address the problematic microstructure in 70nm lines. The capping layers (chromium, nickel, zinc, and tin) were plated on the copper overburden prior to annealing to manipulate the stress gradient and microstructural development during annealing. It appeared that regardless of as-plated stress, nickel capping altered the recrystallized texture of the copper over patterned features. The nickel capping also caused a 2x increase in the number of advantageous 'bamboo' grains that span the entire trench, which effectively block electromigration pathways. These data provides a more fundamental understanding of manipulating the microstructure in copper interconnects using pre-anneal capping layers, and demonstrates a strategy to improve the microstructure beyond the capabilities of simple annealing.

Microstructure characterization via stereological relations — A shortcut for beginners

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pabst, Willi, E-mail: pabstw@vscht.cz; Gregorová, Eva; Uhlířová, Tereza

Stereological relations that can be routinely applied for the quantitative characterization of microstructures of heterogeneous single- and two-phase materials via global microstructural descriptors are reviewed. It is shown that in the case of dense, single-phase polycrystalline materials (e.g., transparent yttrium aluminum garnet ceramics) two quantities have to be determined, the interface density (or, equivalently, the mean chord length of the grains) and the mean curvature integral density (or, equivalently, the Jeffries grain size), while for two-phase materials (e.g., highly porous, cellular alumina ceramics), one additional quantity, the volume fraction (porosity), is required. The Delesse–Rosiwal law is recalled and size measuresmore » are discussed. It is shown that the Jeffries grain size is based on the triple junction line length density, while the mean chord length of grains is based on the interface density (grain boundary area density). In contrast to widespread belief, however, these two size measures are not alternative, but independent (and thus complementary), measures of grain size. Concomitant with this fact, a clear distinction between linear and planar grain size numbers is proposed. Finally, based on our concept of phase-specific quantities, it is shown that under certain conditions it is possible to define a Jeffries size also for two-phase materials and that the ratio of the mean chord length and the Jeffries size has to be considered as an invariant number for a certain type of microstructure, i.e., a characteristic value that is independent of the absolute size of the microstructural features (e.g., grains, inclusions or pores). - Highlights: • Stereology-based image analysis is reviewed, including error considerations. • Recipes are provided for measuring global metric microstructural descriptors. • Size measures are based on interface density and mean curvature integral density. • Phase-specific quantities and a generalized Jeffries size are introduced. • Linear and planar grain size numbers are clearly distinguished and explained.« less

Hierarchical creep cavity formation in an ultramylonite and implications for phase mixing

NASA Astrophysics Data System (ADS)

Gilgannon, James; Fusseis, Florian; Menegon, Luca; Regenauer-Lieb, Klaus; Buckman, Jim

2017-12-01

Establishing models for the formation of well-mixed polyphase domains in ultramylonites is difficult because the effects of large strains and thermo-hydro-chemo-mechanical feedbacks can obscure the transient phenomena that may be responsible for domain production. We use scanning electron microscopy and nanotomography to offer critical insights into how the microstructure of a highly deformed quartzo-feldspathic ultramylonite evolved. The dispersal of monomineralic quartz domains in the ultramylonite is interpreted to be the result of the emergence of synkinematic pores, called creep cavities. The cavities can be considered the product of two distinct mechanisms that formed hierarchically: Zener-Stroh cracking and viscous grain-boundary sliding. In initially thick and coherent quartz ribbons deforming by grain-size-insensitive creep, cavities were generated by the Zener-Stroh mechanism on grain boundaries aligned with the YZ plane of finite strain. The opening of creep cavities promoted the ingress of fluids to sites of low stress. The local addition of a fluid lowered the adhesion and cohesion of grain boundaries and promoted viscous grain-boundary sliding. With the increased contribution of viscous grain-boundary sliding, a second population of cavities formed to accommodate strain incompatibilities. Ultimately, the emergence of creep cavities is interpreted to be responsible for the transition of quartz domains from a grain-size-insensitive to a grain-size-sensitive rheology.

Effect of temperature on the nano/microstructure and mechanical behavior of nanotwinned Ag films

DOE PAGES

Zhang, Huan; Geng, Jie; Ott, Ryan T.; ...

2015-06-24

In situ and ex situ annealed nanotwinned (NT) Ag thin films have been investigated by TEM and tensile testing to reveal the thermal stability of the twin boundaries, grain boundaries, dislocation densities, and their respective influence of the macroscopic yield stress. The NT Ag films synthesized by magnetron sputtering form both coherent (CTB, Σ3{111}) and incoherent (ITB, Σ3{112}) twin boundaries that are thermally stable up to 473 K (200 Celsius), i.e., no obvious changes in grain size, twin spacing, and yield stress. In situ TEM observations show the dislocations become mobile at 453 K (180 Celsius) resulting in dislocation annihilationmore » primarily at twin and grain boundaries. Rotation of grains with low-angle grain boundaries was observed during in situ heating, resulting in the growth of columnar grains above 453 K (180 Celsius). However, no noticeable changes in the spacings of CTBs were observed during the entire in situ and ex situ annealing [up to 873 K (600 Celsius)]. The increase in grain size and concomitant decrease in yield stress following annealing at various temperatures can be described by the Hall-Petch relationship, demonstrating that grain size rather than twin spacing is most sensitive to thermal annealing and plays a dominant role in the deformation of NT Ag films.« less

Boundary migration in a 3D deformed microstructure inside an opaque sample

DOE PAGES

Zhang, Y. B.; Budai, J. D.; Tischler, J. Z.; ...

2017-06-30

How boundaries surrounding recrystallization grains migrate through the 3D network of dislocation boundaries in deformed crystalline materials is unknown and critical for the resulting recrystallized crystalline materials. Furthermore, by using X-ray Laue diffraction microscopy, we show for the first time the migration pattern of a typical recrystallization boundary through a well-characterized deformation matrix. The data provide a unique possibility to investigate effects of both boundary misorientation and plane normal on the migration, information which cannot be accessed with any other techniques. Our results show that neither of these two parameters can explain the observed migration behavior. Instead we suggest thatmore » the subdivision of the deformed microstructure ahead of the boundary plays the dominant role. Our experimental observations challenge the assumptions of existing recrystallization theories, and set the stage for determination of mobilities of recrystallization boundaries.« less

Bulk Nanolaminated Nickel: Preparation, Microstructure, Mechanical Property, and Thermal Stability

NASA Astrophysics Data System (ADS)

Liu, Fan; Yuan, Hao; Goel, Sunkulp; Liu, Ying; Wang, Jing Tao

2018-02-01

A bulk nanolaminated (NL) structure with distinctive fractions of low- and high-angle grain boundaries ( f LAGBs and f HAGBs) is produced in pure nickel, through a two-step process of primary grain refinement by equal-channel angular pressing (ECAP), followed by a secondary geometrical refinement via liquid nitrogen rolling (LNR). The lamellar boundary spacings of 2N and 4N nickel are refined to 40 and 70 nm, respectively, and the yield strength of the NL structure in 2N nickel reaches 1.5 GPa. The impacts of the deformation path, material purity, grain boundary (GB) misorientation, and energy on the microstructure, refinement ability, mechanical strength, and thermal stability are investigated to understand the inherent governing mechanisms. GB migration is the main restoration mechanism limiting the refinement of an NL structure in 4N nickel, while in 2N nickel, shear banding occurs and mediates one-fifth of the total true normal rolling strain at the mesoscale, restricting further refinement. Three typical structures [ultrafine grained (UFG), NL with low f LAGBs, and NL with high f LAGBs] obtained through three different combinations of ECAP and LNR were studied by isochronal annealing for 1 hour at temperatures ranging from 433 K to 973 K (160 °C to 700 °C). Higher thermal stability in the NL structure with high f LAGBs is shown by a 50 K (50 °C) delay in the initiation temperature of recrystallization. Based on calculations and analyses of the stored energies of deformed structures from strain distribution, as characterized by kernel average misorientation (KAM), and from GB misorientations, higher thermal stability is attributed to high f LAGBs in this type of NL structure. This is confirmed by a slower change in the microstructure, as revealed by characterizing its annealing kinetics using KAM maps.

Characterization of the martensite phase formed during hydrogen ion irradiation in austenitic stainless steel

NASA Astrophysics Data System (ADS)

Jin, Hyung-Ha; Lim, Sangyeob; Kwon, Junhyun

2017-10-01

Microstructural changes in austenitic stainless steel caused by hydrogen ion irradiation were investigated using transmission electron microscopy (TEM). It has been confirmed that the irradiation induced the formation of martensite along the grain boundary; the martensite phase exhibited a crystal orientation relationship with the adjacent austenite phase. The results of this study also indicate that the concentration of Cr in the martensite phase is lower compared to that in the austenite matrix. The TEM results showed the development of asymmetric radiation-induced segregation (RIS) near the grain boundary, which leads to local changes in the chemical composition such as reduction of Cr near the grain boundary. The asymmetric RIS serves as a prerequisite for the formation of the martensite under hydrogen irradiation.

Microstructure of Hot Rolled 1.0C-1.5Cr Bearing Steel and Subsequent Spheroidization Annealing

NASA Astrophysics Data System (ADS)

Li, Zhen-Xing; Li, Chang-Sheng; Zhang, Jian; Li, Bin-Zhou; Pang, Xue-Dong

2016-07-01

The effect of final rolling temperature and cooling process on the microstructure of 1.0C-1.5Cr bearing steel was studied, and the relationship between the microstructure parameters and subsequent spheroidization annealing was analyzed. The results indicate that the increase of water-cooling rate after hot rolling and the decrease of final cooling temperature are beneficial to reducing both the pearlite interlamellar spacing and pearlite colony size. Prior austenite grain size can be reduced by decreasing the final rolling temperature and increasing the water-cooling rate. When the final rolling temperature was controlled around 1103 K (830 °C), the subsequent cooling rate was set to 10 K/s and final cooling temperature was 953 K (680 °C), the precipitation of grain boundary cementite was suppressed effectively and lots of rod-like cementite particles were observed in the microstructure. Interrupted quenching was employed to study the dissolution behavior of cementite during the austenitizing at 1073 K (800 °C). The decrease of both pearlite interlamellar spacing and pearlite colony size could facilitate the initial dissolution and fragmentation of cementite lamellae, which could shorten the spheroidization time. The fragmentation of grain boundary cementite tends to form large-size undissolved cementite particles. With the increase of austenitizing time from 20 to 300 minutes, mean diameter of undissolved cementite particles increases, indicating the cementite particle coarsening and cementite dissolution occuring simultaneously. Mean diameter of cementite particles in the final spheroidized microstructure is proportional to the mean diameter of undissolved cementite particles formed during partial austenitizing.

Microstructural effects on the room and elevated temperature low cycle fatigue behavior of Waspaloy. M.S. Thesis Final Report

NASA Technical Reports Server (NTRS)

Lerch, B. A.

1982-01-01

Longitudinal specimens of Waspaloy containing either coarse grains with small gamma or fine grains with large gamma were tested in air at a frequency of 0.33 Hz or 0.50 Hz. The coarse grained structures exhibited planar slip on (III) planes and precipitate shearing at all temperatures. Cracks initiated by a Stage 1 mechanism and propagated by a striation forming mechanism. At 700 C and 800 C, cleavage and intergranular cracking were observed. Testing at 500 C, 700 C, and 800 C caused precipitation of grain boundary carbides. At 700 C, carbides precipitated on slip bands. The fine grained structures exhibited planar slip on (111) planes. Dislocations looped the large gamma precipitates. This structure led to stress saturation and propagation was observed. Increasing temperatures resulted in increased specimen oxidation for both heat treatments. Slip band and grain boundary oxidation were observed. At 800 C, oxidized grain boundaries were cracked by intersecting slip bands which resulted in intergranular failure. The fine specimens had crack initiation later in the fatigue life, but with more rapid propagation crack propagation.

Can grain size sensitive creep lubricate faults during earthquake propagation?

NASA Astrophysics Data System (ADS)

De Paola, N.; Holdsworth, R.; Viti, C.; Collettini, C.; Bullock, R. J.; Faoro, I.

2014-12-01

In the shallow portion of crustal fault zones, fracturing and cataclasis are thought to be the dominant processes during earthquake propagation. In the lower crust/upper mantle, viscous flow is inferred to facilitate aseismic creep along shear zones. Recent studies show that slip zones (SZs), in natural and experimental carbonate seismic faults, are made of nanograins with a polygonal texture, a microstructure consistent with deformation by grain boundary sliding (GBS) mechanisms. Friction experiments performed on calcite fine-grained gouges, at speed v = 1 ms-1, normal stress sn = 18 MPa, displacements d = 0.009-1.46 m, and room temperature and humidity, show a four stage-evolution of the fault strength: SI) attainment of initial value, f = 0.67; SII) increase up to peak value f = 0.82; SIII) sudden decrease to low steady-state value, f = 0.18; and SIV) sudden increase to final value, f = 0.44, during sample deceleration. Samples recovered at the end of each displacement-controlled experiments (Stages I-IV) show the following microstructures evolution of the SZ material, which is: SI) poorly consolidated, and made of fine-grained (1 < D < 5 microns), angular clasts formed by brittle fracturing and cataclasis; SII) cohesive, and made of larger clasts of calcite (D ≈ 1 microns), exhibiting a high density of free dislocations and hosting subgrains (D ≤ 200 nm), dispersed within calcite nanograins. SIII) made of nanograin aggregates exhibiting polygonal grain boundaries, and 120° triple junctions between equiaxial grains. The grains display no preferred elongation, no crystal preferred orientation and low free dislocation densities, possibly due to high temperature (> 900 C) GBS creep deformation. Our microstructural observations suggest that GBS mechanisms can operate in geological materials deformed at high strain rates along frictionally heated seismogenic slip surfaces. The observed microstructures in experimental slip zones are strikingly similar to those predicted by theoretical studies, and to those observed during experiments on metals and fine-grained carbonates deformed at T > 900 °C, where superplastic behaviour due to GBS has been inferred. A regime of frictionally-induced GBS could thus account for the dynamic weakening of carbonate faults during earthquake propagation in nature.

Recrystallization Behavior in SAC305 and SAC305 + 3.0POSS Solder Joints Under Thermal Shock

NASA Astrophysics Data System (ADS)

Han, Jing; Gu, Penghao; Ma, Limin; Guo, Fu; Liu, Jianping

2018-04-01

Sn-3.0Ag-0.5Cu (SAC305) and SAC305 + 3.0 polyhedral oligomeric silsesquioxanes (POSS) ball grid array (BGA) assemblies have been prepared, observed, and subjected to thermal shock. The microstructure and grain orientation evolution of the solder joints located at the same position of the package were characterized by scanning electron microscopy and electron backscattering diffraction, respectively. The results showed that the microstructure of the solder joints was refined by addition of POSS particles. In addition, compared with the single-grained or tricrystal joints normally observed in SAC305 BGA solder joints, the frequency of single-grained as-reflowed SAC305 + 3.0POSS BGA joints was greatly reduced, and the solder joints were typically composed of multicrystals with orientations separated by high-angle grain boundaries. These multicrystal joints appear to be obtained by dominant tricrystals or double tricrystals with deviation of the preferred [110] and [1\\bar{1}0] growth directions of Sn dendrites in Sn-Ag-based solder alloys during solidification from the melt. After 928 thermal shock cycles, the SAC305 solder joint had large-area recrystallization and cracks in contrast to the SAC305 + 3.0POSS solder joint located at the same position of the package, indicating that addition of POSS to SAC305 solder joints may contribute to postponement of recrystallization and subsequent crack initiation and propagation along recrystallized grain boundaries by pinning grain boundaries and movement of dislocations. This finding also confirms the double tricrystal solidification twinning nucleation behavior in Pb-free solder joints.

High-Resolution Characterizations of Grain Boundary Damage and Stress Corrosion Cracks in Cold-Rolled Alloy 690

NASA Astrophysics Data System (ADS)

Bruemmer, S. M.; Olszta, M. J.; Toloczko, M. B.; Thomas, L. E.

Unidirectional cold rolling has been shown to promote intergranular stress corrosion cracking (IGSCC) in alloy 690 tested in PWR primary water. High-resolution scanning (SEM) and transmission electron microscopy (TEM) have been employed to investigate the microstructural reasons for this enhanced susceptibility in two stages, first examining grain boundary damage produced by cold rolling and second by characterization of stress corrosion crack tips. The degree of permanent grain boundary damage from cold rolling was found to depend directly on the initial IG precipitate distribution. Cold rolling to high levels of reduction was discovered to produce small IG voids and cracked carbides in alloys with a high density of grain boundary carbides. For the same degree of cold rolling, alloys with few IG carbides exhibited much less permanent damage. Although this difference in grain boundary damage appears to correlate with measured SCC growth rates, crack tip examinations reveal no interaction between the preexisting voids and cracked carbides with the propagation. In many cases, these features appeared to blunt propagation of IGSCC cracks. High-resolution characterizations are described for cold-rolled alloy 690 CRDM tubing and plate materials to gain insights into IGSCC mechanisms.

Experiment-based modelling of grain boundary β-phase (Mg2Al3) evolution during sensitisation of aluminium alloy AA5083.

PubMed

Zhang, R; Steiner, M A; Agnew, S R; Kairy, S K; Davies, C H J; Birbilis, N

2017-06-07

An empirical model for the evolution of β-phase (Mg 2 Al 3 ) along grain boundaries in aluminium alloy AA5083 (Al-Mg-Mn) during isothermal exposures is proposed herein. Developing a quantitative understanding of grain boundary precipitation is important to interpreting intergranular corrosion and stress corrosion cracking in this alloy system. To date, complete ab initio models for grain boundary precipitation based upon fundamental principles of thermodynamics and kinetics are not available, despite the critical role that such precipitates play in dictating intergranular corrosion phenomena. Empirical models can therefore serve an important role in advancing the understanding of grain boundary precipitation kinetics, which is an approach applicable beyond the present context. High resolution scanning electron microscopy was to quantify the size and distribution of β-phase precipitates on Ga-embrittled intergranular fracture surfaces of AA5083. The results are compared with the degree of sensitisation (DoS) as judged by nitric acid mass loss testing (ASTM-G67-04), and discussed with models for sensitisation in 5xxx series Al-alloys. The work herein allows sensitisation to be quantified from an unambiguous microstructural perspective.

Dependence of critical current density on microstructure and processing of high-T(c) superconductors

NASA Astrophysics Data System (ADS)

Goyal, A.; Specht, E. D.; Wang, Z. L.; Kroeger, D. M.; Sutliff, J. A.; Tkaczyk, J. E.; Deluca, J. A.; Masur, L.; Riley, G. N., Jr.

Microstructural origins for reduced weak-link behavior in high-J(sup c) melt-processed YBCO, spray pyrolyzed thick films of Tl-1223, metallic precursor Y-124 polycrystalline powder-in-tube (PIT) wires and PIT Bi-2212/2223 are discussed. Since the materials studied are the highest J(sub c), polycrystalline, high-T(sub c) superconductors fabricated worldwide, the results provide important guidelines for further improvements in superconducting properties, thereby enabling practical applications of these materials. It is found that strongly linked current flow within domains of melt-processed 123 occurs effectively through a single crystal path. In c-axis oriented, polycrystalline Tl-1223 thick films, local in-plane texture has been found to play a crucial role in the reduced weak-link behavior. Formation of 'colonies' of grains with a common c-axis and modest in-plane misorientation was observed. Furthermore, a colony boundary in general has a varying misorientation along the boundary. Large regions comprised primarily of low angle boundaries were observed. Percolative transport through a network of such small angle boundaries appears to provide the non-weak-linked current path. Although powder-in-tube BSCCO 2212 and 2223 also appear to have a 'colony' microstructure, there are some important differences. Colonies in BSCCO consist of stacks of grains with similar c-axis orientation in contrast to colonies in Tl-1223 films where few grains are stacked on top of one another. In the case of Y-124 wires, weak macroscopic in-plane texture is found. Additional measurements are underway to determine if a sharper, local in-plane texture also exists. It is found that in three of the four types of superconductors studied, reduced weak-link behavior can be ascribed to some degree of biaxial alignment between grains, either on a 'local' or a 'global' scale.

A Study on the Role of Grain-Boundary Engineering in Promoting High-Cycle Fatigue Resistance and Improving Reliability in Metallic Alloys for Propulsion Systems

DTIC Science & Technology

2005-04-30

in addition, air cooling instead of water or oil quenching was adopted to avoid quench cracking. Based on a series of preliminary multi -parametric...microstructures were then grain- boundary engineered using four cycles of strain and high-temperature annealing of the single- phase alloy, specifically...automated load- shedding at a normalized K-gradient of -0.08 mm-, as specified in the standard. Multi -sample tests were conducted to verify the effect of

Effect of initial microstructure on the compactability of rapidly solidified Ti-rich TiAl powder

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nishida, M.; Chiba, A.; Morizono, Y.

1997-12-31

Initial microstructure dependence of compactability at elevated temperature in rapidly solidified Ti-rich TiAl alloy powders produced by plasma rotating electrode process (PREP) has been investigated. There were two kinds of powders with respect to the microstructure. The first one had a surface relief of a martensitic phase, which was referred as M powder. The second one had a dendritic structure, which was referred as D powder. {alpha}{sub 2}+{gamma} microduplex and {alpha}{sub 2}/{gamma} lamellar structures were formed in M and D powders of the Ti-40 at%Al alloy by heat treatment at 1,273 K, respectively. The microduplex structure consisted of {gamma} precipitatemore » in the twin related {alpha}{sub 2} matrix with the usual orientation relationship. It was difficult to compact the D powder by hot pressing at 1,273 K under 50 MPa for 14.4 ks. On the other hand, the M powder was compacted easily by hot pressing with the same condition. The twin related {alpha}{sub 2} and {alpha}{sub 2} boundary changed to random ones and the {alpha}{sub 2} and {gamma} phases lost the usual orientation relationship in the duplex structure during the hot pressing. In other words, the low energy boundaries were changed to the high energy ones suitable for grain boundary sliding. Dislocations were scarcely observed inside of both the {alpha}{sub 2} and {gamma} crystal grains. It was concluded that the grain boundary sliding was a predominant deformation mode in the M powder during the hot pressing. D and M powders in Ti-45 and 47 at%Al alloys showed the same tendency as those in Ti-40 at%Al alloy during hot pressing.« less

Effect of sulfur content on the microstructure and toughness of simulated heat-affected zone in Ti-killed steels

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jyelong Lee; Yeongtsuen Pan

1993-06-01

Four Ti-killed steels were made to study the specific influence of sulfur on the inclusion, microstructure, and toughness of a simulated heat-affected zone (HAZ). The HAZ toughness was mainly determined by the volume fraction of intragranular acicular ferrite (IAF) which was closely related to the supercooling required to initiate austenite to ferrite transformation. The extent of supercooling was strongly influenced by the composition of grain boundary and inclusions. Sulfur addition up to 102 ppm caused a segregation of sulfur to the grain boundaries and a change of inclusion phase from predominantly Ti-oxides to Ti-oxysulphides and MnS. This behavior, in turn,more » suppressed the formation of IAF polygonal ferrite and promoted the formation of IAF. Further addition of sulfur elevated transformation temperature and promoted the formation of polygonal ferrite due to the refinement of grain size and the increase of grain boundary associated inclusions. A methodology was proposed to evaluate the intragranular nucleation potential of inclusions, and the results showed that Ti-oxysulphides possessed better nucleation potential for IAF than Ti-oxides and MnS. With the lowest transformation temperature and most effective nuclei, the best HAZ toughness can be obtained at sulfur content of 102 ppm due to the achievement of the maximum volume fraction of IAF.« less

The effect of 45° grain boundaries and associated Fe particles on Jc and resistivity in Ba(Fe0.9Co0.1)2As2 thin films

NASA Astrophysics Data System (ADS)

Hänisch, J.; Iida, K.; Kurth, F.; Thersleff, T.; Trommler, S.; Reich, E.; Hühne, R.; Schultz, L.; Holzapfel, B.

2014-01-01

The anisotropy of the critical current density Jc depends in general on both the properties of the flux lines (such as line tension, coherence length and penetration depth) and the properties of the defects (such as density, shape, orientation etc.). Whereas the Jc anisotropy in microstructurally clean films can be scaled to an effective magnetic field containing the Ginzburg-Landau anisotropy term, it is in general not possible (or only in a limited field range) for samples containing extended defects. Here, the Jc anisotropy of a Co-doped BaFe2As2 sample with 45° [001] tilt grain boundaries (GBs), i.e. grain boundaries created by 45° in-plane rotated grains, as well as extended Fe particles is investigated. This microstructure leads to c-axis correlated pinning, both due to the GBs and the Fe particles and manifests in a c-axis peak in the Jc anisotropy at low magnetic fields and a deviation from the anisotropic Ginzburg-Landau scaling at higher fields. Strong pinning at ellipsoidal extended defects, i.e. the Fe particles, is discussed, and the full Jc anisotropy is fitted successfully with the vortex path model. The results are compared to a sample without GBs and Fe particles. 45° GBs seem to be good pinning centers rather than detrimental to current flow.

Impact of grain boundaries on efficiency and stability of organic-inorganic trihalide perovskites

DOE PAGES

Chu, Zhaodong; Yang, Mengjin; Schulz, Philip; ...

2017-12-20

Organic-inorganic perovskite solar cells have attracted tremendous attention because of their remarkably high power conversion efficiencies. To further improve device performance, it is imperative to obtain fundamental understandings on the photo-response and long-term stability down to the microscopic level. Here, we report the quantitative nanoscale photoconductivity imaging on two methylammonium lead triiodide thin films with different efficiencies by light-stimulated microwave impedance microscopy. The microwave signals are largely uniform across grains and grain boundaries, suggesting that microstructures do not lead to strong spatial variations of the intrinsic photo-response. In contrast, the measured photoconductivity and lifetime are strongly affected by bulk propertiesmore » such as the sample crystallinity. As visualized by the spatial evolution of local photoconductivity, the degradation process begins with the disintegration of grains rather than nucleation and propagation from visible boundaries between grains. In conclusion, our findings provide insights to improve the electro-optical properties of perovskite thin films towards large-scale commercialization.« less

Study on the Toughness of X100 Pipeline Steel Heat Affected Zone

NASA Astrophysics Data System (ADS)

Li, Xueda; Shang, Chengjia; Ma, Xiaoping; Subramanian, S. V.

Microstructure-property correlation of heat affected zone (HAZ) in X100 longitudinal submerged arc welding (LSAW) real weld joint was studied in this paper. Coarse grained (CG) HAZ and intercritically reheated coarse grained (ICCG) HAZ were characterized by optical microscope (OM), electron backscattered diffraction (EBSD). The microstructure of CGHAZ is mostly composed of granular bainite with low density of high angle boundaries (HAB). Prior austenite grain size is 80μm. In ICCGHAZ, coarse prior austenite grains were decorated by coarse necklacing martensite-austenite (M-A) constituents. Different layers were observed within M-A constituent, which may be martensite and austenite layers. Charpy absorbed energy of two different HAZ regions (ICCGHAZ containing and non-containing regions) was recorded using instrumental Charpy impact test machine. The results showed that the existence of ICCGHAZ resulted in the sharp drop of Charpy absorbed energy from 180J to 50J, while the existence of only CGHAZ could still lead to good toughness. The fracture surface was 60% brittle in the absence of ICCGHAZ, and 100% brittle in the presence of ICCGHAZ in the impact tested samples. The underlying reason is the microstructure of ICCGHAZ consisted of granular bainite and upper bainite with necklace-type M-A constituent along the grain boundaries. Cleavage fracture initiated from M-A constituent, either through cracking of M-A or debonding from the matrix, was observed at the fracture surface of ICCGHAZ. The presence of necklace type M-A constituent in ICCGHAZ notably increases the susceptibility of cleavage microcrack nucleation. Furthermore, the study of secondary microcracks beneath the CGHAZ and the ICCGHAZ through EBSD suggested that the fracture mechanism changes from nucleation-controlled in the CGHAZ to propagation-controlled in the ICCGHAZ because of the presence of necklace-type M-A constituent in the ICCGHAZ region. Both fracture mechanism contribute to the poor toughness of the sample contained ICCGHAZ. In conclusion, big prior austenite grains with low density of HAB plus coarse necklacing M-A products along grain boundary is the dominant factor resulting in low toughness.

Grain boundary engineering to control the discontinuous precipitation in multicomponent U10Mo alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Devaraj, Arun; Kovarik, Libor; Kautz, Elizabeth

Grain boundaries in metallic alloys often play a crucial role, not only in determining the mechanical properties or thermal stability of alloys, but also in dictating the phase transformation kinetics during thermomechanical processing. We demonstrate that locally stabilized structure and compositional segregation at grain boundaries—“grain boundary complexions”—in a complex multicomponent alloy can be modified to influence the kinetics of cellular transformation during subsequent thermomechanical processing. Using aberration-corrected scanning transmission electron microscopy and atom probe tomography analysis of a metallic nuclear fuel highly relevant to worldwide nuclear non-proliferation efforts —uranium-10 wt% molybdenum (U-10Mo) alloy, new evidence for the existence of grainmore » boundary complexion is provided. We then modified the concentration of impurities dissolved in Υ-UMo grain interiors and/or segregated to Υ-UMo grain boundaries by changing the homogenization treatment, and these effects were used used to retard the kinetics of cellular transformation during subsequent sub-eutectoid annealing in this U-10-Mo alloy during sub-eutectoid annealing. Thus, this work provided insights on tailoring the final microstructure of the U-10Mo alloy, which can potentially improve the irradiation performance of this important class of alloy fuels.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shassere, Benjamin; Yamamoto, Yukinori; Poplawsky, Jonathan

We have develooped a new Fe-Cr-Al (FCA) alloy system with good oxidation resistance and creep strength at high temperature. The alloy system is a candidate for use in future fossil-fueled power plants. The creep strength of these alloys at 973 K (700 °C) was found to be comparable with traditional 9 pct Cr ferritic–martensitic steels. A few FCA alloys with general composition of Fe-30Cr-3Al-.2Si-xNb (x = 0, 1, or 2) with a ferrite matrix and Fe 2Nb-type Laves precipitates were prepared. The detailed microstructural characterization of samples, before and after creep rupture testing, indicated precipitation of the Laves phase withinmore » the matrix, Laves phase at the grain boundaries, and a 0.5 to 1.5 μm wide precipitate-free zone (PFZ) parallel to all the grain boundaries. In these alloys, the areal fraction of grain boundary Laves phase and the width of the PFZ controlled the cavitation nucleation and eventual grain boundary ductile failure. Finally, we used a phenomenological model to compare the creep strain rates controlled by the effects of the particles on the dislocations within the grain and at grain boundaries. (The research sponsored by US-DOE, Office of Fossil Energy, the Crosscutting Research Program).« less

Microstructure and mechanical properties of friction stir welded and laser welded high entropy alloy CrMnFeCoNi

NASA Astrophysics Data System (ADS)

Jo, Min-Gu; Kim, Han-Jin; Kang, Minjung; Madakashira, Phaniraj P.; Park, Eun Soo; Suh, Jin-Yoo; Kim, Dong-Ik; Hong, Sung-Tae; Han, Heung Nam

2018-01-01

The high entropy alloy CrMnFeCoNi has been shown to have promising structural properties. For a new alloy to be used in a structural application it should be weldable. In the present study, friction stir welding (FSW) and laser welding (LW) techniques were used to butt weld thin plates of CrMnFeCoNi. The microstructure, chemical homogeneity and mechanical behavior of the welds were characterized and compared with the base metal. The tensile stress-strain behavior of the welded specimens were reasonable when compared with that of the base metal. FSW refined the grain size in the weld region by a factor of ˜14 when compared with the base metal. High-angle annular dark field transmission electron microscopy in combination with energy dispersive X-ray spectroscopy showed chemical inhomogeneity between dendritic and interdendritic regions in the fusion zone of LW. Large fluctuations in composition (up to 15 at%) did not change the crystal structure in the fusion zone. Hardness measurements were carried out in the weld cross section and discussed in view of the grain size, low angle grain boundaries and twin boundaries in FSW specimens and the dendritic microstructure in LW specimens.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Junfeng, E-mail: chenjunfeng@fzu.edu.cn; Zou, Linchi, E-mail: zoulinchi1201@163.com; Li, Qiang

The microstructure evolution of the 7050 Al alloy treated by age-forming was studied using a designed device which can simulate the age-forming process. The grain shape, grain boundary misorientation and grain orientation evolution of 7050 Al alloy during age-forming have been quantitatively characterized by electron backscattering diffraction technique. The results show that age-forming produced abundant low-angle boundaries and elongated grains, which attributed to stress induced dislocation movement and grain boundary migration during the age-forming process. On the other side, the stress along rolling direction caused some unstable orientation grains to rotate towards the Brass and S orientations during the age-formingmore » process. Hence, the intensity of the rolling texture orientation in age-formed samples is enhanced. But this effect decays gradually with increasing aging time, since stress decreases and precipitation hardening occurs during the age-forming process. - Highlights: • Quantitative analysis of grain evolution of 7050 Al alloys during age-forming • Stress induces some grain rotation of 7050 Al alloys during age-forming. • Creep leads to elongate grain of 7050 Al alloys during age-forming. • Obtains a trend on texture evolution during age-forming applied stress.« less

The Strength-Grain Size Relationship in Ultrafine-Grained Metals

NASA Astrophysics Data System (ADS)

Balasubramanian, N.; Langdon, Terence G.

2016-12-01

Metals processed by severe plastic deformation (SPD) techniques, such as equal-channel angular pressing (ECAP) and high-pressure torsion (HPT), generally have submicrometer grain sizes. Consequently, they exhibit high strength as expected on the basis of the Hall-Petch (H-P) relationship. Examples of this behavior are discussed using experimental data for Ti, Al, and Ni. These materials typically have grain sizes greater than 50 nm where softening is not expected. An increase in strength is usually accompanied by a decrease in ductility. However, both high strength and high ductility may be achieved simultaneously by imposing high strain to obtain ultrafine-grain sizes and high fractions of high-angle grain boundaries. This facilitates grain boundary sliding, and an example is presented for a cast Al-7 pct Si alloy processed by HPT. In some materials, SPD may result in a weakening even with a very fine grain size, and this is due to microstructural changes during processing. Examples are presented for an Al-7034 alloy processed by ECAP and a Zn-22 pct Al alloy processed by HPT. In some SPD-processed materials, it is possible that grain boundary segregation and other features are present leading to higher strengths than predicted by the H-P relationship.

Evidence of sealing and brine distribution at grain boundaries in natural fine-grained Halite (Qum Kuh salt fountain, Central Iran): implications for rheology of salt extrusions

NASA Astrophysics Data System (ADS)

Desbois, Guillaume; Urai, Janos L.; de Bresser, J. H. P.

2010-05-01

When grain boundary movement is stopped, surface energy related forces reassert themselves driving the system to its equilibrium conditions ([2], [6], [7], [8]). This could result in growth of islands and shrinking of channels and hence in healing the boundary by internal redistribution of fluid and solid in the contact region. Such islands are proposed to grow preferentially close to the contact rim and promote the healing of the grain-grain contact, which in turn prevents transport in or out the boundary region and thus traps the fluids in isolated inclusions. This contribution is focused on observation of grain boundary microstructures in natural mylonitic rocksalt collected from the distal part of Kum-Quh salt fountain (central Iran) in order to give unprecedented insight of grain boundary microstructures using argon-beam cross-sectioning to prepare high quality polished surfaces suitable for high-resolution SEM imaging. The possibility to use our SEM under cryogenic conditions allows also imaging the in-situ distribution of fluids. Results show that brine at grain boundaries occurs as thick layers (> µm in scale) corresponding to cross-sectioned wetted triple junction tubes, as filling at triple junction and as array of isolated fluids inclusions at grain-grain contacts. Close observations at islands contacts suggest the presence of a very thin fluid film (<100 nm). The most remarkable is evidence for sealing of pore space appearing as subhedral crystals filling the void space and decoupled from surrounding crystals by a thin brine layer. In parallel to this microstructural study, we deformed the same samples in order to simulate the simple shear flow at very low mean stress as in the salt fountain. First results suggest a complicated rheology. Samples loaded at σ < 0.7 MPa show no measurable deformation in a month, indicating strain rates less than 10-12 s-1 though, in fully activated pressure-solution (PS) creep, strain rates of several orders of magnitude are expected for similar grain size ([5]). Other samples, which were loaded to 1 MPa before reducing the stress to 0.5 MPa deformed at much higher but variable rates, up to 10-8 s-1, in good agreement with activated PS creep. If, at first look, our pilot deformation experiments seem to reflect a kind of "yield stress" for activation PS creep ([7]); the experimental stress does not reach the theoritical condition to enable activation of PS. Thus, we interpret that the apparent "yielding stress" may not reflect strictu senso the "yielding stress" as described in [7] but rather to a "yielding stress" corresponding to the elastic reassessment of the grain system before the initiation of PS at privileged seal-brine-grain contacts. In salt fountain conditions, mylonitic samples are expected to be in the healing domain, but "jumps" in active stress required to activate PS creep is hardly probable. Thus, we suggest that rainwater influx plays a fundamental role in activation of PS. Rainwater should enable the marginal dissolution of healed contacts and then decreases in the area fraction of grain boundary occupied by solid island contact causing an increase in island stress. Therefore, this points to cyclic deformation of salt fountain: (1) during rainy periods the fountain will deformed at relative high strain rate by dominant PS; while (2) during dry seasons, it will not significantly flow because the grain boundary healing will prevent PS and lead to dominant dislocation creep. This interpretation is in good agreement with recent structural studies ([1], [4]), which gives evidence for both dynamic dislocation and pressure-solution creeps, and measurement of rapid flow after rainy periods with flow rates compatible with fully activated PS ([3]). [1] Desbois G., Zavada P., Schleder Z. and Urai J.L. (In review). Deformation and recrystallization mechanisms in naturally deformed salt fountain: microstructural evidence for a switch in deformation mechanisms with increased availability of meteoric water and decreased grain size (Qum Kuh, central Iran). Submitted to Journal of Structural Geology. [2] Ghoussoub J., and Leroy Y.M. (2001), Solid-fluid phase transformation within grain boundaries during compaction by pressure solution, J. Mech. Phys. Solids, 49, 737 2385-2430. 738 [3] Jackson, M.P.A., (1985). Natural strain in diapiric and glacial rock salt, with emphasis on Oakwood dome, East Texas, Bureau of Economic Geology, The University of Texas at Austin, Texas. [4] Schléder Z. and Urai J.L. (2007). Deformation and recrystallization mechanisms in mylonitic shear zones in naturally deformed extrusive Eocene-Oligocene rock salt from Eyvanekey plateau and Garmsar hills (central Iran). Journal of structural geology, 29, 241-255. [5] Spiers C.J. and Carter N.L. (1988). Microphysics of rock salt flow in nature. In: M. Aubertin and H.R. Hardy, Editors, The Mechanical Behaviour of Salt: Proceedings of the Fourth Conference Series on Rock and Soil Mechanics, TTP Trans Tech Publications, Clausthal-Zellerfeld, 22: 115-128. [6] Urai J. L. (1983). Water assisted dynamic recrystallization and weakening in polycrystalline bischofite. Tectonophysics 96 (1-2): 125-157. [7] Van Noort R., Visser H.J.M., Spiers C.J. (2008) Influence of grain boundary structure on dissolution controlled pressure solution and retarding effects of grain boundary healing. Journal of Geophysical Research, 113, B03201. [8] Visser, H. J. M. (1999). Mass transfer processes in crystalline aggregates containing a fluid phase, Ph. D. thesis, Utrecht University, Utrecht.

Microstructural characterization of an SA508–309L/308L–316L domestic dissimilar metal welded safe-end joint

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ming, Hongliang; Zhang, Zhiming; Wang, Jianqiu, E-mail: wangjianqiu@imr.ac.cn

2014-11-15

The microstructure of an SA508–309L/308L–316L domestic dissimilar metal welded safe-end joint was characterized in this work by optical microscopy, scanning electron microscopy (with electron back scattering diffraction) and micro-hardness testing. Epitaxial growth and competitive growth are evident in the 308L–316L fusion boundary regions. A martensite layer, carbon-depleted zones, and type-II and type-I boundaries are found in the SA508–309L fusion boundary regions, while only martensite and austenite mixed zones are observed in the SA508–308L fusion boundary regions. The microstructure near the fusion boundary and the microstructure transition in the SA508 heat affected zone are quite complex. Both for SA508–309L/308L and 308L–316L,more » the highest residual strain is located on the outside of the weldment. The residual strain and the grain boundary character distribution change with increasing distance from the fusion boundary in the heat affected zone of 316L. Micro-hardness measurements also reveal non-uniform mechanical properties across the weldment. - Highlights: • The microstructure of SA508 HAZ, especially near the FB, is very complex. • The outside of the dissimilar metal welded joint has the highest residual. • The micro-hardness distributions along the DMWJ are non-uniform.« less

Misoriented grain boundaries vicinal to the (1 1 1) <1 1¯0> twin in nickel Part I: Thermodynamics & temperature-dependent structure

DOE PAGES

O’Brien, Christopher J.; Medlin, Douglas L.; Foiles, Stephen M.

2016-03-30

Here, grain boundary-engineered materials are of immense interest for their corrosion resistance, fracture resistance and microstructural stability. This work contributes to a larger goal of understanding both the structure and thermodynamic properties of grain boundaries vicinal (within ±30°) to the Σ3(1 1 1) <1 1¯0> (coherent twin) boundary which is found in grain boundary-engineered materials. The misoriented boundaries vicinal to the twin show structural changes at elevated temperatures. In the case of nickel, this transition temperature is substantially below the melting point and at temperatures commonly reached during processing, making the existence of such boundaries very likely in applications. Thus,more » the thermodynamic stability of such features is thoroughly investigated in order to predict and fully understand the structure of boundaries vicinal to twins. Low misorientation angle grain boundaries (|θ| ≲ 16°) show distinct ±1/3(1 1 1) disconnections which accommodate misorientation in opposite senses. The two types of disconnection have differing low-temperature structures which show different temperature-dependent behaviours with one type undergoing a structural transition at approximately 600 K. At misorientation angles greater than approximately ±16°, the discrete disconnection nature is lost as the disconnections merge into one another. Free energy calculations demonstrate that these high-angle boundaries, which exhibit a transition from a planar to a faceted structure, are thermodynamically more stable in the faceted configuration.« less

Microstructures and rheology of a calcite-shale thrust fault

NASA Astrophysics Data System (ADS)

Wells, Rachel K.; Newman, Julie; Wojtal, Steven

2014-08-01

A thin (˜2 cm) layer of extensively sheared fault rock decorates the ˜15 km displacement Copper Creek thrust at an exposure near Knoxville, TN (USA). In these ultrafine-grained (<0.3 μm) fault rocks, interpenetrating calcite grains form an interconnected network around shale clasts. One cm below the fault rock layer, sedimentary laminations in non-penetratively deformed footwall shale are cut by calcite veins, small faults, and stylolites. A 350 μm thick calcite vein separates the fault rocks and footwall shale. The vein is composed of layers of (1) coarse calcite grains (>5 μm) that exhibit a lattice preferred orientation (LPO) with pores at twin-twin and twin-grain boundary intersections, and (2) ultrafine-grained (0.3 μm) calcite that exhibits interpenetrating grain boundaries, four-grain junctions and lacks a LPO. Coarse calcite layers crosscut ultrafine-grained layers indicating intermittent vein formation during shearing. Calcite in the fault rock layer is derived from vein calcite and grain-size reduction of calcite took place by plasticity-induced fracture. The ultrafine-grained calcite deformed primarily by diffusion-accommodated grain boundary sliding and formed an interconnected network around shale clasts within the shear zone. The interconnected network of ultrafine-grained calcite indicates that calcite, not shale, was the weak phase in this fault zone.

Grain growth and pore coarsening in dense nano-crystalline UO 2+x fuel pellets

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yao, Tiankai; Mo, Kun; Yun, Di

Dense nano-sized UO 2+x pellets are synthesized by spark plasma sintering with controlled stoichiometries (UO 2.03 and UO 2.11) and grain sizes (~100 nm), and subsequently isothermally annealed to study their effects on grain growth kinetics and microstructure stability. The grain growth kinetics is determined and analyzed focusing on the interaction between grain boundary migration, pore growth and coalescence. Grains grow much bigger in nano-sized UO 2.11 than UO 2.03 upon thermal annealing, consistent with the fact that hyper-stoichiometric UO 2+x is beneficial for sintering due to enhanced U ion diffusion from excessive O ion interstitials. The activation energies ofmore » the grain growth for UO 2.03 and UO 2.11 are determined as ~1.0 and 1.3~2.0 eV, respectively. As compared with the micron-sized UO 2 in which volumetric diffusion dominates the grain coarsening with an activation energy of ~3.0 eV, the enhanced grain growth kinetics in nano-sized UO 2+x suggests that grain boundary diffusion controls grain growth. Lastly, the higher activation energy of more hyper-stoichiometric nano-sized UO 2.11 may be attributed to the excessive O interstitials pinning grain boundary migration.« less

Grain growth and pore coarsening in dense nano-crystalline UO 2+x fuel pellets

DOE PAGES

Yao, Tiankai; Mo, Kun; Yun, Di; ...

2017-03-25

Dense nano-sized UO 2+x pellets are synthesized by spark plasma sintering with controlled stoichiometries (UO 2.03 and UO 2.11) and grain sizes (~100 nm), and subsequently isothermally annealed to study their effects on grain growth kinetics and microstructure stability. The grain growth kinetics is determined and analyzed focusing on the interaction between grain boundary migration, pore growth and coalescence. Grains grow much bigger in nano-sized UO 2.11 than UO 2.03 upon thermal annealing, consistent with the fact that hyper-stoichiometric UO 2+x is beneficial for sintering due to enhanced U ion diffusion from excessive O ion interstitials. The activation energies ofmore » the grain growth for UO 2.03 and UO 2.11 are determined as ~1.0 and 1.3~2.0 eV, respectively. As compared with the micron-sized UO 2 in which volumetric diffusion dominates the grain coarsening with an activation energy of ~3.0 eV, the enhanced grain growth kinetics in nano-sized UO 2+x suggests that grain boundary diffusion controls grain growth. Lastly, the higher activation energy of more hyper-stoichiometric nano-sized UO 2.11 may be attributed to the excessive O interstitials pinning grain boundary migration.« less

An experimental assessment of the size effects on the strength and ductility of freestanding copper films under macroscopically homogenous deformation

NASA Astrophysics Data System (ADS)

Chauhan, Shakti Singh

Metallic interconnects and circuitry has been experiencing excessive deformation beyond their elastic limits in many applications, ranging from micro-electromechanical systems (MEMS) to flexible electronics. These broad applications are creating needs to understand the extent of strength and ductility of freestanding metallic films at scales approaching the micron and sub micron range. This work aims to elucidate the effects of microstructural constraint as well as geometric dimensional constraint on the strength and ductility of freestanding Cu films under uniaxial tension. Two types of films are tested (i) high purity rolled films of 12.5-100microm thickness and average grain sizes of 11-47microm and (ii) electroplated films of 2-50 microm thickness and average grain sizes of 1.8-5microm. Several experimental tools including residual electrical resistivity measurements, surface strain measurements and surface roughness measurements are employed to highlight the underlying deformation mechanisms leading to the observed size effects. With respect to the strength of the specimens, we find that the nature and magnitude of thickness effects is very sensitive to the average grain size. In all cases, coupled thickness and grain size effects were observed. This study shows that this observed coupling, unique to the case of freestanding specimen, arises because the observed size effects are an outcome of the size dependence of two fundamental microstructural parameters i.e. volume fraction of surface grains and grain boundary area per unit specimen volume. For films having thickness and grain sizes greater than 5microm, thickness dependent weakening is observed for a constant grain size. Reducing thickness results in an increase in the volume fraction of grains exposed to the free surface as well as a reduction in the grain boundary area per unit specimen volume. The former effect leads to a reduction in the effective microstructural constraint on the intragranular dislocation activity in individual grains. This free surface related effect is the origin of a weakening contribution to the overall specimen strength with reducing thickness. For specimens with grain sizes ˜ O (10-50microm), this effect was found to be dominating i.e. reducing thickness resulted in reducing strength. A phenomenological model employing the flow strength of surface and bulk grains is proposed to model the observed trends. For films having thickness and grain sizes smaller than 5microm, size dependent strengthening is observed for a constant grain size. At this scale, grain boundary dislocations dominate. As a consequence, thickness effects arise because grain boundary dislocation source density per unit specimen volume reduces with reducing specimen thickness. This statistical reduction in dislocation source density leads to increasing specimen strength via source starvation strengthening. Our results show that such increasing specimen strength with reducing thickness, which has only been observed previously for nanocrystalline thin films, first appears at average grain size of ˜5microm or xx smaller. The measurements showed a characteristic length scale of about 5microm, which defines the size dependent strengthening or weakening of the film. With respect to the thickness effects on ductility, it was found that both thickness and average grain size affect ductility. While prominent thickness effects persist at larger grain sizes, for specimens with grain size approaching 1microm, the loss of strain hardening ability at such fine microstructures dominates and a limiting ductility of ˜2% is seen irrespective of the thickness. The observed thickness effects on ductility were investigated via surface roughness measurements that allow the characterization of initiation and evolution of deformation heterogeneities. It was found that thickness has a strong influence on the characteristic heterogeneity of deformation. At small specimen thicknesses, the deformation was found to be highly localized i.e. widely spaced regions showing substantial thickness reduction, hence increasing the vulnerability to the onset of plastic instabilities. At larger thicknesses, however, the increasing microstructural constraint delocalizes the strain and thereby precludes the early onset of instability, leading to enhanced ductility.

Precipitate Redistribution during Creep of Alloy 617

DOE Office of Scientific and Technical Information (OSTI.GOV)

S. Schlegel; S. Hopkins; E. Young

2009-12-01

Nickel-based superalloys are being considered for applications within advanced nuclear power generation systems due to their high temperature strength and corrosion resistance. Alloy 617, a candidate for use in heat exchangers, derives its strength from both solid solution strengthening and the precipitation of carbide particles. However, during creep, carbides that are supposed to retard grain boundary motion are found to dissolve and re-precipitate on boundaries in tension. To quantify the redistribution, we have used electron backscatter diffraction and energy dispersive spectroscopy to analyze the microstructure of 617 after creep testing at 900 and 1000°C. The data were analyzed with respectmore » to location of the carbides (e.g., intergranular vs. intragranular), grain boundary character, and precipitate type (i.e., Cr-rich or Mo-rich). We find that grain boundary character is the most important factor in carbide distribution; some evidence of preferential distribution to boundaries in tension is also observed at higher applied stresses. Finally, the results suggest that the observed redistribution is due to the migration of carbides to the boundaries and not the migration of boundaries to the precipitates.« less

Ultra-fine grained microstructure of metastable beta Ti-15Mo alloy and its effects on the phase transformations

NASA Astrophysics Data System (ADS)

Václavová, K.; Stráský, J.; Zháňal, P.; Veselý, J.; Polyakova, V.; Semenova, I.; Janeček, M.

2017-05-01

Processing of metastable titanium alloys by severe plastic deformation provides an opportunity to achieve exceptional grain refinement, to enhance the strength and to affect phase transformations occurring during thermal treatment. The main aim of this study is to investigate the microstructure of ultra-fine grained (UFG) material and effect of microstructural changes on phase transformations in metastable β-Ti alloy Ti-15Mo. Metastable β-Ti alloys are currently the most studied Ti-based materials with prospective use in medicine. Ti-15Mo alloy after solution treatment contains metastable β-phase. Metastable ω-phase and stable α-phase particles are formed upon annealing,. Solution treated Ti-15Mo alloy was deformed by high pressure torsion (HPT) at room temperature. Severely deformed structure after HPT with grain size of ~200 nm was studied by transmission electron microscopy. In-situ electrical resistance measurements showed significant changes in undergoing phase transformations when compared to coarse-grained (CG) material. Scanning electron microscopy revealed heterogeneous precipitation of α-particles at grain boundaries (GB). Due to the high density of GBs in UFG structure, these precipitates are very fine and equiaxed. The study demonstrates that SPD is capable of enhancing mechanical properties due to grain refinement and via affecting precipitation processes in metastable β-Ti alloys.

Enhancement of ductility and improvement of abnormal Goss grain growth of magnetostrictive Fe-Ga rolled alloys

NASA Astrophysics Data System (ADS)

Li, Ji-heng; Yuan, Chao; Mu, Xing; Bao, Xiao-qian; Gao, Xue-xu

2018-04-01

The influences of initial microstructures on the mechanical properties and the recrystallization texture of magnetostrictive 0.1at% NbC-doped Fe83Ga17 alloys were investigated. The directionally solidified columnar-grained structure substantially enhanced the tensile elongation at intermediate temperatures by suppressing fracture along the transverse boundaries. Compared with tensile elongations of 1.0% at 300°C and 12.0% at 500°C of the hot-forged equiaxed-grained alloys, the columnar-grained alloys exhibited substantially increased tensile elongations of 21.6% at 300°C and 46.6% at 500°C. In the slabs for rolling, the introduction of <001>-oriented columnar grains also promotes the secondary recrystallization of Goss grains in the finally annealed sheets, resulting in an improvement of the saturation magnetostriction. For the columnar-grained specimens, the inhomogeneous microstructure and disadvantage in number and size of Goss grains are improved in the primarily annealed sheets, which is beneficial to the abnormal growth of Goss grains during the final annealing process.

The Effect of Titanium Inclusions on HY-80 GMA Weld Deposits

DTIC Science & Technology

1990-12-01

to a tempered bainite- martensite microstructure. The Tim--Temperature- Transformation diagram shown in Figure 1 on page 4 illustrates, these...acicular ferrite laths, or adjacent to grain boundary fcrrite, may eithcr transform to ferrite and carbide aggregates or martensite . or may rcmain...microscopy. While the microstructures do consist mainly of lowver bainite, tempered and untempered martensite can also be present, especially, at faster

A Mechanical, Microstructural, and Damage Study of Various Tailor Hot Stamped Material Conditions Consisting of Martensite, Bainite, Ferrite, and Pearlite

NASA Astrophysics Data System (ADS)

Bardelcik, Alexander; Vowles, Caryn J.; Worswick, Michael J.

2018-04-01

This paper examines the mechanical, microstructural, and damage characteristics of five different material conditions that were created using the tailored hot stamping process with in-die heating. The tailored material conditions, TMC1 to TMC5 (softest-hardest), were created using die temperatures ranging from 700 °C to 400 °C, respectively. The tensile strength (and total elongation) ranged from 615 MPa (0.24) for TMC1 to 1122 MPa (0.11) for TMC5. TMC3 and TMC4 exhibited intermediate strength levels, with almost no increase in total elongation relative to TMC5. FE-SEM microscopy was used to quantify the mixed-phase microstructures, which ranged in volume fractions of ferrite, pearlite, bainite, and martensite. High-resolution optical microscopy was used to quantify void accumulation and showed that the total void area fraction at 0.60 thickness strain was low for TMC1 and TMC5 ( 0.09 pct) and highest for TMC3 (0.31 pct). Damage modes were characterized and revealed that the poor damage behavior of TMC3 (martensite/bainite/ferrite composition) was a result of small martensitic grains forming at grain boundaries and grain boundary junctions, which facilitated void nucleation as shown by the highest measured void density for this particular material condition. The excellent ductility of TMC1 was a result of a large grained ferritic/pearlitic microstructure that was less susceptible to void nucleation and growth. Large titanium nitride (TiN) inclusions were observed in all of the tailored material conditions and it was shown that they noticeably contributed to the total void accumulation, specifically for the TMC3 and TMC4 material conditions.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guo, Rui; Gao, Liming, E-mail: liming.gao@sjtu.edu.cn; Li, Ming, E-mail: mingli90@sjtu.edu.cn

As the continuous shrinkage of the interconnect line width in microelectronics devices, there is a growing concern about the electromigration (EM) failure of bonding wire. In addition, an innovative Ag–8Au–3Pd alloy wire has shown promise as an economical substitute for gold wire interconnects due to the cost pressure of gold in the last decade. In present study of the Ag–8Au–3Pd alloy wire, the surface diffusion occupied the dominant position during EM failure, and the activation energy was found to be 0.61 eV. In order to reveal the failure mechanism, the cross-sections of the Ag–8Au–3Pd alloy wire during EM were preparedmore » by focused ion beam (FIB) micro-machining for electron backscatter diffraction (EBSD) analysis. The microstructure evolution of the Ag–8Au–3Pd alloy wire was characterized by the grain size and grain boundary. As a result, the EM failure originates in the atom transportation, which causes grain size increasing and atom diffusion on the wire surface. - Highlights: • The activation energy of Ag–8Au–3Pd alloy wire was obtained as 0.61 eV. • During EM, the silver atoms diffused from negative to the positive terminal on the wire surface. • The microstructure (grain size and grain boundary) was characterized by FIB-EBSD. • During EM, the atom transportation was found to cause grain size growth and atom diffusion on the wire surface.« less

Additively manufactured hierarchical stainless steels with high strength and ductility.

PubMed

Wang, Y Morris; Voisin, Thomas; McKeown, Joseph T; Ye, Jianchao; Calta, Nicholas P; Li, Zan; Zeng, Zhi; Zhang, Yin; Chen, Wen; Roehling, Tien Tran; Ott, Ryan T; Santala, Melissa K; Depond, Philip J; Matthews, Manyalibo J; Hamza, Alex V; Zhu, Ting

2018-01-01

Many traditional approaches for strengthening steels typically come at the expense of useful ductility, a dilemma known as strength-ductility trade-off. New metallurgical processing might offer the possibility of overcoming this. Here we report that austenitic 316L stainless steels additively manufactured via a laser powder-bed-fusion technique exhibit a combination of yield strength and tensile ductility that surpasses that of conventional 316L steels. High strength is attributed to solidification-enabled cellular structures, low-angle grain boundaries, and dislocations formed during manufacturing, while high uniform elongation correlates to a steady and progressive work-hardening mechanism regulated by a hierarchically heterogeneous microstructure, with length scales spanning nearly six orders of magnitude. In addition, solute segregation along cellular walls and low-angle grain boundaries can enhance dislocation pinning and promote twinning. This work demonstrates the potential of additive manufacturing to create alloys with unique microstructures and high performance for structural applications.

Additively manufactured hierarchical stainless steels with high strength and ductility

NASA Astrophysics Data System (ADS)

Wang, Y. Morris; Voisin, Thomas; McKeown, Joseph T.; Ye, Jianchao; Calta, Nicholas P.; Li, Zan; Zeng, Zhi; Zhang, Yin; Chen, Wen; Roehling, Tien Tran; Ott, Ryan T.; Santala, Melissa K.; Depond, Philip J.; Matthews, Manyalibo J.; Hamza, Alex V.; Zhu, Ting

2018-01-01

Many traditional approaches for strengthening steels typically come at the expense of useful ductility, a dilemma known as strength-ductility trade-off. New metallurgical processing might offer the possibility of overcoming this. Here we report that austenitic 316L stainless steels additively manufactured via a laser powder-bed-fusion technique exhibit a combination of yield strength and tensile ductility that surpasses that of conventional 316L steels. High strength is attributed to solidification-enabled cellular structures, low-angle grain boundaries, and dislocations formed during manufacturing, while high uniform elongation correlates to a steady and progressive work-hardening mechanism regulated by a hierarchically heterogeneous microstructure, with length scales spanning nearly six orders of magnitude. In addition, solute segregation along cellular walls and low-angle grain boundaries can enhance dislocation pinning and promote twinning. This work demonstrates the potential of additive manufacturing to create alloys with unique microstructures and high performance for structural applications.

Additively manufactured hierarchical stainless steels with high strength and ductility

DOE PAGES

Wang, Y. Morris; Voisin, Thomas; McKeown, Joseph T.; ...

2017-10-30

Many traditional approaches for strengthening steels typically come at the expense of useful ductility, a dilemma known as strength–ductility trade-off. New metallurgical processing might offer the possibility of overcoming this. Here we report that austenitic 316L stainless steels additively manufactured via a laser powder-bed-fusion technique exhibit a combination of yield strength and tensile ductility that surpasses that of conventional 316L steels. High strength is attributed to solidification-enabled cellular structures, low-angle grain boundaries, and dislocations formed during manufacturing, while high uniform elongation correlates to a steady and progressive work-hardening mechanism regulated by a hierarchically heterogeneous microstructure, with length scales spanning nearlymore » six orders of magnitude. In addition, solute segregation along cellular walls and low-angle grain boundaries can enhance dislocation pinning and promote twinning. This work demonstrates the potential of additive manufacturing to create alloys with unique microstructures and high performance for structural applications.« less

Additively manufactured hierarchical stainless steels with high strength and ductility

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Y. Morris; Voisin, Thomas; McKeown, Joseph T.

Many traditional approaches for strengthening steels typically come at the expense of useful ductility, a dilemma known as strength–ductility trade-off. New metallurgical processing might offer the possibility of overcoming this. Here we report that austenitic 316L stainless steels additively manufactured via a laser powder-bed-fusion technique exhibit a combination of yield strength and tensile ductility that surpasses that of conventional 316L steels. High strength is attributed to solidification-enabled cellular structures, low-angle grain boundaries, and dislocations formed during manufacturing, while high uniform elongation correlates to a steady and progressive work-hardening mechanism regulated by a hierarchically heterogeneous microstructure, with length scales spanning nearlymore » six orders of magnitude. In addition, solute segregation along cellular walls and low-angle grain boundaries can enhance dislocation pinning and promote twinning. This work demonstrates the potential of additive manufacturing to create alloys with unique microstructures and high performance for structural applications.« less

Microstructural evolution of pure tungsten neutron irradiated with a mixed energy spectrum

NASA Astrophysics Data System (ADS)

Koyanagi, Takaaki; Kumar, N. A. P. Kiran; Hwang, Taehyun; Garrison, Lauren M.; Hu, Xunxiang; Snead, Lance L.; Katoh, Yutai

2017-07-01

Microstructures of single-crystal bulk tungsten (W) and polycrystalline W foil with a strong grain texture were investigated using transmission electron microscopy following neutron irradiation at ∼90-800 °C to 0.03-4.6 displacements per atom (dpa) in the High Flux Isotope Reactor with a mixed energy spectrum. The dominant irradiation defects were dislocation loops and small clusters at ∼90 °C. Additional voids were formed in W irradiated at above 460 °C. Voids and precipitates involving transmutation rhenium and osmium were the dominant defects at more than ∼1 dpa. We found a new phenomenon of microstructural evolution in irradiated polycrystalline W: Re- and Os-rich precipitation along grain boundaries. Comparison of results between this study and previous studies using different irradiation facilities revealed that the microstructural evolution of pure W is highly dependent on the neutron energy spectrum in addition to the irradiation temperature and dose.

Viscoplastic Creep Response and Microstructure of As-Fabricated Microscale Sn-3.0Ag-0.5Cu Solder Interconnects

NASA Astrophysics Data System (ADS)

Cuddalorepatta, Gayatri; Williams, Maureen; Dasgupta, Abhijit

2010-10-01

The viscoplastic behavior of as-fabricated, undamaged, microscale Sn-3.0 Ag-0.5Cu (SAC305) Pb-free solder is investigated and compared with that of eutectic Sn-37Pb solder and near-eutectic Sn-3.8Ag-0.7Cu (SAC387) solder from prior studies. Creep measurements of microscale SAC305 solder shear specimens show significant piece-to-piece variability under identical loading. Orientation imaging microscopy reveals that these specimens contain only a few, highly anisotropic Sn grains across the entire joint. For the studied loads, the coarse-grained Sn microstructure has a more significant impact on the scatter in primary creep compared to that in the secondary creep. The observed lack of statistical homogeneity (microstructure) and joint-dependent mechanical behavior of microscale SAC305 joints are consistent with those observed for functional microelectronics interconnects. Compared with SAC305 joints, microscale Sn-37Pb shear specimens exhibit more homogenous behavior and microstructure with a large number of small Sn (and Pb) grains. Creep damage in the Pb-free joint is predominantly concentrated at highly misoriented Sn grain boundaries. The coarse-grained Sn microstructure recrystallizes into new grains with high misorientation angles under creep loading. In spite of the observed joint-dependent behavior, as-fabricated SAC305 is significantly more creep resistant than Sn-37Pb solder and slightly less creep resistant than near-eutectic SAC387 solder. Average model constants for primary and secondary creep of SAC305 are presented. Since the viscoplastic measurements are averaged over a wide range of grain configurations, the creep model constants represent the effective continuum behavior in an average sense. The average secondary creep behavior suggests that the dominant creep mechanism is dislocation climb assisted by dislocation pipe diffusion.

Development of Age-Hardening Technology for Ultrafine-Grained Al-Li-Cu Alloys Fabricated by High-Pressure Torsion

NASA Astrophysics Data System (ADS)

Motoshima, Hiroaki; Hirosawa, Shoichi; Lee, Seungwon; Horita, Zenji; Matsuda, Kenji; Terada, Daisuke

The age-hardening behavior and precipitation microstructures with high dislocation density and ultrafine grains have been studied for cold-rolled and severely deformed 2091 Al-Li-Cu alloy. The age-hardenability at 463K was reduced by high-pressure torsion (HPT) due to the accelerated formation of larger 8-AlLi precipitates at grain boundaries, in place of transgranular precipitation of refined δ'-Al3Li particles that are predominantly observable in the no-deformed and 10%-rolled specimens. When aged at 373K, however, it was successfully achieved for the HPT specimen to increase the hardness up to 290HV, the highest level of hardness among conventional wrought aluminum alloys. The corresponding TEM microstructures confirmed that refined δ' particles precipitate within ultrafine grains while keeping the grain size at 206nm. This result suggests that the combined processing of severe plastic deformation with age-hardening technique enables the fabrication of novel aluminum alloys concurrently strengthened by ultrafine-grained and precipitation hardenings.

Creep of quartz by dislocation and grain boundary processes

NASA Astrophysics Data System (ADS)

Fukuda, J. I.; Holyoke, C. W., III; Kronenberg, A. K.

2015-12-01

Wet polycrystalline quartz aggregates deformed at temperatures T of 600°-900°C and strain rates of 10-4-10-6 s-1 at a confining pressure Pc of 1.5 GPa exhibit plasticity at low T, governed by dislocation glide and limited recovery, and grain size-sensitive creep at high T, governed by diffusion and sliding at grain boundaries. Quartz aggregates were HIP-synthesized, subjecting natural milky quartz powder to T=900°C and Pc=1.5 GPa, and grain sizes (2 to 25 mm) were varied by annealing at these conditions for up to 10 days. Infrared absorption spectra exhibit a broad OH band at 3400 cm-1 due to molecular water inclusions with a calculated OH content (~4000 ppm, H/106Si) that is unchanged by deformation. Rate-stepping experiments reveal different stress-strain rate functions at different temperatures and grain sizes, which correspond to differing stress-temperature sensitivities. At 600-700°C and grain sizes of 5-10 mm, flow law parameters compare favorably with those for basal plasticity and dislocation creep of wet quartzites (effective stress exponents n of 3 to 6 and activation enthalpy H* ~150 kJ/mol). Deformed samples show undulatory extinction, limited recrystallization, and c-axis maxima parallel to the shortening direction. Similarly fine-grained samples deformed at 800°-900°C exhibit flow parameters n=1.3-2.0 and H*=135-200 kJ/mol corresponding to grain size-sensitive Newtonian creep. Deformed samples show some undulatory extinction and grain sizes change by recrystallization; however, grain boundary deformation processes are indicated by the low value of n. Our experimental results for grain size-sensitive creep can be compared with models of grain boundary diffusion and grain boundary sliding using measured rates of silicon grain boundary diffusion. While many quartz mylonites show microstructural and textural evidence for dislocation creep, results for grain size-sensitive creep may apply to very fine-grained (<10 mm) quartz mylonites.

Characterization of microstructure and texture across dissimilar super duplex/austenitic stainless steel weldment joint by austenitic filler metal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eghlimi, Abbas, E-mail: a.eghlimi@ma.iut.ac.ir; Shamanian, Morteza; Eskandarian, Masoomeh

The evolution of microstructure and texture across an as-welded dissimilar UNS S32750 super duplex/UNS S30403 austenitic stainless steel joint welded by UNS S30986 (AWS A5.9 ER309LMo) austenitic stainless steel filler metal using gas tungsten arc welding process was evaluated by optical micrography and EBSD techniques. Due to their fabrication through rolling process, both parent metals had texture components resulted from deformation and recrystallization. The weld metal showed the highest amount of residual strain and had large austenite grain colonies of similar orientations with little amounts of skeletal ferrite, both oriented preferentially in the < 001 > direction with cub-on-cube orientationmore » relationship. While the super duplex stainless steel's heat affected zone contained higher ferrite than its parent metal, an excessive grain growth was observed at the austenitic stainless steel's counterpart. At both heat affected zones, austenite underwent some recrystallization and formed twin boundaries which led to an increase in the fraction of high angle boundaries as compared with the respective base metals. These regions showed the least amount of residual strain and highest amount of recrystallized austenite grains. Due to the static recrystallization, the fraction of low degree of fit (Σ) coincident site lattice boundaries, especially Σ3 boundaries, was increased in the austenitic stainless steel heat affected zone, while the formation of subgrains in the ferrite phase increased the content of < 5° low angle boundaries at that of the super duplex stainless steel. - Graphical abstract: Display Omitted - Highlights: • Extensive grain growth in the HAZ of austenitic stainless steel was observed. • Intensification of < 100 > orientated grains was observed adjacent to both fusion lines. • Annealing twins with Σ3 CSL boundaries were formed in the austenite of both HAZ. • Cub-on-cube OR was observed between austenite and ferrite in the weld metal. • Weld metal had the lowest texture intensity and ratio of low angle and CSL boundaries.« less

Unraveling Recrystallization Mechanisms Governing Texture Development from Rare Earth Element Additions to Magnesium

NASA Astrophysics Data System (ADS)

Imandoust, Aidin

The origin of texture components associated with rare-earth (RE) element additions in wrought magnesium (Mg) alloys is a long-standing problem in magnesium technology. The objective of this research is to identify the mechanisms accountable for rare-earth texture during dynamic recrystallization (DRX). Towards this end, we designed binary Mg-Cerium and Mg-Gadolinium alloys along with complex alloy compositions containing zinc, yttrium and Mischmetal. Binary alloys along with pure Mg were designed to individually investigate their effects on texture evolutions, while complex compositions are designed to develop randomized texture, and be used in automotive and aerospace applications. We selected indirect extrusion to thermo-mechanically process our materials. Different extrusion ratios and speeds were designed to produce partially and fully recrystallized microstructures, allowing us to analyze DRX from its early stages to completion. X-ray diffraction, electron backscattered diffraction (EBSD) and transmission electron microscopy (TEM) were used to conduct microstructure and texture analyses. Our analyses revealed that rare-earth elements in zinc-containing magnesium alloys promote discontinuous dynamic recrystallization at the grain boundaries. During nucleation, the effect of rare earth elements on orientation selection was explained by the concomitant actions of multiple Taylor axes in the same grain. Isotropic grain growth was observed due to rare earth elements segregating to grain boundaries, which lead to texture randomization. The nucleation in binary Mg-RE alloys took place by continuous formation of necklace structures. Stochastic relaxation of basal and non-basal dislocations into low-angle grain boundaries produced chains of embryos with nearly random orientations. Schmid factor analysis showed a lower net activation of dislocations in RE textured grains compared to ones on the other side of the stereographic triangle. Lower dislocation densities within RE grains favored their growth by setting the boundary migration direction toward grains with higher dislocation density, thereby decreasing the system energy. We investigated the influence of RE elements on extension twinning induced hardening. RE addition enhanced tensile twinning induced hardening significantly. EBSD analysis illustrated that tensile twins cross low angle grain boundaries in Mg-RE alloys, which produced large twins and facilitated transmutation of basal to prismatic dislocations. Higher activity of pyramidal II dislocations in Mg-RE alloys resulted in higher twinning induced hardening.

Impact of Martensite Spatial Distribution on Quasi-Static and Dynamic Deformation Behavior of Dual-Phase Steel

NASA Astrophysics Data System (ADS)

Singh, Manpreet; Das, Anindya; Venugopalan, T.; Mukherjee, Krishnendu; Walunj, Mahesh; Nanda, Tarun; Kumar, B. Ravi

2017-12-01

The effects of microstructure parameters of dual-phase steels on tensile high strain dynamic deformation characteristic were examined in this study. Cold-rolled steel sheets were annealed using three different annealing process parameters to obtain three different dual-phase microstructures of varied ferrite and martensite phase fraction. The volume fraction of martensite obtained in two of the steels was near identical ( 19 pct) with a subtle difference in its spatial distribution. In the first microstructure variant, martensite was mostly found to be situated at ferrite grain boundaries and in the second variant, in addition to at grain boundaries, in-grain martensite was also observed. The third microstructure was very different from the above two with respect to martensite volume fraction ( 67 pct) and its morphology. In this case, martensite packets were surrounded by a three-dimensional ferrite network giving an appearance of core and shell type microstructure. All the three steels were tensile deformed at strain rates ranging from 2.7 × 10-4 (quasi-static) to 650 s-1 (dynamic range). Field-emission scanning electron microscope was used to characterize the starting as well as post-tensile deformed microstructures. Dual-phase steel consisting of small martensite volume fraction ( 19 pct), irrespective of its spatial distribution, demonstrated high strain rate sensitivity and on the other hand, steel with large martensite volume fraction ( 67 pct) displayed a very little strain rate sensitivity. Interestingly, total elongation was found to increase with increasing strain rate in the dynamic regime for steel with core-shell type of microstructure containing large martensite volume fraction. The observed enhancement in plasticity in dynamic regime was attributed to adiabatic heating of specimen. To understand the evolving damage mechanism, the fracture surface and the vicinity of fracture ends were studied in all the three dual-phase steels.

Impact of Martensite Spatial Distribution on Quasi-Static and Dynamic Deformation Behavior of Dual-Phase Steel

NASA Astrophysics Data System (ADS)

Singh, Manpreet; Das, Anindya; Venugopalan, T.; Mukherjee, Krishnendu; Walunj, Mahesh; Nanda, Tarun; Kumar, B. Ravi

2018-02-01

The effects of microstructure parameters of dual-phase steels on tensile high strain dynamic deformation characteristic were examined in this study. Cold-rolled steel sheets were annealed using three different annealing process parameters to obtain three different dual-phase microstructures of varied ferrite and martensite phase fraction. The volume fraction of martensite obtained in two of the steels was near identical ( 19 pct) with a subtle difference in its spatial distribution. In the first microstructure variant, martensite was mostly found to be situated at ferrite grain boundaries and in the second variant, in addition to at grain boundaries, in-grain martensite was also observed. The third microstructure was very different from the above two with respect to martensite volume fraction ( 67 pct) and its morphology. In this case, martensite packets were surrounded by a three-dimensional ferrite network giving an appearance of core and shell type microstructure. All the three steels were tensile deformed at strain rates ranging from 2.7 × 10-4 (quasi-static) to 650 s-1 (dynamic range). Field-emission scanning electron microscope was used to characterize the starting as well as post-tensile deformed microstructures. Dual-phase steel consisting of small martensite volume fraction ( 19 pct), irrespective of its spatial distribution, demonstrated high strain rate sensitivity and on the other hand, steel with large martensite volume fraction ( 67 pct) displayed a very little strain rate sensitivity. Interestingly, total elongation was found to increase with increasing strain rate in the dynamic regime for steel with core-shell type of microstructure containing large martensite volume fraction. The observed enhancement in plasticity in dynamic regime was attributed to adiabatic heating of specimen. To understand the evolving damage mechanism, the fracture surface and the vicinity of fracture ends were studied in all the three dual-phase steels.

The influence of manufacturing processes on the microstructure, grain boundary characteristics and SCC behavior of Alloy 690 steam generator tubing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sarver, J.M.; Doherty, P.E.; Doyle, D.M.

1995-12-31

Thermally treated Alloy 690 is the tubing material of choice for replacement steam generators in the United States. Throughout the world, it is manufactured using different melting and thermomechanical processing methods. The influence of different processing steps on the intergranular stress corrosion cracking (IGSCC) behavior of Alloy 690 has not been thoroughly evaluated. Evaluations were performed on Alloy 690 steam generator tubing produced using several different melting practices and thermomechanical processing procedures. The evaluations included extensive microstructural examinations as well as constant extension rate (CERT) tests. The CERT test results indicated that the thermally treated Alloy 690 tubing which wasmore » subjected to higher annealing temperatures displayed the highest degree of resistance to stress corrosion cracking (SCC). Examination of the microstructures indicated that the microstructural changes which are produced by increased annealing temperatures are subtle. In an attempt to further elucidate and quantify the effect of manufacturing processes on corrosion behavior, grain boundary character distribution (GBCD) measurements were performed on the same materials which were CERT tested. Analysis of GBCDs of the samples used in this study indicate that Alloy 690 exhibits a significantly larger fraction of special boundaries as compared to Alloy 600 and Alloy 800, regardless of the processing history of the tubing. Preliminary results indicate that a correlation may exist between processing method, GBCD`s and degree of IGSCC exhibited by the thermally treated samples examined in this study.« less

Formation of Widmanstätten Austenite in Strip Cast Grain-Oriented Silicon Steel

NASA Astrophysics Data System (ADS)

Song, Hong-Yu; Liu, Hai-Tao; Wang, Guo-Dong; Jonas, John J.

2017-04-01

The formation of Widmanstätten austenite was studied in strip cast grain-oriented silicon steel. The microstructure was investigated by optical microscopy and scanning electron microscopy. The orientations of the ferrite, Widmanstätten austenite, and martensite were determined using electron backscatter diffraction. The Widmanstätten austenite exhibits a lath-like shape and nucleates directly on the ferrite grain boundaries. This differs significantly from earlier work on duplex stainless steels. The orientation relationship between the Widmanstätten austenite and the parent ferrite is closer to Kurdjumov-Sachs than to Nishiyama-Wassermann. The ferrite boundaries migrate so as to accommodate the habit planes of the laths, leading to the presence of zigzag boundaries in the as-cast strip. Carbon partitioning into the Widmanstätten austenite and silicon partitioning into the parent ferrite were observed.

Friction stir welded AM50 and AZ31 Mg alloys: Microstructural evolution and improved corrosion resistance

DOE Office of Scientific and Technical Information (OSTI.GOV)

Templeman, Yael

One of the major drawbacks of Mg alloys is poor weldability, caused by porosity formation during conventional fusion welding processes. Friction Stir Welding (FSW) is promising technique in this context since it is a solid state technique. Contradicting results were published in the literature regarding the FSWed Mg alloys joint's properties. Current research was performed in order to investigate the microstructure and corrosion properties of FSWed Mg alloys, studying representatives of two commercial families: wrought AZ31-H24 and die cast AM50. It was found that in both alloys recrystallization occurred during the FSW. In AM50 the mechanism of the recrystallization wasmore » continuous, manifested by dislocation rearrangement into sub grain boundaries. In AZ31 discontinuous recrystallization had occurred through grain boundaries migration - twins rotated with respect to the matrix, turning into low angle grain boundaries. Corrosion resistance has improved during the FSW in both alloys to different extents. In the AM50 alloy, the nugget exhibited significantly higher surface potential than the base metal mainly due to the higher Al concentration in the matrix of the nugget, resulting from the dissolution of Al-enrichment and β-Mg{sub 17}Al{sub 12} phase. In the AZ31 alloy, no change in Al concentration had occurred, and the surface potential measured in the nugget was only slightly higher than in the base metal. These results underline the appropriateness of the FSW for Mg alloys since during the conventional welding deterioration of the corrosion resistance occurs. - Highlights: • Following FSW, AZ31-H24 experienced discontinuous recrystallization. • In AZ31 grain boundaries migration occurred, thus twins rotated. • In die cast AM50 continuous recrystallization occurred during the FSW. • In AM50 - dislocations rearranged into sub grain boundaries. • Corrosion resistance has improved during the FSW in both alloys to different extent.« less

Extreme creep resistance in a microstructurally stable nanocrystalline alloy

NASA Astrophysics Data System (ADS)

Darling, K. A.; Rajagopalan, M.; Komarasamy, M.; Bhatia, M. A.; Hornbuckle, B. C.; Mishra, R. S.; Solanki, K. N.

2016-09-01

Nanocrystalline metals, with a mean grain size of less than 100 nanometres, have greater room-temperature strength than their coarse-grained equivalents, in part owing to a large reduction in grain size. However, this high strength generally comes with substantial losses in other mechanical properties, such as creep resistance, which limits their practical utility; for example, creep rates in nanocrystalline copper are about four orders of magnitude higher than those in typical coarse-grained copper. The degradation of creep resistance in nanocrystalline materials is in part due to an increase in the volume fraction of grain boundaries, which lack long-range crystalline order and lead to processes such as diffusional creep, sliding and rotation. Here we show that nanocrystalline copper-tantalum alloys possess an unprecedented combination of properties: high strength combined with extremely high-temperature creep resistance, while maintaining mechanical and thermal stability. Precursory work on this family of immiscible alloys has previously highlighted their thermo-mechanical stability and strength, which has motivated their study under more extreme conditions, such as creep. We find a steady-state creep rate of less than 10-6 per second—six to eight orders of magnitude lower than most nanocrystalline metals—at various temperatures between 0.5 and 0.64 times the melting temperature of the matrix (1,356 kelvin) under an applied stress ranging from 0.85 per cent to 1.2 per cent of the shear modulus. The unusual combination of properties in our nanocrystalline alloy is achieved via a processing route that creates distinct nanoclusters of atoms that pin grain boundaries within the alloy. This pinning improves the kinetic stability of the grains by increasing the energy barrier for grain-boundary sliding and rotation and by inhibiting grain coarsening, under extremely long-term creep conditions. Our processing approach should enable the development of microstructurally stable structural alloys with high strength and creep resistance for various high-temperature applications, including in the aerospace, naval, civilian infrastructure and energy sectors.

Effect of cold rolling on microstructure and mechanical property of extruded Mg–4Sm alloy during aging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Rongguang, E-mail: lirongguang1980@126.com; Xin, Renlong; Chapuis, Adrien

Microstructure and mechanical properties of the Mg–4Sm (wt.%) alloy, prepared via combined processes of extrusion, cold rolling and aging, have been investigated. The hot extruded alloy exhibits a weak rare earth magnesium alloy texture with < 11 − 21 >//ED, while the cold-rolled alloy shows a stronger basal texture with < 0001 >//ND. Many tensile twins and double twins are observed in grains after rolling. The cold-rolled alloy shows a weak age-hardening response compared with the extruded alloy, which is the result of more precipitation in the twin boundary during aging. The rolled alloy exhibits almost no precipitate free zonemore » during aging compared with the extruded alloy. The higher proof stress of the rolled alloy in peak-aged condition is attributed to the presence of twin boundaries, stronger basal texture, higher dislocation density, and the suppression of precipitate free zone compared with the extruded alloy. - Highlights: • No precipitate free zone appears in cold-rolled alloy after aging. • Segregation and precipitates are observed in twin boundaries and grain boundaries. • Cold-rolled alloy shows a weak age-hardening response.« less

Annealing Effects on Microstructure and Mechanical Properties of Ultrafine-Grained Al Composites Reinforced with Nano-Al2O3 by Rotary Swaging

NASA Astrophysics Data System (ADS)

Chen, Cunguang; Wang, Wenwen; Guo, Zhimeng; Sun, Chunbao; Volinsky, Alex A.; Paley, Vladislav

2018-03-01

Microstructure evolution and variations in mechanical properties of Al-Al2O3 nanocomposite produced by powder metallurgy were investigated and compared with commercially pure aluminum (Al-1050) after furnace annealing. Fine gas-atomized Al powder compacts were first sintered in flowing nitrogen, subsequently consolidated into wires by rotary swaging and eventually annealed at 300 and 500 °C for 24 h each. Scanning and transmission electron microscopy with energy-dispersive spectroscopy was utilized to document the microstructure evolution. Rotary swaging was proven to lead to a marked decrease in grain size. After heavy swaging to true deformation degree of φ = 6 and annealing at 500 °C, obvious recrystallization was observed at Al-1050's existing grain boundaries and the crystals began to grow perpendicular to the flow direction. In the Al-Al2O3 nanocomposite, fabricated from d 50 = 6 μm Al powder, recrystallization partially occurred, while grains were still extremely fine. Due to the dual role of fine-grained Al2O3 dispersion strengthening, the nanocomposite showed improved mechanical performance in terms of tensile strength, approximately twice higher than Al-1050 after annealing at 500 °C.

Method of manufacture of single phase ceramic superconductors

DOEpatents

Singh, J.P.; Poeppel, R.B.; Goretta, K.C.; Chen, N.

1995-03-28

A ceramic superconductor is produced by close control of oxygen partial pressure during sintering of the material. The resulting microstructure of YBa{sub 2}Cu{sub 3}O{sub x} indicates that sintering kinetics are enhanced at reduced p(O{sub 2}) and that because of second phase precipitates, grain growth is prevented. The density of specimens sintered at 910 C increased from 79 to 94% theoretical when p(O{sub 2}) was decreased from 0.1 to 0.0001 MPa. The increase in density with decrease in p(O{sub 2}) derives from enhanced sintering kinetics, due to increased defect concentration and decreased activation energy of the rate-controlling species undergoing diffusion. Sintering at 910 C resulted in a fine-grain microstructure, with an average grain size of about 4 {mu}m. Post sintering annealing in a region of stability for the desired phase converts the second phases and limits grain growth. The method of pinning grain boundaries by small scale decompositive products and then annealing to convert its product to the desired phase can be used for other complex asides. Such a microstructure results in reduced microcracking, strengths as high as 230 MPa and high critical current density capacity. 25 figures.

Method of manufacture of single phase ceramic superconductors

DOEpatents

Singh, Jitrenda P.; Poeppel, Roger B.; Goretta, Kenneth C.; Chen, Nan

1995-01-01

A ceramic superconductor is produced by close control of oxygen partial pressure during sintering of the material. The resulting microstructure of YBa.sub.2 Cu.sub.3 O.sub.x indicates that sintering kinetics are enhanced at reduced p(O.sub.2) and that because of second phase precipitates, grain growth is prevented. The density of specimens sintered at 910.degree. C. increased from 79 to 94% theoretical when p(O.sub.2) was decreased from 0.1 to 0.0001 MPa. The increase in density with decrease in p(O.sub.2) derives from enhanced sintering kinetics, due to increased defect concentration and decreased activation energy of the rate-controlling species undergoing diffusion. Sintering at 910.degree. C resulted in a fine-grain microstructure, with an average grain size of about 4 .mu.m. Post sintering annealing in a region of stability for the desired phase converts the second phases and limits grain growth. The method of pinning grain boundaries by small scale decompositive products and then annealing to convert its product to the desired phase can be used for other complex asides. Such a microstructure results in reduced microcracking, strengths as high as 230 MPa and high critical current density capacity.

Influences of electric current on the wettability and interfacial microstructure in Sn/Fe system

NASA Astrophysics Data System (ADS)

Shen, Ping; Gu, Yan; Yang, Nan-Nan; Zheng, Rui-Peng; Ren, Li-Hua

2015-02-01

The wettability of oxidized and clean Fe substrates by liquid Sn was investigated using a dispensed sessile drop method with and without the application of a direct current (DC) and their interfacial microstructures were compared. The initial contact angles were 107 ± 3° at 623 K when the Fe substrate was covered by an oxide film, and they did not show an appreciable decrease during isothermal dwells in the absence of DC application but progressively decreased to 42 ± 3° when a 7.5 ampere current was applied. However, in the case of the oxide film being removed by a high-vacuum pre-annealing treatment at 1073 K, the current and its polarity had a negligible effect on the wetting behavior. Nevertheless, they had a noticeable influence on the interfacial microstructure. In the absence of DC, the interface was covered by a product layer consisting of a single FeSn2 phase for the samples tested at 623 K and the FeSn2/FeSn2 grain boundaries were incompletely wetted by the Sn melt; whereas, under DC, the reaction layer was much thicker and the Sn melt wet well the FeSn2/FeSn2 grain boundaries. Moreover, a FeSn phase also formed as a result of enhanced mass transfer. The amount of the FeSn phase was larger and the grain boundary wetting of FeSn2 by liquid Sn was better for the current flowing from the molten Sn drop to the Fe substrate due to an electromigration effect.

Effect of isothermal heat treatment on microstructure and mechanical properties of Reduced Activation Ferritic Martensitic steel

NASA Astrophysics Data System (ADS)

Chandravathi, K. S.; Sasmal, C. S.; Laha, K.; Parameswaran, P.; Nandagopal, M.; Vijayanand, V. D.; Mathew, M. D.; Jayakumar, T.; Rajendra Kumar, E.

2013-04-01

Hardness, tensile properties and microstructural changes in 9Cr-1W-0.06Ta-0.22V-0.08C Reduced Activation Ferritic-Martensitic steel have been investigated after subjecting the steel with isothermal heat treatments for 5 min at temperatures in the range 973-1473 K (below Ac1 to above Ac3 transformation temperatures) followed by oil quenching and tempering at 1033 K for 1 h. These studies have been carried out in an effort to assess the strength of the steel at different microstructural conditions. Optical, scanning and transmission electron microscopic investigations have been carried out to assess the microstructural changes of the steel upon various heat treatments. The steel developed predominantly tempered martensitic structure after the heat treatments. The hardness, tensile strength and the prior austenitic grain size of the steel exhibited minimum values for soaking heat treatment in the intercritical temperature range (i.e.) between Ac1 and Ac3; whereas the ductility was maximum. With increase in isothermal heat treatment temperature above Ac3, hardness, tensile strength and grain size of the steel were found to increase with consequent decrease in tensile ductility. TEM investigations revealed that the coarsening of subgrain and precipitates at grain and sub-grain boundaries on heat treatment of the steel in the inter-critical temperature range. The tensile properties of the steel have been correlated with microstructure.

Multiscale Analysis of Structurally-Graded Microstructures Using Molecular Dynamics, Discrete Dislocation Dynamics and Continuum Crystal Plasticity

NASA Technical Reports Server (NTRS)

Saether, Erik; Hochhalter, Jacob D.; Glaessgen, Edward H.; Mishin, Yuri

2014-01-01

A multiscale modeling methodology is developed for structurally-graded material microstructures. Molecular dynamic (MD) simulations are performed at the nanoscale to determine fundamental failure mechanisms and quantify material constitutive parameters. These parameters are used to calibrate material processes at the mesoscale using discrete dislocation dynamics (DD). Different grain boundary interactions with dislocations are analyzed using DD to predict grain-size dependent stress-strain behavior. These relationships are mapped into crystal plasticity (CP) parameters to develop a computationally efficient finite element-based DD/CP model for continuum-level simulations and complete the multiscale analysis by predicting the behavior of macroscopic physical specimens. The present analysis is focused on simulating the behavior of a graded microstructure in which grain sizes are on the order of nanometers in the exterior region and transition to larger, multi-micron size in the interior domain. This microstructural configuration has been shown to offer improved mechanical properties over homogeneous coarse-grained materials by increasing yield stress while maintaining ductility. Various mesoscopic polycrystal models of structurally-graded microstructures are generated, analyzed and used as a benchmark for comparison between multiscale DD/CP model and DD predictions. A final series of simulations utilize the DD/CP analysis method exclusively to study macroscopic models that cannot be analyzed by MD or DD methods alone due to the model size.

Effect of microstructure on high-temperature mechanical behavior of nickel-base superalloys for turbine disc applications

NASA Astrophysics Data System (ADS)

Sharpe, Heather Joan

2007-05-01

Engineers constantly seek advancements in the performance of aircraft and power generation engines, including, lower costs and emissions, and improved fuel efficiency. Nickel-base superalloys are the material of choice for turbine discs, which experience some of the highest temperatures and stresses in the engine. Engine performance is proportional to operating temperatures. Consequently, the high-temperature capabilities of disc materials limit the performance of gas-turbine engines. Therefore, any improvements to engine performance necessitate improved alloy performance. In order to take advantage of improvements in high-temperature capabilities through tailoring of alloy microstructure, the overall objectives of this work were to establish relationships between alloy processing and microstructure, and between microstructure and mechanical properties. In addition, the projected aimed to demonstrate the applicability of neural network modeling to the field of Ni-base disc alloy development and behavior. The first phase of this work addressed the issue of how microstructure varies with heat treatment and by what mechanisms these structures are formed. Further it considered how superalloy composition could account for microstructural variations from the same heat treatment. To study this, four next-generation Ni-base disc alloys were subjected to various controlled heat-treatments and the resulting microstructures were then quantified. These quantitative results were correlated to chemistry and processing, including solution temperature, cooling rate, and intermediate hold temperature. A complex interaction of processing steps and chemistry was found to contribute to all features measured; grain size, precipitate distribution, grain boundary serrations. Solution temperature, above a certain threshold, and cooling rate controlled grain size, while cooling rate and intermediate hold temperature controlled precipitate formation and grain boundary serrations. Diffusion, both intergranular and grain boundary, was identified as the most pertinent mechanism. Variations in chemistry between alloys created different amounts of gamma/gamma' misfit strain, which affected precipitate size and morphology. Next the question of how a disc alloy with differing microstructures would respond to constant or cyclic stresses as a function of time was addressed. To this end, mechanical testing at elevated temperatures was conducted, including tensile, hardness, creep deformation, creep crack growth and fatigue crack growth. Overall, mechanical properties were primarily related to the cooling rate during processing with hold temperatures being secondary. Whether the impact was positive or negative depended on the behavior under consideration. Fast cooling rates improved yield strength and creep resistance, but were detrimental to creep crack growth rates. The ability of precipitate particles to impede dislocation motion was the most frequently cited mechanism behind structure-property interaction. Neural network models were successfully generated for processing-structure predictions, as well as for structure-property predictions. Training data was limited, none-the-less models were able to predict outputs with minimal relative errors. This was achieved through careful balance between the number of inputs and amount of training data. Despite the demonstrated correlation between microstructure and yield strength, microstructural quantities did not need to be directly inputted. Neural networks were sufficiently sensitive as to infer these effects from processing and chemistry inputs. This result improves the efficiency of this technique, while also demonstrating the capability of neural network techniques. A full program of heat-treatment, microstructure quantification, mechanical testing, and neural network modeling was successfully applied to next generation Ni-base disc alloys. From this work the mechanisms of processing-structure and structure-property relationships were studied. Further, testing results were used to demonstrate the applicability of machine-learning techniques to the development and optimization of this family of superalloys.

Microstructural evolution of diamond films from CH{sub 4}/H{sub 2}/N{sub 2} plasma and their enhanced electrical properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sankaran, K. J.; Tai, N. H., E-mail: nhtai@mx.nthu.edu.tw; Lin, I. N., E-mail: inanlin@mail.tku.edu.tw

2015-02-21

The influence of N{sub 2} concentration in CH{sub 4}/H{sub 2}/N{sub 2} plasma on microstructural evolution and electrical properties of diamond films is systematically investigated. While the diamond films grown in CH{sub 4}/H{sub 2} plasma contain large diamond grains, for the diamond films grown using CH{sub 4}/H{sub 2}/(4%)N{sub 2} plasma, the microstructure drastically changed, resulting in ultra-nanosized diamond grains with Fd3m structure and a{sub 0} = 0.356 nm, along with the formation of n-diamond (n-D), a metastable form of diamond with space group Fm3m and a{sub 0} = 0.356 nm, and i-carbon (i-C) clusters, the bcc structured carbon with a{sub 0} = 0.432 nm. In addition, these films contain widemore » grain boundaries containing amorphous carbon (a-C). The electron field emission (EFE) studies show the best EFE behavior for 4% N{sub 2} films among the CH{sub 4}/H{sub 2}/N{sub 2} grown diamond films. They possess the lowest turn-on field value of 14.3 V/μm and the highest EFE current density value of 0.37 mA/cm{sup 2} at an applied field of 25.4 V/μm. The optical emission spectroscopy studies confirm that CN species are the major criterion to judge the changes in the microstructure of the films. It seems that the grain boundaries can provide electron conduction networks to transport efficiently the electrons to emission sites for field emission, as long as they have sufficient thickness. Whether the matrix nano-sized grains are 3C-diamond, n-D or i-C is immaterial.« less

Thermal stability of the microstructure of silver films

NASA Astrophysics Data System (ADS)

Sursaeva, V. G.; Straumal, A. B.

2017-04-01

The thermal stability of freely suspended silver films 100 nm thick is studied during isothermal annealing at temperatures of 350-600°C for different times. At temperatures of 350-450°C, only grain growth is observed. Above 450°C, along with grain growth, the formation and growth of hillocks and holes take place; in this case, grain boundaries are essential in the processes. A continuous film transforms into a cellular one. At 500°C, the growth processes of both grains and holes have the same incubation period, during which no grain growth, hole formation, and hole growth take place.

The deformation record of olivine in mylonitic peridotites from the Finero Complex, Ivrea Zone: Separate deformation cycles during exhumation

NASA Astrophysics Data System (ADS)

Matysiak, Agnes K.; Trepmann, Claudia A.

2015-12-01

Mylonitic peridotites from the Finero complex are investigated to detect characteristic olivine microfabrics that can resolve separate deformation cycles at different metamorphic conditions. The heterogeneous olivine microstructures are characterized by deformed porphyroclasts surrounded by varying amounts of recrystallized grains. A well-developed but only locally preserved foam structure is present in recrystallized grain aggregates. This indicates an early stage of dynamic recrystallization and subsequent recovery and recrystallization at quasi-static stress conditions, where the strain energy was reduced such that a reduction in surface energy controlled grain boundary migration. Ultramylonites record a renewed stage of localized deformation and recrystallization by a second generation of recrystallized grains that do not show a foam structure. This second generation of recrystallized grains as well as sutured grain and kink band boundaries of porphyroclasts indicate that these microstructures developed during a stage of localized deformation after development of the foam structure. The heterogeneity of the microfabrics is interpreted to represent several (at least two) cycles of localized deformation separated by a marked hiatus with quasi-static recrystallization and recovery and eventually grain growth. The second deformation cycle did not only result in reactivation of preexisting shear zones but instead also locally affected the host rock that was not deformed in the first stage. Such stress cycles can result from sudden increases in differential stress imposed by seismic events, i.e., high stress-loading rates, during exhumation of the Finero complex.

Structure-composition-property relationships in 5xxx series aluminum alloys

NASA Astrophysics Data System (ADS)

Unocic, Kinga A.

Al-Mg alloys are well suited for marine applications due to their low density, ease of fabrication, structural durability, and most notably resistance to corrosion. The purpose of this study is to investigate the effects of alloying additions, mechanical processing and heat treatments on the development of grain boundary phases that have an effect on intergranular corrosion (IGC). Cu, Zn, and Si modified compositions of AA5083 were produced that were subjected to a low and high degree of cold work and various heat treatments. ASTM G67 (NAMLT) intergranular corrosion testing and detailed microstructural characterization for various alloys was carried out. An optimal composition and processing condition that yielded the best intergranular corrosion resistant material was identified based on the ASTM G67 test screening. Further, the outstanding modified AA5083 was selected for further microstructural analysis. This particular alloy with has a magnesium level high enough to make it susceptible to intergranular corrosion is very resistant to IGC. It was found that development of the appropriate sub-structure with some Cu, Si and Zn resulted in a material very resistant to IGC. Formation of many sinks, provided by sub-boundaries, within microstructure is very beneficial since it produces a relatively uniform distribution of Mg in the grain interiors, and this can suppress sensitization of this alloy very successfully. This is a very promising rote for the production of high-strength, and corrosion resistant aluminum alloys. Additionally in this study, TEM sample preparation become very crucial step in grain boundary phase investigation. Focus Ion Beam (FIB) milling was used as a primary TEM sample preparation technique because it enables to extract the samples from desired and very specific locations without dissolving grain boundary phases as it was in conventional electropolishing method. However, other issues specifically relevant to FIB milling of aluminum alloys related to Ga accumulation were discovered, that produce significant microstructural artifacts. It is well known that liquid gallium can cause Liquid Metal Embitterment (LME) aluminum alloys, and gallium readily penetrates aluminum grain boundaries. Low energy Ar ion nanomilling is potentially quite effective at removing gallium from the external and internal surfaces of aluminum thin foils, but can still leave persistent artifacts. Al-Mg alloys can be also susceptible to localized corrosion such as pitting corrosion in the presence of chloride ions. In this study the phases responsible for this type of corrosion were identified. ASSET (ASTM G66) test was used to determine the influence of heat-treatment on pitting corrosion on various modified AA5083 alloys. Additionally, potentiodynamic polarization as well as potentiostatic measurements in conjunction with SEM analysis were carried out to obtain pitting potential (Epit) and to determine the location of metastable pit initiation, respectively.

Relationship between chemistry, microstructure and mechanical properties of alpha-silicon aluminum oxynitride

NASA Astrophysics Data System (ADS)

Shuba, Roman

The aim of this thesis was to improve the mechanical properties of Y-alpha-SiAlON ceramics by controlling microstructure and tailoring grain boundary composition. Three properties of importance for engineering applications were targeted: strength retention and oxidation resistance at high temperature, fracture toughness at room temperature, and machinability. As a result of this work, several ceramics with one or more of the above properties optimized have been developed. The performance of Si3N4/SiAlON-based ceramics at high (>1000 degree C) temperature is generally limited by the softening of grain-boundary glass. Refractory alpha-SiAlONs was obtained by three methods: reducing residual liquid by minimizing nitride powder oxidation during processing, promoting liquid/SiAlON conversion by adding excess AlN, and improving refractoriness by incorporating La2O3 into glass. Ceramics thus, obtained featured excellent room-temperature strength (1050 MPa) and high-temperature strength (650 MPa at 1300 degree C), as well as good oxidation resistance. In all cases grain growth was inhibited, which resulted in a relatively low toughness (5--7 MPa x m1/2). In-situ toughened Y-alpha-SiAlON (9 MPa x m1/2) was obtained through growth of large elongated grains with low debonding strength. This was achieved by introducing seed crystals to the starting powder mixtures, in addition to using sintering aids and dopants. Additives modified the properties of grain boundary glass, while dopants lowered the strength of glass/grain interface. Through the use of nanosized turbostratic BN precursor obtained via pyrolysis of melamine borate salt, which yielded finely dispersed hexagonal BN particles in alpha-SiAlON, high-strength (800 MPa) Y-alpha-SiAlON/BN composites, machinable using WC/Co tools, were also fabricated.

Textural evolution of plagioclase feldspar across a shear zone: Implications for deformation mechanism and rock strength

NASA Astrophysics Data System (ADS)

Putnis, Andrew; Austrheim, Håkon; Mukai, Hiroki; Putnis, Christine V.

2014-05-01

Caledonian amphibolite facies shear zones developed in granulite facies anorthosites and anorthositic gabbros of the Bergen Arcs, western Norway allow a detailed study of the relationships between fluid-infiltration, mineral reactions, the evolution of microstructure and deformation mechanisms. A sequence of rocks from the relatively pristine granulites into a shear zone has been studied by optical microscopy, EMPA, SEM, EBSD and TEM, focusing on the progressive development of microstructure in the plagioclase feldspars, leading up to their deformation in the shear zone. At the outcrop scale, fluid infiltration into the granulites is marked by a distinct colour change in the plagioclase from lilac/brown to white. This is associated with the breakdown of the intermediate composition plagioclase (~An50) in the granulite to a complex intergrowth of Na-rich and Ca-rich domains. EBSD analysis shows that this intergrowth retains the crystallographic orientation of the parent feldspar, but that the Ca-rich domains contain many low-angle boundaries as well as twin-related domains. Within the shear zone, this complex intergrowth coarsens by grain boundary migration, annihilating grain boundaries but retaining the Na-rich and Ca-rich zoning pattern. Analysis of nearest-neighbour misorientations of feldspar grains in the shear zone demonstrates that local crystallographic preferred orientation (CPO) is inherited from the parent granulite grain orientations. Random pair misorientation angle distributions show that there is no CPO in the shear zone as a whole, nor is there significant shape preferred orientation (SPO) in individual grains. These observations are interpreted in terms of fluid-induced weakening and deformation by dissolution-precipitation (pressure solution) creep.

Effects of rolling conditions on recrystallization microstructure and texture in magnetostrictive Fe-Ga-Al rolled sheets

NASA Astrophysics Data System (ADS)

Li, Jiheng; Liu, Yangyang; Li, Xiaojuan; Mu, Xing; Bao, Xiaoqian; Gao, Xuexu

2018-07-01

The effects of different rolling conditions on the microstructure and texture of primary and secondary recrystallization in magnetostrictive Fe82Ga9Al9+0.1at%NbC alloy sheets were investigated. After the primary recrystallization annealing at 850 °C for 5 min, the as-rolled sheets prepared by warm-cold rolling with an intermediate annealing, can be fully recrystallized, and obtain the homogeneous matrix in which the fine dispersed NbC precipitate particles are distributed. The primary recrystallization textures of sheets with different rolling conditions consist mostly of strong {1 0 0} textures, γ-fiber textures, {4 1 1}〈1 4 8〉 texture and weak Goss texture. In the primary recrystallized sheets prepared by warm-cold rolling with an intermediate annealing, the high energy grain boundaries and ∑9 boundaries have the highest proportion. After high temperature annealing, the secondary recrystallizations of Goss grains in these sheets are more complete, and the size of abnormal grown Goss grain is up to several centimeters, which results in the strongest Goss texture. Correspondingly, the largest magnetostriction of 183 ppm is observed. The sample prepared by warm-cold rolling with an intermediate annealing, has homogeneous primary matrix, special texture components and grain boundary distribution, all of which provide a better surrounding for the abnormal growth of Goss grains. This work indicates that the control of rolling conditions of Fe-Ga-Al alloy sheets is necessary to achieve the strong Goss texture and obtain a possible high magnetostriction if other appropriate conditions (stress, domain structure) are achieved.

Effect of oxygen content of Nd-Fe-B sintered magnet on grain boundary diffusion process of DyH2 dip-coating

NASA Astrophysics Data System (ADS)

Bae, Kyoung-Hoon; Lee, Seong-Rae; Kim, Hyo-Jun; Lee, Min-Woo; Jang, Tae-Suk

2015-11-01

We investigated the effect of oxygen content on the microstructural and magnetic properties of a DyH2 dip-coated Nd-Fe-B sintered magnet. When the magnet had a low oxygen content (1500 ppm), the volume and size of the rare-earth-rich oxide (Nd-Dy-O) phase was reduced, and a uniform and continuous thin Nd-rich grain boundary phase (GBP) was well developed. The grain boundary diffusion depth of Dy increased from 200 to 350 μm with decreasing oxygen content from ˜3000 to 1500 ppm. The coercivity of the low-oxygen magnet increased from 19.98 to 23.59 kOe after grain boundary diffusion process (GBDP) while the remanence reduction was minimized. The formation of an fcc-NdOx Nd-rich phase in the high-oxygen magnet hindered the formation of a Nd-rich triple-junction phase and GBP. In contrast, a metallic dhcp-Nd phase, which was closely related to coercivity enhancement after GBDP, was formed in the low-oxygen magnet.

Microstructural Characterization and Mechanical Properties Analysis of Weld Metals with Two Ni Contents During Post-Weld Heat Treatments

NASA Astrophysics Data System (ADS)

Wu, Da-yong; Han, Xiu-lin; Tian, Hong-tao; Liao, Bo; Xiao, Fu-ren

2015-05-01

This study designed post-weld heat treatments, including reheating and tempering, associated with hot bending to investigate the microstructures, toughness, and hardness of two weld metals with different Ni contents (<1 wt pct level). The results indicated that a high Ni content decreased the ferrite transformation temperature and increased the proportion of acicular ferrite (AF). Furthermore, a high Ni content promoted the martensite/austenite (M/A) constituent formation after reheating. The promotion of the M/A formation increased the number of cementite particles, and accelerated cementite coarsening during tempering. The large-angle grain boundary density from the AF improved the toughness despite the negative effect of cementite. The strengthening contributions were calculated, and the grain refinement was the greatest. The high Ni content decreased the effective grain size with a 2 deg tolerance angle, thus enhancing the grain refinement contribution.

The microstructure and properties of rapidly solidified, dispersion-strengthened NiAl

NASA Technical Reports Server (NTRS)

Jha, S. C.; Ray, R.

1990-01-01

An advanced rapid solidification technology for processing reactive and refractory alloys, utilized to produce large quantities of melt-spun filaments of NiAl, is presented. The melt-spun filaments are pulverized to fine particle sizes, and subsequently consolidated by hot extrusion or hot isostatic pressing. Rapid solidification process gives rise to very fine-grained microstructures. However, exposure to elevated temperature during hot consolidation leads to grain growth. Alloying agents such as borides, carbides, and tungsten can pin the grain boundaries and retard the grain growth. Various alloy compositions are investigated. The eventual goal is to utilize the hot-extruded and forged stock to grow single-crystal NiAl blades for advanced gas-turbine engine applications. Single-crystal NiAl, containing a uniform dispersion of carbide strengthening precipitates, is expected to lead to highly creep-resistant turbine blades, and is of considerable interest to the aerospace propulsion industry.

Colossal internal barrier layer capacitance effect in polycrystalline copper (II) oxide

NASA Astrophysics Data System (ADS)

Sarkar, Sudipta; Jana, Pradip Kumar; Chaudhuri, B. K.

2008-01-01

Dielectric spectroscopy analysis of the high permittivity (κ˜104) copper (II) oxide (CuO) ceramic shows that the grain contribution plays a major role for the giant-κ value at low temperature, whereas grain boundary (GB) contribution dominates around room temperature and above. Moreover, impedance spectroscopy analysis reveals electrically heterogeneous microstructure in CuO consisting of semiconducting grains and insulating GBs. Finally, the giant dielectric phenomenon exhibited by CuO is attributed to the internal barrier layer (due to GB) capacitance mechanism.

Effects of sputtering mode on the microstructure and ionic conductivity of yttria-stabilized zirconia films

NASA Astrophysics Data System (ADS)

Yeh, Tsung-Her; Lin, Ruei-De; Cherng, Bo-Ruei; Cherng, Jyh-Shiarn

2018-05-01

The microstructure and ionic conductivity of reactively sputtered yttria-stabilized zirconia (YSZ) films are systematically studied. Those films were reactively sputtered in various sputtering modes using a closed-loop controlled system with plasma emission monitoring. A transition-mode sputtering corresponding to 45% of target poisoning produces a microstructure with ultrafine crystallites embedded in an amorphous matrix, which undergoes an abnormal grain growth upon annealing at 800 °C. At 500 °C, the measured ionic conductivity of this annealed film is higher, by about a half order of magnitude, than those of its poisoned-mode counterparts, which are in turn significantly higher than that of the YSZ bulk by about two orders of magnitude. The abnormally-grown ultra-large grain size of the film deposited in the transition mode and then annealed is believed to be responsible for the former comparison due to the suppression of the grain boundary blocking effect, while the latter comparison can be attributed to the interface effect.

Properties of WZ21 (%wt) alloy processed by a powder metallurgy route.

PubMed

Cabeza, Sandra; Garcés, Gerardo; Pérez, Pablo; Adeva, Paloma

2015-06-01

Microstructure, mechanical properties and corrosion behaviour of WZ21 (%wt) alloy prepared by a powder metallurgy route from rapidly solidified powders have been studied. Results were compared to those of the same alloy prepared through a conventional route of casting and extrusion. The microstructure of the extruded ingot consisted of α-Mg grains and Mg3Zn3Y2 (W-phase) and LPSO-phase particles located at grain boundaries. Moreover, stacking faults were also observed within α-Mg grains. The alloy processed by the powder metallurgy route exhibited a more homogeneous and finer microstructure, with a grain size of 2 μm. In this case W-phase and Mg24Y5 phase were identified, but not the LPSO-phase. The microstructural refinement induced by the use of rapidly solidified powders strengthened the alloy at room temperature and promoted superplasticity at higher strain rates. Corrosion behaviour in PBS medium evidenced certain physical barrier effect of the almost continuous arrangements of second phases aligned along the extrusion direction in conventionally processed WZ21 alloy, with a stable tendency around 7 mm/year. On the other hand, powder metallurgy processing promoted significant pitting corrosion, inducing accelerated corrosion rate during prolonged immersion times. Copyright © 2015 Elsevier Ltd. All rights reserved.

High temperature coarsening of Cr2Nb precipitates in Cu-8 Cr-4 Nb alloy

NASA Technical Reports Server (NTRS)

Anderson, Kenneth Reed

1996-01-01

A new high-temperature-strength, high-conductivity Cu-Cr-Nb alloy with a CrNb ratio of 2:1 was developed to achieve improved performance and durability. The Cu-8 Cr4 Nb alloy studied has demonstrated remarkable thermal and microstructural stability after long exposures at temperatures up to 0.98 T(sub m). This stability was mainly attributed to the slow coarsening kinetics of the Cr2Nb precipitates present in the alloy. At all temperatures, the microstructure consists of a bimodal and sometimes trimodal distribution of strengthening Cr2Nb precipitates, depending on precipitation condition, i.e. from liquid or solid solution, and cooling rates. These precipitates remain in the same size range, i.e. large precipitates of approximately I pm, and small precipitates less dm 300 nm, and effectively pin the grain boundaries thus retaining a fine grain size of 2.7 micro-m after 100 h at 1323 K. (A relatively small number of Cr-rich and Nb-rich particles were also present.) This grain boundary pinning and sluggish coarsening of Cr2Nb particles explain the retention of good mechanical properties after prolonged holding at very high temperatures, e.g., 75% of the original hardness after aging for 100 h at 1273 K. Application of LSW-based coarsening models indicated that the coarsening kinetics of the large precipitates are most likely governed by grain boundary diffsion and, to a lesser extent, volume diffusion mechanisms.

Microstructure control of Al-Cu films for improved electromigration resistance

DOEpatents

Frear, D.R.; Michael, J.R.; Romig, A.D. Jr.

1994-04-05

A process for the forming of Al-Cu conductive thin films with reduced electromigration failures is useful, for example, in the metallization of integrated circuits. An improved formation process includes the heat treatment or annealing of the thin film conductor at a temperature within the range of from 200 C to 300 C for a time period between 10 minutes and 24 hours under a reducing atmosphere such as 15% H[sub 2] in N[sub 2] by volume. Al-Cu thin films annealed in the single phase region of a phase diagram, to temperatures between 200 C and 300 C have [theta]-phase Al[sub 2] Cu precipitates at the grain boundaries continuously become enriched in copper, due, it is theorized, to the formation of a thin coating of [theta]-phase precipitate at the grain boundary. Electromigration behavior of the aluminum is, thus, improved because the [theta]-phase precipitates with copper hinder aluminum diffusion along the grain boundaries. Electromigration, then, occurs mainly within the aluminum grains, a much slower process. 5 figures.

Disintegration of the net-shaped grain-boundary phase by multi-directional forging and its influence on the microstructure and properties of Cu-Ni-Si alloy

NASA Astrophysics Data System (ADS)

Zhang, Jinlong; Lu, Zhenlin; Zhao, Yuntao; Jia, Lei; Xie, Hui; Tao, Shiping

2017-09-01

Cu-Ni-Si alloys with 90% Cu content and Ni to Si ratios of 5:1 were fabricated by fusion casting, and severe plastic deformation of the Cu-Ni-Si alloy was carried out by multi-direction forging (MDF). The results showed that the as-cast and homogenized Cu-Ni-Si alloys consisted of three phases, namely the matrix phase α-Cu (Ni, Si), the reticular grain boundary phase Ni31Si12 and the precipitated phase Ni2Si. MDF significantly destroyed the net-shaped grain boundary phase, the Ni31Si12 phase and refined the grain size of the Cu matrix, and also resulted in the dissolving of Ni2Si precipitates into the Cu matrix. The effect of MDF on the conductivity of the solid solution Cu-Ni-Si alloy was very significant, with an average increase of 165.16%, and the hardness of the Cu-Ni-Si alloy also increased obviously.

Evolution of Grain Interfaces in Annealed Duplex Stainless Steel after Parallel Cross Rolling and Direct Rolling

PubMed Central

Wang, Ming; Li, Haoqing; Tian, Yujing; Guo, Hong; Fang, Xiaoying; Guo, Yuebin

2018-01-01

Changes in various grain interfaces, including the grain boundary and phase boundary, are a strong indication of microstructural changes, particularly ultra-fined grains achieved by large strain deformation and subsequent annealing. After direct rolling and cross rolling with the same strain of ε = 2, the distributions of the interfaces in annealed UNS S32304 duplex stainless steel were investigated using electron backscatter diffraction (EBSD) in this study. The ferrite experienced continued recovery, and a high density of low-angle grain boundaries (LAGBs) was produced. The percentage and number of twin boundaries (TBs) and LAGBs varied within the austenite. TBs were frequently found within austenite, showing a deviation from the Kurdjumov-Sachs (K-S) orientation relationship (OR) with ferrite matrix. However, LAGBs usually occur in austenite, with the K-S OR in the ferrite matrix. LAGBs were prevalent in the precipitated austenite grains, and therefore a strong texture was introduced in the cross-rolled and annealed samples, in which the precipitated austenite readily maintained the K-S OR in the ferrite matrix. By contrast, more TBs and a less robust texture were found in the precipitated austenite in direct-rolled and annealed samples, deviating from the K-S OR. PMID:29772723

EBSD characterization of low temperature deformation mechanisms in modern alloys

NASA Astrophysics Data System (ADS)

Kozmel, Thomas S., II

For structural applications, grain refinement has been shown to enhance mechanical properties such as strength, fatigue resistance, and fracture toughness. Through control of the thermos-mechanical processing parameters, dynamic recrystallization mechanisms were used to produce microstructures consisting of sub-micron grains in 9310 steel, 4140 steel, and Ti-6Al-4V. In both 9310 and 4140 steel, the distribution of carbides throughout the microstructure affected the ability of the material to dynamically recrystallize and determined the size of the dynamically recrystallized grains. Processing the materials at lower temperatures and higher strain rates resulted in finer dynamically recrystallized grains. Microstructural process models that can be used to estimate the resulting microstructure based on the processing parameters were developed for both 9310 and 4140 steel. Heat treatment studies performed on 9310 steel showed that the sub-micron grain size obtained during deformation could not be retained due to the low equilibrium volume fraction of carbides. Commercially available aluminum alloys were investigated to explain their high strain rate deformation behavior. Alloys such as 2139, 2519, 5083, and 7039 exhibit strain softening after an ultimate strength is reached, followed by a rapid degradation of mechanical properties after a critical strain level has been reached. Microstructural analysis showed that the formation of shear bands typically preceded this rapid degradation in properties. Shear band boundary misorientations increased as a function of equivalent strain in all cases. Precipitation behavior was found to greatly influence the microstructural response of the alloys. Additionally, precipitation strengthened alloys were found to exhibit similar flow stress behavior, whereas solid solution strengthened alloys exhibited lower flow stresses but higher ductility during dynamic loading. Schmid factor maps demonstrated that shear band formation behavior was influenced by texturing in these alloys.

Finite element approximation of the fields of bulk and interfacial line defects

NASA Astrophysics Data System (ADS)

Zhang, Chiqun; Acharya, Amit; Puri, Saurabh

2018-05-01

A generalized disclination (g.disclination) theory (Acharya and Fressengeas, 2015) has been recently introduced that goes beyond treating standard translational and rotational Volterra defects in a continuously distributed defects approach; it is capable of treating the kinematics and dynamics of terminating lines of elastic strain and rotation discontinuities. In this work, a numerical method is developed to solve for the stress and distortion fields of g.disclination systems. Problems of small and finite deformation theory are considered. The fields of a single disclination, a single dislocation treated as a disclination dipole, a tilt grain boundary, a misfitting grain boundary with disconnections, a through twin boundary, a terminating twin boundary, a through grain boundary, a star disclination/penta-twin, a disclination loop (with twist and wedge segments), and a plate, a lenticular, and a needle inclusion are approximated. It is demonstrated that while the far-field topological identity of a dislocation of appropriate strength and a disclination-dipole plus a slip dislocation comprising a disconnection are the same, the latter microstructure is energetically favorable. This underscores the complementary importance of all of topology, geometry, and energetics in understanding defect mechanics. It is established that finite element approximations of fields of interfacial and bulk line defects can be achieved in a systematic and routine manner, thus contributing to the study of intricate defect microstructures in the scientific understanding and predictive design of materials. Our work also represents one systematic way of studying the interaction of (g.)disclinations and dislocations as topological defects, a subject of considerable subtlety and conceptual importance (Aharoni et al., 2017; Mermin, 1979).

Additive manufacturing of 316L stainless steel by electron beam melting for nuclear fusion applications

NASA Astrophysics Data System (ADS)

Zhong, Yuan; Rännar, Lars-Erik; Liu, Leifeng; Koptyug, Andrey; Wikman, Stefan; Olsen, Jon; Cui, Daqing; Shen, Zhijian

2017-04-01

A feasibility study was performed to fabricate ITER In-Vessel components by one of the metal additive manufacturing methods, Electron Beam Melting® (EBM®). Solid specimens of SS316L with 99.8% relative density were prepared from gas atomized precursor powder granules. After the EBM® process the phase remains as austenite and the composition has practically not been changed. The RCC-MR code used for nuclear pressure vessels provides guidelines for this study and tensile tests and Charpy-V tests were carried out at 22 °C (RT) and 250 °C (ET). This work provides the first set of mechanical and microstructure data of EBM® SS316L for nuclear fusion applications. The mechanical testing shows that the yield strength, ductility and toughness are well above the acceptance criteria and only the ultimate tensile strength of EBM® SS316L is below the RCC-MR code. Microstructure characterizations reveal the presence of hierarchical structures consisting of solidified melt pools, columnar grains and irregular shaped sub-grains. Lots of precipitates enriched in Cr and Mo are observed at columnar grain boundaries while no sign of element segregation is shown at the sub-grain boundaries. Such a unique microstructure forms during a non-equilibrium process, comprising rapid solidification and a gradient 'annealing' process due to anisotropic thermal flow of accumulated heat inside the powder granule matrix. Relations between process parameters, specimen geometry (total building time) and sub-grain structure are discussed. Defects are formed mainly due to the large layer thickness (100 μm) which generates insufficient bonding between a few of the adjacently formed melt pools during the process. Further studies should focus on adjusting layer thickness to improve the strength of EBM® SS316L and optimizing total building time.

Effects of hot extrusion and heat treatment on microstructure and properties of industrial large-scale spray-deposited 7055 aluminum alloy

NASA Astrophysics Data System (ADS)

Yang, Yonggang; Zhao, Yutao; Kai, Xizhou; Zhang, Zhen; Zhang, Hao; Tao, Ran; Chen, Gang; Yin, Houshang; Wang, Min

2018-01-01

The industrial large-scale 7055 aluminum alloy fabricated by spray forming technology was subjected to hot extrusion and heat treatment to achieve high strength and ductility. Microstructure of the as-deposited alloy indicates that higher density billets with equiaxed grains (20-40 μm) were fabricated rather than a typical dendritic microstructure of the as-cast alloy. The grains of the as-extruded alloy exhibit fibrous morphology, the original boundaries disappear and fined second phases with size about 0.5-5 μm distribute along with extrusion direction. Meanwhile, the defects could be eliminated by hot extrusion, which resulted in good strength as well as ductility. The ultimate tensile strength, yield strength and elongation of the as-extruded alloy are 345 MPa, 236 MPa and 18.5%, respectively. After heat treatment, the partial recrystallization is observed around the un-recrystallized grains and sub-grains. And the platelet/rod-shaped precipitates (MgZn2) show a uniform distribution in the matrix alloy. The alloy reaches the maximum tensile strength of 730 MPa after T6 temper treatment, associated with a fine precipitation (MgZn2). However, with further deepen aging degree (from T6 to T73 temper), the size of dominant precipitated phases (MgZn2) grows obviously, the grain boundary precipitates transform from continuous to individual ones and the width of precipitate free zone increases. The result shows that the alloy after T7X temper treatment exhibits higher electrical conductivity (>35 %IACS) and facture toughness (>25.6 MPa m1/2) although a 8%-17% reduction in strength compared with that at T6 temper.

Prediction of the Grain-Microstructure Evolution Within a Friction Stir Welding (FSW) Joint via the Use of the Monte Carlo Simulation Method

NASA Astrophysics Data System (ADS)

Grujicic, M.; Ramaswami, S.; Snipes, J. S.; Avuthu, V.; Galgalikar, R.; Zhang, Z.

2015-09-01

A thermo-mechanical finite element analysis of the friction stir welding (FSW) process is carried out and the evolution of the material state (e.g., temperature, the extent of plastic deformation, etc.) monitored. Subsequently, the finite-element results are used as input to a Monte-Carlo simulation algorithm in order to predict the evolution of the grain microstructure within different weld zones, during the FSW process and the subsequent cooling of the material within the weld to room temperature. To help delineate different weld zones, (a) temperature and deformation fields during the welding process, and during the subsequent cooling, are monitored; and (b) competition between the grain growth (driven by the reduction in the total grain-boundary surface area) and dynamic-recrystallization grain refinement (driven by the replacement of highly deformed material with an effectively "dislocation-free" material) is simulated. The results obtained clearly revealed that different weld zones form as a result of different outcomes of the competition between the grain growth and grain refinement processes.

Ductile deformation mechanisms of synthetic halite: a full field measurement approach

NASA Astrophysics Data System (ADS)

Dimanov, Alexandre; Bourcier, Mathieu; Héripré, Eva; Bornert, Michel; Raphanel, Jean

2013-04-01

Halite is a commonly used analog polycristalline material. Compared to most rock forming minerals, halite exhibits extensively ductile behavior at even low temperatures and fast deformation rates. Therefore, it allows an easier study of the fundamental mechanisms of crystal plasticity, recrystallization, grain growth and texture development than any other mineral. Its high solubility also makes it an ideal candidate for investigating pressure solution creep. Most importantly, halite is very convenient to study the interactions of simultaneously occurring deformation mechanisms. We investigated uniaxial deformation of pure synthetic NaCl polycrystals with controlled grain sizes and grain size distributions at room and moderate temperatures (400°C). The mechanical tests were combined with "in-situ" optical and scanning electron microscopy, in order to perform 2D digital image correlation (2D-DIC) and to obtain the full surface strain fields at the sample scale and at the scales of the microstructure. We observed dominantly intracrystalline plasticity, as revealed by the occurrence of physical slip lines on the surface of individual grains and of deformation bands at the microstructure (aggregate) scale, as revealed by DIC. Crystal orientation mapping (performed by EBSD) allowed relating the latter to the traces of crystallographic slip planes and inferring the active slip systems considering the macroscopic stress state and computing Schmid factors. The strain heterogeneities are more pronounced at low temperature, at both the aggregate scale and within individual grains. The local activity of slip systems strongly depends on the relative crystallographic and interfacial orientations of the adjacent grains with respect to the loading direction. The easy glide {110} <110> systems are not the only active ones. We could identify the activity of all slip systems, especially near grain boundaries, which indicates local variations of the stress state. But, we also clearly evidenced grain boundary sliding (GBS), which occurred as a secondary but necessary mechanism for accommodation of local strain incompatibilities between neighboring grains, related to the anisotropy of crystal plasticity. The DIC technique allowed the precise quantification of the relative contribution of each mechanism. The latter clearly depends on the microstructure (i.e. grain size and its distribution): the smaller is the grain size and the stronger is the GBS contribution. Finite element modeling of the viscoplastic polycrystalline behavior was started on the basis of our experimental microstructures with large grains (where GBS activity is limited to < 10 %), considering an extruded columnar structure in depth and single crystal flow laws from literature. The results show that the computed strain fields do not sufficiently match the experimentally measured ones. The reasons for the discrepancies are likely related to the activity of GBS, which was not accounted for, and to the influence of the real microstructure at depth (underlying grains and orientations of interfaces), which strongly condition the surface response.

Microstructural-Scale Model for Surfaces Spreading of Intergranular Corrosion in Sensitized Stainless Steels and Aluminum-Magnesium (AA5XXX) Alloys

NASA Astrophysics Data System (ADS)

Jain, Swati

Components from AA5XXX (Al-Mg alloys with more than 3 wt% Mg) alloys are X attractive due to availability of low cost, high strength to weight ratio and good weldability. Therefore, these alloys have potential applications in Naval ships. However, these alloys become susceptible to IGC (intergranular corrosion) due to beta-phase precipitation due to improper heat treatment or inadvertent thermal exposure. Stainless steels may also become susceptible due to carbide precipitation and chromium depletion on grain boundaries. IGC susceptibility depends on the interplay between the metallurgical conditions, electrochemical conditions, and chemical conditions. Specific combinations cause IGC while others do not. The objective of this study is to investigate the conditions which bring about surface spreading of IGC in these alloy classes. To accomplish this goal, a microstructure scale model was developed with experimental inputs to understand the 2-D IGC spreading in stainless steels and AA5XXX alloys. The conditions strongly affecting IGC spreading were elucidated. Upon natural and artificial aging, the stainless steels become susceptible to intergranular corrosion because of chromium depletion in the grain boundaries. After aging Al-Mg (AA5XXX) alloys show susceptibility due to the precipitation of the beta-phase (Al3Mg7) in the grain boundaries. Chromium depleted grain boundaries in stainless steels are anodically more active as compared to the interior of the grains. (3-phase rich grain boundaries have lower OCP (open circuit potential) and pitting potentials as compared to the Al-Mg solid solutions. A new approach to modeling the IGC surface spreading in polycrystalline materials that is presented. This model is the first to couple several factors into one granular scale model that illustrates the way in which they interact and IGC occurs. It sheds new information on conditions which cause IGC spreading in two alloy classes and describes a new theory for the critical potential associated with IGC. The outcomes from this contribute to ways to advance the goal of corrosion resistant computational design of alloys, guiding mitigation strategies for suppressing IGC in existing alloys, and to damage prognosis aimed at predicting damage and structural integrity.

Analysis of microstructure of steel 20 in the range of healing of internal crack

NASA Astrophysics Data System (ADS)

Zhang, Yongjun; Han, Jingtao

2012-03-01

The microstructure and hardness of steel 20 are studied in the range of healing of an artificially created internal crack. In the range of healing of the crack the microstructure is represented primarily by ferrite. The ferrite grains grow through the boundary of the internal crack and contain polyhedral subgrains several hundred nanometers in size. The hardness of the ferrite in the range of healing of the internal crack is higher than in the matrix. A possible cause of this is substructural hardening.

Microstructural Evaluations of Baseline HSR/EPM Disk Alloys

NASA Technical Reports Server (NTRS)

Gabb, Timothy P.; Garg, Anita; Ellis, David L.

2004-01-01

Six alloys representing two classes of powder metallurgy nickel-based superalloys were examined by transmission electron microscopy (TEM) and phase extraction. Alloys KM4, CH98, IN-100 and 456 are based on a Ni-18Co-12Cr composition while alloys Rene' 88 DT and SR 3 have lower Al and Co and higher Cr contents. The lambda size distributions were determined from quantitative image analysis of the TEM images. The volume fraction of lambda and carbides and the composition of the phases were determined by a combination of phase extraction and TEM. The results showed many similarities in lambda size distributions, grain boundary serrations, and grain boundary carbide frequencies between alloys KM4, CH98, 456, Rene' 88 DT and SR 3 when heat treated to give an approximate grain size of ASTM 6. The density of grain boundary carbides in KM4 was shown to substantially increase as the grain size increased. IN-100 and 456 subjected to a serration cooling heat treatment had much more complex lambda size distributions with very large intergranular and intragranular secondary lambda as well as finer than average cooling and aging lambda. The grain boundary carbides in IN-100 were similar to the other alloys, but 456 given the serration cooling heat treatment had a more variable density of grain boundary carbides. Examination of the phases extracted from the matrix showed that there were significant differences in the phase chemistries and elemental partitioning ratios between the various alloys.

Reduction of intergranular exchange coupling and grain size for high Ku CoPt-based granular media: Metal-oxide buffer layer and multiple oxide boundary materials

NASA Astrophysics Data System (ADS)

Tham, Kim Kong; Kushibiki, Ryosuke; Kamada, Tomonari; Hinata, Shintaro; Saito, Shin

2018-05-01

Investigation of magnetic properties and microstructure of granular media with various multiple oxides as the grain boundary material is reported. Saturation magnetization (Ms), uniaxial magnetocrystalline anisotropy (Ku), and magnetic grain diameter (GD) of the granular media show linear correlation with volume weighted average for melting point (Tm) of each oxides (Tmave). Ku of magnetic grains (Kugrain) shows a trade-off relation with GD that it is a big challenge to satisfy both high Kugrain and small GD by only controlling Tmave. To obtain a granular medium with appropriate Kugrain, GD, and low degree of intergranular exchange coupling, the combination of Tmave control of grain boundary material by mixing oxides and employment of a buffer layer are required. Here the degree of intergranular exchange coupling is estimated from the slope of M-H loop at around coercivity (α). By applying this technique, a typical granular medium with Kugrain of 1.0×107 erg/cm3, GD of 5.1 nm, and α of 1.2 is realized.

Continuum and crystal strain gradient plasticity with energetic and dissipative length scales

NASA Astrophysics Data System (ADS)

Faghihi, Danial

This work, standing as an attempt to understand and mathematically model the small scale materials thermal and mechanical responses by the aid of Materials Science fundamentals, Continuum Solid Mechanics, Misro-scale experimental observations, and Numerical methods. Since conventional continuum plasticity and heat transfer theories, based on the local thermodynamic equilibrium, do not account for the microstructural characteristics of materials, they cannot be used to adequately address the observed mechanical and thermal response of the micro-scale metallic structures. Some of these cases, which are considered in this dissertation, include the dependency of thin films strength on the width of the sample and diffusive-ballistic response of temperature in the course of heat transfer. A thermodynamic-based higher order gradient framework is developed in order to characterize the mechanical and thermal behavior of metals in small volume and on the fast transient time. The concept of the thermal activation energy, the dislocations interaction mechanisms, nonlocal energy exchange between energy carriers and phonon-electrons interactions are taken into consideration in proposing the thermodynamic potentials such as Helmholtz free energy and rate of dissipation. The same approach is also adopted to incorporate the effect of the material microstructural interface between two materials (e.g. grain boundary in crystals) into the formulation. The developed grain boundary flow rule accounts for the energy storage at the grain boundary due to the dislocation pile up as well as energy dissipation caused by the dislocation transfer through the grain boundary. Some of the abovementioned responses of small scale metallic compounds are addressed by means of the numerical implementation of the developed framework within the finite element context. In this regard, both displacement and plastic strain fields are independently discretized and the numerical implementation is performed in the finite element program ABAQUS/standard via the user element subroutine UEL. Using this numerical capability, an extensive study is conducted on the major characteristics of the proposed theories for bulk and interface such as size effect on yield and kinematic hardening, features of boundary layer formation, thermal softening and grain boundary weakening, and the effect of soft and stiff interfaces.

Effect of He implantation on fracture behavior and microstructural evolution in F82H

NASA Astrophysics Data System (ADS)

Yabuuchi, Kiyohiro; Sato, Kiminori; Nogami, Shuhei; Hasegawa, Akira; Ando, Masami; Tanigawa, Hiroyasu

2014-12-01

Reduced-activation ferritic/martensitic steels (RAFMs) are the primary candidate structural materials for fusion reactor blanket components. He bubbles, which formed under 14 MeV neutron irradiation, is considered to cause some mechanical property changes. In a previous study, Hasegawa et al. investigated the fracture behavior using Charpy impact test of He implanted F82H by 50 MeV α-particles with cyclotron accelerator, and the ductile brittle transition temperature (DBTT) was increased and intergranular fracture (IGF) was observed. However, the cause of the IGF was not shown in the previous study. To clarify the cause of the IGF of the He implanted F82H by 50 MeV α-particles with cyclotron accelerator, the microstructure of the He implanted F82H was investigated. After Charpy impact test at 233 K, the brittle fracture surface of the He implanted specimen was observed by SEM and TEM. By SEM observation, grain boundary surface was clearly observed from the bottom of the notch to a depth of about 400 μm. This area correspond to the He implanted region. On the other hand, at unimplanted region, river pattern was observed and transgranular fracture occurred. TEM observation revealed the He bubbles agglomeration at dislocations, lath boundaries, and grain boundaries, and the coarsening of precipitates on grain boundaries. IGF of the He implanted F82H was caused by both He bubbles and coarsening precipitates.

Effects of long time exposures in Rene-41

DOE Office of Scientific and Technical Information (OSTI.GOV)

Radavich, J.F.

1995-12-31

A microstructural study was carried out on Rene-41 samples to determine the cause(s) of embrittlement developed after longtime engine exposures. The structural changes in Rene-41 samples exposed 12,000 to 15,000 hours as part of a thermal shield were compared to new material and re-heat treated exposed material. Selective metallographic, SEM, EDS and x-ray diffraction techniques showed that in long exposures the {gamma} phase coarsens, a Mu phase forms, and a continuous Cr rich carbide forms at the grain boundaries. The continuous grain boundary carbide is the main cause for the embrittlement. Exposed material that is given the standard Rene-41 heatmore » treatment becomes ductile as the grain boundary carbide is solutioned. Samples of exposed brittle material that initially shows a brittle intergranular fracture exhibit a ductile transgranular mode after re-heat treatment. Results of the various characterization techniques will be presented.« less

The analysis of critical cooling rate for high-rise building steel S460

NASA Astrophysics Data System (ADS)

Lu, Shiping; Chen, Xia; Li, Qun; Wang, Haibao; Gu, Linhao

2017-09-01

High-rise building steel S460 is an important structure steel.The product process of the steel is Quenching&Tempering. The critical cooling rate of steel is very important in heavy plate quenching process, and it is also the basis of the cooling process[1].The critical cooling rate of HSLA steel S460 is obtained from the Thermal simulation method,and the differences about the microstructure and properties of different cooling rate is also analyzed.In this article, the angle of the grain boundary and the average grain size are analyzed by EBSD under different cooling rate. The relationship between grain boundary angle and grain size with the cooling rate is obtained. According to the experiment,it provides the basis for the formulation of the quenching process of the industrial production.

The Microstructure Evolution and Deformation Behavior of AZ80 During Gradient Increment Cyclic Loading

NASA Astrophysics Data System (ADS)

Ren, Lingbao; Quan, Gaofeng; Boehlert, Carl J.; Zhou, Mingyang; Guo, Yangyang; Fan, Lingling

2018-06-01

Cyclic loading-unloading uniaxial tension experiments were conducted at temperatures ranging between 293 K and 623 K and a strain rate of 10-3 s-1 to study the cyclic accumulated plastic deformation (CAP) behavior of extruded AZ80. The 673 K/4-h heat treatment to the as-extruded AZ80 led to a noticeable decrease in yield strength which was associated with both dissolution of the β-Mg17Al12 phase and growth of the matrix grain size. The critical number of cycles needed to soften the material (N c) decreased from 5 to 4 when the cyclic strain amplitude (ɛ a) increased from 3.3 to 5.0 pct for the as-extruded AZ80. The average cyclic hardening rate (Θ) increased from 11 to 23 MPa/cycle after heat treatment, and this was attributed to the more pronounced twinning process in the coarse-grained microstructure. During the 293 K to 473 K CAP deformation, the increasing accumulated cyclic tension strain may have accelerated the propagation of secondary twinning leading to the Lüders-like post-yield softening. Twinning was prevalent at low temperature (293 K to 473 K) in the ɛ a = 3.0 pct CAP deformation for the heat-treated alloy, and twin-assisted precipitation occurred during the 523 K CAP deformation, which implied that the high diffusivity in the twin boundary accelerated the heterogeneous nucleation of precipitates. The preferred cracking locations changed from twin boundaries to grain boundaries when the CAP deformation temperature increased from 473 K to 523 K. As for the 623 K CAP deformation, cavities initiated at the grain boundaries, and the volume fraction of the cracks/cavities increased from 0.01 to 0.05 with increasing temperature.

Investigation on the Microstructure and Ductility-Dip Cracking Susceptibility of the Butt Weld Welded with ENiCrFe-7 Nickel-Base Alloy-Covered Electrodes

NASA Astrophysics Data System (ADS)

Qin, Renyao; Wang, Huang; He, Guo

2015-03-01

The weld metal of the ENiCrFe-7 nickel-based alloy-covered electrodes was investigated in terms of the microstructure, the grain boundary precipitation, and the ductility-dip cracking (DDC) susceptibility. Besides the dendritic gamma-Ni(Cr,Fe) phase, several types of precipitates dispersed on the austenitic matrix were observed, which were determined to be the Nb-rich MC-type carbides with "Chinese script" morphology and size of approximately 3 to 10 µm, the Mn-rich MO-type oxides with size of approximately 1 to 2 µm, and the spherical Al/Ti-rich oxides with size of less than 1 µm. The discontinuous Cr-rich M23C6-type carbides predominantly precipitate on the grain boundaries, which tend to coarsen during reheating but begin to dissolve above approximately 1273 K (1000 °C). The threshold strain for DDC at each temperature tested shows a certain degree of correlation with the grain boundary carbides. The DDC susceptibility increases sharply as the carbides coarsen in the temperature range of 973 K to 1223 K (700 °C to 950 °C). The growth and dissolution of the carbides during the welding heat cycles deteriorate the grain boundaries and increase the DDC susceptibility. The weld metal exhibits the minimum threshold strain of approximately 2.0 pct at 1323 K (1050 °C) and the DTR less than 873 K (600 °C), suggesting that the ENiCrFe-7—covered electrode has less DDC susceptibility than the ERNiCrFe-7 bare electrode but is comparable with the ERNiCrFe-7A.

Microstructure Evolution and Composition Control during the Processing of Thin-gage Metallic Foil (Preprint)

DTIC Science & Technology

2012-02-01

the presence of somewhat randomly-distributed carbides and borides (white particles in BSE images), this grain size was comparable to that observed...pinned by carbide/ boride particles (imaging white in Figure 8c). The very fine gamma-prime precipitates likely produced during magnetron sputtering...sputtered material. First, the carbide/ boride particles were nucleated and hence located preferentially at the grain boundaries in the sputtered

Evidences of grain boundary capacitance effect on the colossal dielectric permittivity in (Nb + In) co-doped TiO2 ceramics

PubMed Central

Li, Jinglei; Li, Fei; Li, Chao; Yang, Guang; Xu, Zhuo; Zhang, Shujun

2015-01-01

The (Nb + In) co-doped TiO2 ceramics were synthesized by conventional solid-state sintering (CSSS) and spark plasma sintering (SPS) methods. The phases and microstructures were studied by X-ray diffraction, Raman spectra, field-emission scanning electron microscopy and transmission electron microscopy, indicating that both samples were in pure rutile phase while showing significant difference in grain size. The dielectric and I–V behaviors of SPS and CSSS samples were investigated. Though both possess colossal permittivity (CP), the SPS samples exhibited much higher dielectric permittivity/loss factor and lower breakdown electric field when compared to their CSSS counterparts. To further explore the origin of CP in co-doped TiO2 ceramics, the I–V behavior was studied on single grain and grain boundary in CSSS sample. The nearly ohmic I–V behavior was observed in single grain, while GBs showed nonlinear behavior and much higher resistance. The higher dielectric permittivity and lower breakdown electric field in SPS samples, thus, were thought to be associated with the feature of SPS, by which reduced space charges and/or impurity segregation can be achieved at grain boundaries. The present results support that the grain boundary capacitance effect plays an important role in the CP and nonlinear I–V behavior of (Nb + In) co-doped TiO2 ceramics. PMID:25656713

Evidences of grain boundary capacitance effect on the colossal dielectric permittivity in (Nb + In) co-doped TiO2 ceramics

NASA Astrophysics Data System (ADS)

Li, Jinglei; Li, Fei; Li, Chao; Yang, Guang; Xu, Zhuo; Zhang, Shujun

2015-02-01

The (Nb + In) co-doped TiO2 ceramics were synthesized by conventional solid-state sintering (CSSS) and spark plasma sintering (SPS) methods. The phases and microstructures were studied by X-ray diffraction, Raman spectra, field-emission scanning electron microscopy and transmission electron microscopy, indicating that both samples were in pure rutile phase while showing significant difference in grain size. The dielectric and I-V behaviors of SPS and CSSS samples were investigated. Though both possess colossal permittivity (CP), the SPS samples exhibited much higher dielectric permittivity/loss factor and lower breakdown electric field when compared to their CSSS counterparts. To further explore the origin of CP in co-doped TiO2 ceramics, the I-V behavior was studied on single grain and grain boundary in CSSS sample. The nearly ohmic I-V behavior was observed in single grain, while GBs showed nonlinear behavior and much higher resistance. The higher dielectric permittivity and lower breakdown electric field in SPS samples, thus, were thought to be associated with the feature of SPS, by which reduced space charges and/or impurity segregation can be achieved at grain boundaries. The present results support that the grain boundary capacitance effect plays an important role in the CP and nonlinear I-V behavior of (Nb + In) co-doped TiO2 ceramics.

Evidences of grain boundary capacitance effect on the colossal dielectric permittivity in (Nb + In) co-doped TiO2 ceramics.

PubMed

Li, Jinglei; Li, Fei; Li, Chao; Yang, Guang; Xu, Zhuo; Zhang, Shujun

2015-02-06

The (Nb + In) co-doped TiO2 ceramics were synthesized by conventional solid-state sintering (CSSS) and spark plasma sintering (SPS) methods. The phases and microstructures were studied by X-ray diffraction, Raman spectra, field-emission scanning electron microscopy and transmission electron microscopy, indicating that both samples were in pure rutile phase while showing significant difference in grain size. The dielectric and I-V behaviors of SPS and CSSS samples were investigated. Though both possess colossal permittivity (CP), the SPS samples exhibited much higher dielectric permittivity/loss factor and lower breakdown electric field when compared to their CSSS counterparts. To further explore the origin of CP in co-doped TiO2 ceramics, the I-V behavior was studied on single grain and grain boundary in CSSS sample. The nearly ohmic I-V behavior was observed in single grain, while GBs showed nonlinear behavior and much higher resistance. The higher dielectric permittivity and lower breakdown electric field in SPS samples, thus, were thought to be associated with the feature of SPS, by which reduced space charges and/or impurity segregation can be achieved at grain boundaries. The present results support that the grain boundary capacitance effect plays an important role in the CP and nonlinear I-V behavior of (Nb + In) co-doped TiO2 ceramics.

Development of Weld Metal Microstructures in Pulsed Laser Welding of Duplex Stainless Steel

NASA Astrophysics Data System (ADS)

Mirakhorli, F.; Malek Ghaini, F.; Torkamany, M. J.

2012-10-01

The microstructure of the weld metal of a duplex stainless steel made with Nd:YAG pulsed laser is investigated at different travel speeds and pulse frequencies. In terms of the solidification pattern, the weld microstructure is shown to be composed of two distinct zones. The presence of two competing heat transfer channels to the relatively cooler base metal and the relatively hotter previous weld spot is proposed to develop two zones. At high overlapping factors, an array of continuous axial grains at the weld centerline is formed. At low overlapping factors, in the zone of higher cooling rate, a higher percentage of ferrite is transformed to austenite. This is shown to be because with extreme cooling rates involved in pulsed laser welding with low overlapping, the ferrite-to-austenite transformation can be limited only to the grain boundaries.

Micro-structure and Mechanical Properties of Nano-TiC Reinforced Inconel 625 Deposited using LAAM

NASA Astrophysics Data System (ADS)

Bi, G.; Sun, C. N.; Nai, M. L.; Wei, J.

In this paper, deposition of Ni-base Inconel 625 mixed with nano-TiC powders using laser aided additive manufacturing (LAAM) was studied. Micro-structure and mechanical properties were intensively investigated. The results showed that nano-size TiC distributed uniformly throughout the Ni- matrix. Inconel 625 can be reinforced by the strengthened grain boundaries with nano-size TiC. Improved micro-hardness and tensile properties were observed.

Effect of Friction Stir Processing on Microstructure and Mechanical Properties of AZ91C Magnesium Cast Alloy Weld Zone

NASA Astrophysics Data System (ADS)

Hassani, Behzad; Karimzadeh, Fathallah; Enayati, Mohammad Hossein; Sabooni, Soheil; Vallant, Rudolf

2016-07-01

In this study, friction stir processing (FSP) was applied to the GTAW (TIG)-welded AZ91C cast alloy to refine the microstructure and optimize the mechanical properties of the weld zone. Microstructural investigation of the samples was performed by optical microscopy and the phases in the microstructure were determined by x-ray diffraction (XRD). The microstructural evaluations showed that FSP destroys the coarse dendritic microstructure. Furthermore, it dissolves the secondary hard and brittle β-Mg17Al12 phase existing at grain boundaries of the TIG weld zone. The closure and decrease in amount of porosities along with the elimination of the cracks in the microstructure were observed. These changes were followed by a significant grain refinement to an average value of 11 µm. The results showed that the hardness values increased to the mean ones, respectively, for as-cast (63 Hv), TIG weld zone (67 Hv), and stir zone (79 Hv). The yield and ultimate strength were significantly enhanced after FSP. The fractography evaluations, by scanning electron microscopy (SEM), indicated to a transition from brittle to ductile fracture surface after applying FSP to the TIG weld zone.

Effect of Strain Rate on Hot Ductility Behavior of a High Nitrogen Cr-Mn Austenitic Steel

NASA Astrophysics Data System (ADS)

Wang, Zhenhua; Meng, Qing; Qu, Minggui; Zhou, Zean; Wang, Bo; Fu, Wantang

2016-03-01

18Mn18Cr0.6N steel specimens were tensile tested between 1173 K and 1473 K (900 °C and 1200 °C) at 9 strain rates ranging from 0.001 to 10 s-1. The tensile strained microstructures were analyzed through electron backscatter diffraction analysis. The strain rate was found to affect hot ductility by influencing the strain distribution, the extent of dynamic recrystallization and the resulting grain size, and dynamic recovery. The crack nucleation sites were primarily located at grain boundaries and were not influenced by the strain rate. At 1473 K (1200 °C), a higher strain rate was beneficial for grain refinement and preventing hot cracking; however, dynamic recovery appreciably occurred at 0.001 s-1 and induced transgranular crack propagation. At 1373 K (1100 °C), a high extent of dynamic recrystallization and fine new grains at medium strain rates led to good hot ductility. The strain gradient from the interior of the grain to the grain boundary increased with decreasing strain rate at 1173 K and 1273 K (900 °C and 1000 °C), which promoted hot cracking. Grain boundary sliding accompanied grain rotation and did not contribute to hot cracking.

Stress evolution and associated microstructure during transient creep of olivine at 1000-1200 °C

NASA Astrophysics Data System (ADS)

Thieme, M.; Demouchy, S.; Mainprice, D.; Barou, F.; Cordier, P.

2018-05-01

We study the mechanical response and correlated microstructure of axial deformed fine-grained olivine aggregates as a function of incremental finite strains. Deformation experiments were conducted in uniaxial compression in an internally heated gas-medium deformation apparatus at temperatures of 1000 and 1200 °C, at strain rates of 10-6 s-1 to 10-5 s-1 and at confining pressure of 300 MPa. Sample volumes are around 1.2 cm3. Finite strains range from 0.1 to 8.6% and corresponding maximal (final) differential stresses range from 80 to 1073 MPa for deformation at 1000 °C and from 71 to 322 MPa for deformation at 1200 °C. At 1200 °C, samples approach steady state deformation after about 8% of strain. At 1000 °C, significant strain hardening leads to stresses exceeding the confining pressure by a factor of 3.5 with brittle deformation after 3% of strain. Deformed samples were characterized by electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). EBSD maps with step sizes as low as 50 nm were acquired without introducing analytical artifacts for the first time. The grain size of deformed samples ranges from 2.1 to 2.6 μm. Despite clear strain hardening, texture or microstructure do not change as a function of stress or finite strain. This observation is supported by a constant texture strength (J-index) and symmetry (BA-index), constant grain shape and aspect ratio, constant density of geometrically necessary dislocations, grain orientation spread, and constant subgrain boundary spacing and misorientation in between samples. TEM shows that all samples exhibit unambiguous dislocation activity but with a highly heterogeneous dislocation distribution. Olivine grains display evidence of [1 0 0] and [0 0 1] slip activity, but there is no evidence of interaction between the dislocations from the different slip systems. Several observations of grain boundaries acting as dislocation sources have been found. We find no confirmation of increasing dislocation densities as the cause for strain hardening during transient creep. This suggests other, yet not fully understood mechanisms affecting the strength of deformed olivine. These mechanisms could possibly involve grain boundaries. Such mechanisms are relevant for the deformation of uppermost mantle rocks, where the Si diffusion rate is too slow and dislocation glide must be accommodated in another way to fulfill the von Mises criterion.

Effect of heat input on microstructure and properties of hybrid fiber laser-arc weld joints of the 800 MPa hot-rolled Nb-Ti-Mo microalloyed steels

NASA Astrophysics Data System (ADS)

Wang, X.-N.; Zhang, S.-H.; Zhou, J.; Zhang, M.; Chen, C.-J.; Misra, R. D. K.

2017-04-01

Hybrid fiber laser-arc welding (HLAW) process was applied to a novel hot-rolled Nb-Ti-Mo microalloyed steels of 8 mm thickness. The steel is primarily used to manufacture automotive and construction machinery components, etc. To elucidate the effect of heat input on geometry, microstructure and mechanical properties, different heat inputs (3.90, 5.20 and 7.75 kJ/cm) were used by changing the welding speeds. With increased heat input, the depth/width of penetration was decreased, and the geometry of fusion zone (FZ) changed to "wine cup-like" shape. In regard to the microstructural constituents, the martensite content was decreased, but granular bainite (GB) content was increased. The main microstructural difference was in the FZ cross-section at 7.75 kJ/cm because of the effect of thermal source on the top and bottom. The microstructure of the top part consisted of GB, grain boundary ferrite, and acicular ferrite, while the bottom part was primarily lath martensite. The hardness distribution was similar for different heat inputs. Hardness in FZ, coarse-grained HAZ and mixed-grained HAZ was higher than the base metal (BM), but for the fine-grained HAZ was similar or marginally less than the base metal (BM). Tensile strain was concentrated in the BM such that the fracture occurred in this region. In summary, the geometry, microstructure, and mechanical properties of weld joints were superior at heat input of 5.20 kJ/cm.

High-temperature studies of grain boundaries in ultrafine grained alloys by means of positron lifetime

NASA Astrophysics Data System (ADS)

Würschum, R.; Shapiro, E.; Dittmar, R.; Schaefer, H.-E.

2000-11-01

Atomic free volumes and vacancies in the ultrafine grained alloys Pd84Zr16, Cu 0.1 wt % ZrO2, and Fe91Zr9 were studied by means of positron lifetime. The thermally stable microstructures serve as a novel type of model system for studying positron trapping and annihilation as well as the thermal behavior of vacancy-sized free volumes over a wide temperature range up to ca. 1200 K by making use of a metallic 58Co positron source. In ultrafine grained Cu the thermal formation of lattice vacancies could be observed. In Pd84Zr16 an increase of the specific positron trapping rate of nanovoids and, in addition, detrapping of positrons from free volumes with a mean size slightly smaller than one missing atom in the grain boundaries contributes to a reversible increase of the positron lifetime of more than 60 ps with measuring temperature. In Fe91Zr9 similar linear high-temperature increases of the positron lifetime are observed in the nanocrystalline and the amorphous state. The question of thermal vacancy formation in grain boundaries is addressed taking into account the different types of interface structures of the present alloys.

Multi-scale characterization by FIB-SEM/TEM/3DAP.

PubMed

Ohkubo, T; Sepehri-Amin, H; Sasaki, T T; Hono, K

2014-11-01

In order to improve properties of functional materials, it is important to understand the relation between the structure and the properties since the structure has large effect to the properties. This can be done by using multi-scale microstructure analysis from macro-scale to nano and atomic scale. Scanning electron microscope (SEM) equipped with focused ion beam (FIB), transmission electron microscope (TEM) and 3D atom probe (3DAP) are complementary analysis tools making it possible to know the structure and the chemistry from micron to atomic resolution. SEM gives us overall microstructural and chemical information by various kinds of detectors such as secondary electron, backscattered electron, EDS and EBSD detectors. Also, it is possible to analyze 3D structure and chemistry via FIB serial sectioning. In addition, using TEM we can focus on desired region to get more complementary information from HRTEM/STEM/Lorentz images, SAED/NBD patterns and EDS/EELS to see the detail micro or nano-structure and chemistry. Especially, combination of probe Cs corrector and split EDS detectors with large detector size enable us to analyze the atomic scale elemental distribution. Furthermore, if the specimen has a complicated 3D nanostructure, or we need to analyze light elements such as hydrogen, lithium or boron, 3DAP can be used as the only technique which can visualize and analyze distribution of all constituent atoms of our materials within a few hundreds nm area. Hence, site-specific sample preparation using FIB/SEM is necessary to get desired information from region of interest. Therefore, this complementary analysis combination works very well to understand the detail of materials.In this presentation, we will show the analysis results obtained from some of functional materials by Carl Zeiss CrossBeam 1540EsB FIB/SEM, FEI Tecnai G(2) F30, Titan G2 80-200 TEMs and locally build laser assisted 3DAP. As the one of the example, result of multi-scale characterization for ultra-fine grain Nd-Fe-B permanent magnet will be shown [1]. In order to improve the magnetic properties, especially to increase the coercivity (resistance against magnetization reversal) of the magnet, decreasing the grain size and isolating each grain by non-ferromagnetic grain boundary phase are quite important since the nucleation of magnetic reversal from grain boundary phase can be suppressed and pinning force of magnetic domain wall at the grain boundary phase can be strengthened. Therefore, micro and nano structure and chemistry analysis can shed a light do grain boundary engineering.Figure 1(a,b) shows SEM BSE images of ultrafine grain Nd-Fe-B sintered magnet and the reconstructed 3D tomography of Nd-rich phases obtained by FIB/SEM serial sectioning. This data can provide us information about the distribution of Nd-rich phase and its volume fraction. Moreover, the HRTEM image from the grain boundary phase, the 3DAP maps and the concentration depth profiles are shown in Fig. 1(c,d,e). This magnet shows high coercivity (1517kA/m), and by comparing these results with the microstructures of low coercivity specimen, importance of grain boundary formation was confirmed and it gives us hint to improve the coercivity further. We will show the detail and results from other materials.jmicro;63/suppl_1/i6/DFU046F1F1DFU046F1Fig. 1.(a) SEM BSE images of ultrafine grain Nd-Fe-B sintered magnet. (b) 3D FIB/SEM tomography of Nd-rich phases. (c) HRTEM image from the grain boundary phase. (d) 3DAP maps of Nd, Cu and Al. (e) Concentration depth profiles for Fe, Nd+Pr, B, Co, Cu and Al, determined from the selected box in (d)[1]. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Deformation of the lithosphere and what microstructures can tell us about it (Stephan Mueller Medal Lecture)

NASA Astrophysics Data System (ADS)

Heilbronner, Renée

2016-04-01

The lithosphere is a roughly stratified and heterogeneous rock body that constitutes the outer layer of our planet. It is subdivided into irregularly shaped stiff plates that move with respect to one another deforming each other along their margins. At the large scale the lithosphere is usually modeled as a flat-lying multi-layer, its rheological profile being based on flow laws determined experimentally for key minerals of the crust and upper mantle. At the somewhat smaller scale of field observations, geometrical and physical complexities become apparent: rocks are folded, sheared and fractured, and - in general - quite heterogeneously deformed. And finally, at the even smaller scale of mechanical testing and microscopic investigations, rocks are seen as polycrystalline aggregates or granular composites whose bulk properties depends both on the composition and shape of the individual grains and the spatial arrangement of the crystals with respect to one another. In other words, the physical properties of the lithosphere and the inferred style or type of deformation depend very much on the scale of observation. Microstructures and textures (crystallographic preferred orientations) of deformed rocks provide a wealth of information: when used as archives of the deformation history, they allow us to unravel the tectonic evolution of the lithosphere at plate boundaries. At the same time, they enable us to assess past and/or present geophysical properties. By comparing the microstructures of experimentally and naturally deformed rocks it is possible to infer the active deformation mechanisms and thus to extrapolate flow laws to geological time scales. With the advent of digital image processing, microstructure and texture analysis have taken a great leap forward. By amalgamating methods from neighbouring disciplines such as mathematical morphometry, stereology, geostatistics, material sciences, etc., microstructure and texture analysis have come a long way since the early days of strain analysis and X-ray texture goniometry. During my lecture, I will try to retrace this development: we will start by taking a dive down to the nano-scale, deep into the ductile regime, and inspect the shape, alignments and preferred orientations of sub-grain boundaries during simple shear deformation. What can the microstructure tell us about the deformation mechanism and the amount of strain that the rock material has undergone, and is it really 'strain' we are looking at? We will also look at orientation images and track the development in space and time of crystallographic orientations with temperature, strain rate and strain: do we reach a 'steady state'? We will then come up in scale and look at various definitions of grain size and test the validity of piezometers: how precise is the flow stress that we determine, does it really only depend on grain size, and what do we mean by 'grains size'? Back at the surface, we will look at brittle microstructures and consider distributions: fractal distributions of grain size and spatial distributions of grains: how can we get a handle on the microstructures of cataclastic deformation or granular flow? - At each step, I hope that it becomes apparent that there is more to microstructure and texture than the aspect ratio of an ellipse, the diameter of a grain, or the maximum of a c-axis pole figure...

Thermal Stabilization and Mechanical Properties of Nanocrystalline Iron-Nickel-Zirconium Alloys

NASA Astrophysics Data System (ADS)

Kotan, Hasan

Ultrafine grained and nanostructured materials are promising for structural applications because of the high strength compared to coarse grained counterparts. However, their widespread application is limited by an inherently high driving force for thermally induced grain growth, even at low temperatures. Accordingly, the understanding of and control over grain growth in nanoscale materials is of great technological and scientific importance as many physical properties (i.e. mechanical properties) are functions of the average grain size and the grain size distribution within the microstructure. Here, we investigate the microstructural evolution and grain growth in Fe-Ni alloys with Zr addition and differentiate the stabilization mechanisms acting on grain boundaries. Fe-Ni alloys are chosen for stability investigations since they are important for understanding the behavior of many steels and other ferrous alloys. Zirconium is proven to be an effective grain size stabilizer in pure Fe and Fe-base systems. In this study, nanocrystalline alloys were prepared by high energy ball milling. In situ and ex situ experiments were utilized to directly follow grain growth and microstructural evolution as a function of temperature and composition. The information obtained from these experiments enables the real time observation of microstructural evolution and phase transformation and provides a unique view of dynamic reactions as they occur. The knowledge of the thermal stability will exploit the potential high temperature applications and the consolidation conditions (i.e. temperature and pressure) to obtain high dense materials for advanced mechanical tests. Our investigations reveal that the grain growth of Fe-Ni alloys is not affected by Ni content but strongly inhibited by the addition of 1 at% Zr up to about 700 °C. The microstructural stability is lost due to the bcc-to-fcc transformation (occurring at 700°C) by the sudden appearance of abnormally grown fcc grains. However it was determined grain growth can be suppressed kinetically at higher temperatures for high Zr containing alloys by precipitation of intermetallic compounds. Eventually at high enough temperatures the retention of nanocrystallinity was lost, leaving behind fine micron grains filled with nanoscale intermetallic precipitates. Despite the loss of stability the in-situ formed precipitates were found to induce an Orowan hardening affect. The results from the mechanical tests show that Orowan particle strengthening can be as significant as Hall Petch hardening is at the smallest grain sizes.

Microstructure and Property Modifications of Cold Rolled IF Steel by Local Laser Annealing

NASA Astrophysics Data System (ADS)

Hallberg, Håkan; Adamski, Frédéric; Baïz, Sarah; Castelnau, Olivier

2017-10-01

Laser annealing experiments are performed on cold rolled IF steel whereby highly localized microstructure and property modification are achieved. The microstructure is seen to develop by strongly heterogeneous recrystallization to provide steep gradients, across the submillimeter scale, of grain size and crystallographic texture. Hardness mapping by microindentation is used to reveal the corresponding gradients in macroscopic properties. A 2D level set model of the microstructure development is established as a tool to further optimize the method and to investigate, for example, the development of grain size variations due to the strong and transient thermal gradient. Particular focus is given to the evolution of the beneficial γ-fiber texture during laser annealing. The simulations indicate that the influence of selective growth based on anisotropic grain boundary properties only has a minor effect on texture evolution compared to heterogeneous stored energy, temperature variations, and nucleation conditions. It is also shown that although the α-fiber has an initial frequency advantage, the higher probability of γ-nucleation, in combination with a higher stored energy driving force in this fiber, promotes a stronger presence of the γ-fiber as also observed in experiments.

Thermal conductivity in Bi0.5Sb1.5Te3+x and the role of dense dislocation arrays at grain boundaries.

PubMed

Deng, Rigui; Su, Xianli; Zheng, Zheng; Liu, Wei; Yan, Yonggao; Zhang, Qingjie; Dravid, Vinayak P; Uher, Ctirad; Kanatzidis, Mercouri G; Tang, Xinfeng

2018-06-01

Several prominent mechanisms for reduction in thermal conductivity have been shown in recent years to improve the figure of merit for thermoelectric materials. Such a mechanism is a hierarchical all-length-scale architecturing that recognizes the role of all microstructure elements, from atomic to nano to microscales, in reducing (lattice) thermal conductivity. In this context, there have been recent claims of remarkably low (lattice) thermal conductivity in Bi 0.5 Sb 1.5 Te 3 that are attributed to seemingly ordinary grain boundary dislocation networks. These high densities of dislocation networks in Bi 0.5 Sb 1.5 Te 3 were generated via unconventional materials processing with excess Te (which formed liquid phase, thereby facilitating sintering), followed by spark plasma sintering under pressure to squeeze out the liquid. We reproduced a practically identical microstructure, following practically identical processing strategies, but with noticeably different (higher) thermal conductivity than that claimed before. We show that the resultant microstructure is anisotropic, with notable difference of thermal and charge transport properties across and along two orthonormal directions, analogous to anisotropic crystals. Thus, we believe that grain boundary dislocation networks are not the primary cause of enhanced ZT through reduction in thermal conductivity. Instead, we can reproduce the purported high ZT through a favorable but impractical and incorrect combination of thermal conductivity measured along the pressing direction of anisotropy while charge transport measured in the direction perpendicular to the anisotropic direction. We believe that our work underscores the need for consistency in charge and thermal transport measurements for unified and verifiable measurements of thermoelectric (and related) properties and phenomena.

Activity of slip in amphibolite facies, fine-grained recrystallized quartz aggregates: high differential stress during high-T creep of quartz?

NASA Astrophysics Data System (ADS)

Viegas, G.; Menegon, L. M.; Archanjo, C. J.

2016-12-01

Quartz axis fabrics are a valuable tool to investigate strain partitioning/distribution in both naturally- and experimentally deformed quartz. Previous works have shown that slip dominates at high temperatures (> 600º C) and water-rich, commonly sub-magmatic conditions, typically associated with large grain sizes and grain boundary migration microstructures. In the Pernambuco shear zone, sheared quartz veins from a protomylonitic granitoid formed during the main amphibolite facies event constrained at mid-crustal conditions (550-600ºC, 5 kbar). The veins contain heterogeneously-deformed primary quartz grains, which typically form both flattened and elongated ribbons as well as more equant porphyroclasts surrounded by aggregates of fine-grained (ca. 20 µm) recrystallized aggregates. Recrystallized quartz with the same fine grain size may also occur in intracrystalline bands within the porphyroclasts. Chessboard extinction is widely observed in the porphyroclasts, and subgrain boundaries are either parallel or normal to the (0001) direction, suggesting slip on both basal and prismatic planes during recrystallization. Crystallographic preferred orientations (CPOs) of porphyroclasts (≥ 100 µm) show maxima of (0001) axes subparallel to Z and X, suggesting coeval glide along both basal and prism planes during shearing. In the recrystallized aggregates, fabric strength tends to become weaker, but still records glide along and directions. These preliminary results suggest that naturally deformed quartz veins record coeval activity of and slip during dynamic recrystallization under amphibolite facies conditions. The microstructure suggests that the CPO of the fine-grained aggregates is host-controlled and results from dominant subgrain rotation recrystallization. To our knowledge, activity of slip in fine-grained recrystallized aggregates has never been reported before. Thus, these preliminary results call into question the general view that slip is expected to be active only during dominant high-T grain boundary migration in the lower crust. In our samples, a fine grain size of dynamically recrystallized quartz associated with slip might indicate high differential stress/strain rates during high-T viscous creep along the Pernambuco shear zone.

Microstructure, strengthening mechanisms and hot deformation behavior of an oxide-dispersion strengthened UFG Al6063 alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Asgharzadeh, H.; Kim, H.S.; Simchi, A., E-mail: simchi@sharif.edu

2013-01-15

An ultrafine-grained Al6063/Al{sub 2}O{sub 3} (0.8 vol.%, 25 nm) nanocomposite was prepared via powder metallurgy route through reactive mechanical alloying and hot powder extrusion. Scanning electron microcopy, transmission electron microscopy, and back scattered electron diffraction analysis showed that the grain structure of the nanocomposite is trimodal and composed of nano-size grains (< 0.1 {mu}m), ultrafine grains (0.1-1 {mu}m), and micron-size grains (> 1 {mu}m) with random orientations. Evaluation of the mechanical properties of the nanocomposite based on the strengthening-mechanism models revealed that the yield strength of the ultrafine-grained nanocomposite is mainly controlled by the high-angle grain boundaries rather than nanometricmore » alumina particles. Hot deformation behavior of the material at different temperatures and strain rates was studied by compression test and compared to coarse-grained Al6063 alloy. The activation energy of the hot deformation process for the nanocomposite was determined to be 291 kJ mol{sup -1}, which is about 64% higher than that of the coarse-grained alloy. Detailed microstructural analysis revealed that dynamic recrystallization is responsible for the observed deformation softening in the ultrafine-grained nanocomposite. - Highlights: Black-Right-Pointing-Pointer The strengthening mechanisms of Al6063/Al{sub 2}O{sub 3} nanocomposite were evaluated. Black-Right-Pointing-Pointer Hot deformation behavior of the nanocomposite was studied. Black-Right-Pointing-Pointer The hot deformation activation energy was determined using consecutive models. Black-Right-Pointing-Pointer The restoration mechanisms and microstructural changes are presented.« less

Explore the Effects of Microstructural Defects on Voltage Fade of Li- and Mn-Rich Cathodes

DOE PAGES

Hu, E.; Lyu, Y.; Xin, H.; ...

2016-09-26

Li- and Mn-rich (LMR) cathode materials have been considered as promising candidates for energy storage applications due to high energy density. However, these materials suffer from a serious problem of voltage fade. Oxygen loss and the layer to spinel phase transition are two major contributors of such voltage fade. In this paper, using a combination of x-ray diffraction (XRD), pair distribution function (PDF), x-ray absorption (XAS) techniques and aberration-corrected scanning transmission electron microscopy (STEM), we studied the effects of micro structural defects, especially the grain boundaries on the oxygen loss and layered-to-spinel phase transition through prelithiation of a model compoundmore » Li2Ru0.5Mn0.5O3. It is found that the nano-sized micro structural defects, especially the large amount of grain boundaries created by the prelithiation can greatly accelerate the oxygen loss and voltage fade. Defects (such as nano-sized grain boundaries) and oxygen release form a positive feedback loop, promote each other during cycling, and accelerate the two major voltage fade contributors: the transition metal reduction and layered-to-spinel phase transition. These results clearly demonstrate the important relationships among the oxygen loss, microstructural defects and voltage fade. The importance of maintaining good crystallinity and protecting the surface of LMR material are also suggested.« less

Tensile Properties and Fracture Characteristics of Nanostructured Copper and Cu-SiC Nanocomposite Produced by Mechanical Milling and Spark Plasma Sintering Process

NASA Astrophysics Data System (ADS)

Akbarpour, M. R.

2018-03-01

The presence of large grains within nanometric and ultrafine grain matrix is an effective method in order to enhance strength while keeping the high ductility of metals. For this purpose, in this research, spark plasma sintering (SPS) was used to consolidate milled Cu and Cu-SiC powders. In SPS process, local sparks with high temperature between particles take place and locally lead to intense grain growth, and therefore, this method has the ability to produce bimodal grain structures in copper and copper-based composites. Microstructural and mechanical studies showed ≈ 185 and ≈ 437 nm matrix grain sizes, high tensile yield strength values of ≈ 188.4 and ≈ 296.9 MPa, and fracture strain values of 15.1 and 6.7% for sintered Cu and Cu-4 vol.% SiC nanocomposite materials, respectively. The presence of nanoparticles promoted the occurrence of static recrystallization and decreased the fraction of coarse grains in microstructure. The high tensile properties of the produced materials are attributed to fine grain size, homogenous dispersion of nanoparticles and retarded grain boundary migration during sintering.

Corrosion behavior of alloy 800H (Fe-21Cr-32Ni) in supercritical water

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tan, Lizhen; Allen, Todd R.; Yang, Ying

2011-01-01

The effect of testing conditions (temperature, time, and oxygen content) and material's microstructure (the as-received and the grain boundary engineered conditions) on the corrosion behavior of alloy 800H in high-temperature pressurized water was studied using a variety of characterization techniques. Oxidation was observed as the primary corrosion behavior on the samples. Oxide exfoliation was significantly mitigated on the grain boundary engineered samples compared to the as-received ones. The oxide formation, including some 'mushroom-shaped oxidation', is predicted via a combination of thermodynamics and kinetics influenced by the preferential diffusion of specific species using short-cut diffusion paths.

Microstructural Modeling of Dynamic Intergranular and Transgranular Fracture Modes in Zircaloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mohammed, I.; Zikry, M.A.; Ziaei, S.

2017-04-01

In this time period, we have continued to focus on (i) refining the thermo-mechanical fracture model for zirconium (Zr) alloys subjected to large deformations and high temperatures that accounts for the cracking of ZrH and ZrH2 hydrides, (ii) formulating a framework to account intergranular fracture due to iodine diffusion and pit formation in grain-boundaries (GBs). Our future objectives are focused on extending to a combined population of ZrH and ZrH2 populations and understanding how thermo-mechanical behavior affects hydride reorientation and cracking. We will also refine the intergranular failure mechanisms for grain boundaries with pits.

Effect of crystal size distribution on thermoelectric performance for Lanthanum-doped strontium titanate bulk material

NASA Astrophysics Data System (ADS)

Zhang, Boyu; Wang, Jun; Yaer, Xinba; Huo, Zhenzhen; Wu, Yin; Li, Yan; Miao, Lei; Liu, Chengyan; Zou, Tao; Ma, Wen

2015-07-01

Effect of crystal size distribution on thermoelectric performance of Lanthanum-doped strontium titanate (La-SrTiO3) ceramics are investigated in this study. Thermoelectric performance measurement, coupled with microstructure studies, shows that the electrical conductivity strongly depends on the crystal size, potential barrier on the grain boundary and porosity. Meantime, because the average potential barriers height are increased along with the reduction of crystal size, the Seebeck coefficients are increased by energy filtering effect at the large number of grain boundaries. As a result, by controlling of crystal size distribution, ZT value of La-SrTiO3 is improved.

Microstructural evolution of pure tungsten neutron irradiated with a mixed energy spectrum

DOE PAGES

Koyanagi, Takaaki; Kumar, N. A. P. Kiran; Hwang, Taehyun; ...

2017-04-13

Here, microstructures of single-crystal bulk tungsten (W) and polycrystalline W foil with a strong grain texture were investigated using transmission electron microscopy following neutron irradiation at ~90–800 °C to 0.03–4.6 displacements per atom (dpa) in the High Flux Isotope Reactor with a mixed energy spectrum. The dominant irradiation defects were dislocation loops and small clusters at ~90 °C. Additional voids were formed in W irradiated at above 460 °C. Voids and precipitates involving transmutation rhenium and osmium were the dominant defects at more than ~1 dpa. We found a new phenomenon of microstructural evolution in irradiated polycrystalline W: Re- andmore » Os-rich precipitation along grain boundaries. Comparison of results between this study and previous studies using different irradiation facilities revealed that the microstructural evolution of pure W is highly dependent on the neutron energy spectrum in addition to the irradiation temperature and dose.« less

Microstructural evolution of pure tungsten neutron irradiated with a mixed energy spectrum

DOE Office of Scientific and Technical Information (OSTI.GOV)

Koyanagi, Takaaki; Kumar, N. A. P. Kiran; Hwang, Taehyun

Here, microstructures of single-crystal bulk tungsten (W) and polycrystalline W foil with a strong grain texture were investigated using transmission electron microscopy following neutron irradiation at ~90–800 °C to 0.03–4.6 displacements per atom (dpa) in the High Flux Isotope Reactor with a mixed energy spectrum. The dominant irradiation defects were dislocation loops and small clusters at ~90 °C. Additional voids were formed in W irradiated at above 460 °C. Voids and precipitates involving transmutation rhenium and osmium were the dominant defects at more than ~1 dpa. We found a new phenomenon of microstructural evolution in irradiated polycrystalline W: Re- andmore » Os-rich precipitation along grain boundaries. Comparison of results between this study and previous studies using different irradiation facilities revealed that the microstructural evolution of pure W is highly dependent on the neutron energy spectrum in addition to the irradiation temperature and dose.« less

Microstructure and mechanical properties of AZ91 magnesium alloy subject to deep cryogenic treatments

NASA Astrophysics Data System (ADS)

Li, Gui-rong; Wang, Hong-ming; Cai, Yun; Zhao, Yu-tao; Wang, Jun-jie; Gill, Simon P. A.

2013-09-01

AZ91 magnesium alloy was subjected to a deep cryogenic treatment. X-ray diffraction (XRD), scanning electronic microscopy (SEM), and transmission electronic microscopy (TEM) methods were utilized to characterize the composition and microstructure of the treated samples. The results show that after two cryogenic treatments, the quantity of the precipitate hardening β phase increases, and the sizes of the precipitates are refined from 8-10 μm to 2-4 μm. This is expected to be due to the decreased solubility of aluminum in the matrix at low temperature and the significant plastic deformation owing to internal differences in thermal contraction between phases and grains. The polycrystalline matrix is also noticeably refined, with the sizes of the subsequent nanocrystalline grains in the range of 50-100 nm. High density dislocations are observed to pile up at the grain boundaries, inducing the dynamic recrystallization of the microstructure, leading to the generation of a nanocrystalline grain structure. After two deep cryogenic treatments, the tensile strength and elongation are found to be substantially increased, rising from 243 MPa and 4.4% of as-cast state to 299 MPa and 5.1%.

Calcium-Magnesium-Aluminosilicate (CMAS) Reactions and Degradation Mechanisms of Advanced Environmental Barrier Coatings

NASA Technical Reports Server (NTRS)

Ahlborg, Nadia L.; Zhu, Dongming

2013-01-01

The thermochemical reactions between calcium-magnesium-aluminosilicate- (CMAS-) based road sand and several advanced turbine engine environmental barrier coating (EBC) materials were studied. The phase stability, reaction kinetics and degradation mechanisms of rare earth (RE)-silicates Yb2SiO5, Y2Si2O7, and RE-oxide doped HfO2 and ZrO2 under the CMAS infiltration condition at 1500 C were investigated, and the microstructure and phase characteristics of CMAS-EBC specimens were examined using Scanning Electron Microscopy (SEM) and X-ray Diffraction (XRD). Experimental results showed that the CMAS dissolved RE-silicates to form crystalline, highly non-stoichiometric apatite phases, and in particular attacking the silicate grain boundaries. Cross-section images show that the CMAS reacted with specimens and deeply penetrated into the EBC grain boundaries and formed extensive low-melting eutectic phases, causing grain boundary recession with increasing testing time in the silicate materials. The preliminary results also showed that CMAS reactions also formed low melting grain boundary phases in the higher concentration RE-oxide doped HfO2 systems. The effect of the test temperature on CMAS reactions of the EBC materials will also be discussed. The faster diffusion exhibited by apatite and RE-doped oxide phases and the formation of extensive grain boundary low-melting phases may limit the CMAS resistance of some of the environmental barrier coatings at high temperatures.

Two types of diffusions at the cathode/electrolyte interface in IT-SOFCs

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li Zhipeng, E-mail: LI.Zhipeng@nims.go.jp; Mori, Toshiyuki; Auchterlonie, Graeme John

2011-09-15

Analytical transmission electron microscopy, in particular with the combination of energy dispersive X-ray spectroscopy (EDX) and electron energy-loss spectroscopy (EELS), has been performed to investigate the microstructure and microchemistry of the interfacial region between the cathode (La{sub 0.6}Sr{sub 0.4}Co{sub 0.8}Fe{sub 0.2}O{sub 3}, LSCF) and the electrolyte (Gd-doped ceria, GDC). Two types of diffusions, mutual diffusion between cathode and electrolyte as well as the diffusion along grain boundaries, have been clarified. These diffusions suggest that the chemical stability of LSCF and GDC are not as good as previously reported. The results are more noteworthy if we take into consideration the factmore » that such interdiffusions occur even during the sintering process of cell preparation. - Graphical Abstract: Two types of diffusions, the mutual diffusion and the diffusion along grain boundaries, occurred at the cathode/electrolyte interface of intermediate temperature solid state fuel cells, during cell preparation. The mutual diffusion is denoted by black arrows and the diffusion along grain boundaries assigned by pink arrows. Highlights: > All the cations in cathode (LSCF) and electrolyte (GDC) can mutually diffuse into each other. > Diffusing elements will segregate at grain boundaries or triple junctions around the cathode/electrolyte interface. > Two types of diffusions, the mutual diffusion and diffusion along grain boundaries, have been clarified thereafter.« less

Microstructural evolution in the HAZ of Inconel 718 and correlation with the hot ductility test

NASA Technical Reports Server (NTRS)

Thompson, R. G.; Genculu, S.

1983-01-01

The nickel-base alloy 718 was evaluated to study the role of preweld heat treatment in reducing or eliminating heat-affected zone hot cracking. Three heat treatments were studied using the Gleeble hot ductility test. A modified hot ductility test was also used to follow the evolution of microstructure during simulated welding thermal cycles. The microstructural evolution was correlated with the hot ductility data in order to evaluate the mechanism of hot cracking in alloy 718. The correlation of hot ductility with microstructure showed that recrystallization, grain growth, and dissolution of precipitates did not in themselves cause any loss of ductility during cooling. Ductility loss during cooling was not initiated until the constitutional liquation of NbC particles was observed in the microstructure. Laves-type phases were found precipitated in the solidified grain boundaries but were not found to correlate with any ductility loss parameter. Mechanisms are reviewed which help to explain how heat treatment controls the hot crack susceptibility of alloy 718 as measured in the hot ductility test.

Ferrite grain refinement in low carbon Cu–P–Cr–Ni–Mo weathering steel at various temperatures in the (α + γ) region

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Chunling, E-mail: zhangchl@ysu.edu.cn; School of Materials Science and Engineering, Hebei University of Technology, Tianjin 300401; Zhang, Mengmeng

2016-03-15

Self-designed Cu–P–Cr–Ni–Mo weathering steel was subjected to compression test to determine the mechanism of ferrite grain refinement from 750 °C to 925 °C. Optical microscopic images showed that ferrite grain size declined, whereas the ferrite volume fraction increased with increasing compression temperature. Electron backscatter diffraction patterns revealed that several low-angle boundaries shifted to high-angle boundaries, thereby generating fine ferrite grains surrounded by high-angle boundaries. Numerous low-angle boundaries were observed within ferrite grains at 750 °C, which indicated the existence of pre-eutectoid ferrite. Results showed that ferrite grain refinement could be due to continuous dynamic recrystallization at 750 °C and 775more » °C, and deformation-induced ferrite transformation could be the main mechanism at 800 °C and 850 °C. Fine equiaxed ferrite grains with size ranging from 1.77 μm to 2.69 μm were produced in the (α + γ) dual-phase region. - Graphical abstract: There is a close relationship between the microstructure evolution and flow curves during deformation. Fine equiaxed ferrite grains with size ranging from 1.77 μm to 2.69 μm were achieved in the (α + γ) dual-phase region. Ferrite grain refinement could be due to continuous dynamic recrystallization at 750 °C and 775 °C, and deformation-induced ferrite transformation at 800 °C and 850 °C. The occurrence of deformation-induced ferrite transformation and continuous dynamic recrystallization can be monitored by analysis of flow curves and microstructures. Deformation-induced ferrite transformation leads to the dynamic softening in flow curve when temperature just below A{sub r3}, while the dynamic softening in flow curve is ferrite continuous dynamic recrystallization (Special Fig. 5b). - Highlights: • Compression deformation was operated at temperatures from 750 °C to 925 °C at a strain rate of 0.1 s–1, and a strain of 1.2. • Fine equiaxed ferrite grains of ~1.77–2.19 μm were obtained at 750 °C and 775 °C via continuous dynamic recrystallization. • Ferrite grain size of ~2.31–2.69 μm at 800 °C and 850 °C can be obtained by deformation-induced ferrite transformation. • With decreasing deformation temperature the average grain size of ferrite decreased while volume fraction increased. • Ferrite refinement was from deformation-induced ferrite to continuous dynamic recrystallization as temperature reduced.« less

Effect of Alloy Elements on Microstructures and Mechanical Properties in Al-Mg-Si Alloys

NASA Astrophysics Data System (ADS)

Kato, Yoshikazu; Hisayuki, Koji; Sakaguchi, Masashi; Higashi, Kenji

Microstructures and mechanical properties in the modified Al-Mg-Si alloys with variation in the alloy elements and their contents were investigated to enhance higher strength and ductility. Optimizing both the alloy element design and the industrial processes including heat-treatments and extrusion technology was carried out along the recent suggestion from the first principles calculation. The investigation concluded that the addition of Fe and/or Cu could recovery their lost ductility, furthermore increase their tensile strength up to 420 MPa at high elongation of 24 % after T6 condition for Al-0.8mass%Mg-1.0mass%Si-0.8mass%Cu-0.5mass%Fe alloy with excess Si content. The excellent combination between strength and ductility could be obtained by improvement to the grain boundary embitterment caused by grain boundary segregation of Si as a result from the interaction of Si with Cu or Fe with optimizing the amount of Cu and Fe contents.

Optimization of the injection molding process for development of high performance calcium oxide -based ceramic cores

NASA Astrophysics Data System (ADS)

Zhou, P. P.; Wu, G. Q.; Tao, Y.; Cheng, X.; Zhao, J. Q.; Nan, H.

2018-02-01

The binder composition used for ceramic injection molding plays a crucial role on the final properties of sintered ceramic and to avoid defects on green parts. In this study, the effects of binder compositions on the rheological, microstructures and the mechanical properties of CaO based ceramic cores were investigated. It was found that the optimized formulation for dispersant, solid loading was 1.5 wt% and 84 wt%, respectively. The microstructures, such as porosity, pore size distribution and grain boundary density were closely related to the plasticizer contents. The decrease of plasticizer contents can enhance the strength of the ceramic cores but with decreased shrinkage. Meanwhile, the creep resistance of ceramic cores was enhanced by decreasing of plasticizer contents. The flexural strength of the core was found to decrease with the increase of the porosity, the improvement of creep resistance is closely related to the decrease of porosity and grain boundary density.

Effect of cold deformation on the electrochemical behaviour of 304L stainless steel in contaminated sulfuric acid environment

NASA Astrophysics Data System (ADS)

Luo, Hong; Su, Huaizhi; Ying, Guobing; Dong, Chaofang; Li, Xiaogang

2017-12-01

The effect of cold deformation on the microstructure and electrochemical corrosion behaviour of 304L stainless steel in contaminated sulfuric acid solutions (simulated proton exchange membrane fuel cells environments) were evaluated using electron backscatter diffraction analyses, electrochemical measurements, and surface analyses. The internal microstructure,including the grain sizes, angles of the grain boundaries, low coincidence site lattice boundaries, and phase transformations, was changed due to the cold deformation. No noticeable modifications of the pitting corrosion potential were observed during the various deformations, except for a slight enhancement in the passive current density with an increase in the deformation. The CrO3 and metal Ni species in the passive film were investigated after deformation. After heavy deformation (greater than 60%), nickel oxides were detected. Moreover, the Cr/Fe and O2-/OH- ratios in the passive film were higher before deformation, and they decreased with an increase in the deformation level.

Mechanical and Microstructural Characterization of a New Corrosion Resistant Stainless Steel

NASA Astrophysics Data System (ADS)

Voiculescu, I.; Geantă, V.; Stefănoiu, R.; Cotruţ, C.; Ciocoiu, R.; Ionescu, M.

2018-06-01

The paper investigates the manner in which the chemical composition and delivery status of a new type of stainless steel, highly alloyed with Ni and Cr, affect mechanical properties, microstructure and corrosion resistance. The results obtained during the mechanical test (tensile, compression, Charpy test and micro-hardness) have revealed promising values. During the corrosion test, the preferential attack of the reagent (Aqua regia) located on the grain boundaries, inclusions or polyhedral precipitates have been observed. On the corroded surfaces, some localized pitting effects on grain boundaries have been revealed. The analyses of the parameter values recorded during the corrosion test revealed that the corrosion current density had a low value, comparable to that of other specific types of stainless steels. The actual Icorr (1.089 µA/cm2) value measured for the experimental alloy proves good resistance to corrosion in 3% NaCl saline solution. The estimated rate of corrosion presented acceptable values (0.011 mm/year).

Influence of Step Annealing Temperature on the Microstructure and Pitting Corrosion Resistance of SDSS UNS S32760 Welds

NASA Astrophysics Data System (ADS)

Yousefieh, M.; Shamanian, M.; Saatchi, A.

2011-12-01

In the present work, the influence of step annealing heat treatment on the microstructure and pitting corrosion resistance of super duplex stainless steel UNS S32760 welds have been investigated. The pitting corrosion resistance in chloride solution was evaluated by potentiostatic measurements. The results showed that step annealing treatments in the temperature ranging from 550 to 1000 °C resulted in a precipitation of sigma phase and Cr2N along the ferrite/austenite and ferrite/ferrite boundaries. At this temperature range, the metastable pits mainly nucleated around the precipitates formed in the grain boundary and ferrite phase. Above 1050 °C, the microstructure contains only austenite and ferrite phases. At this condition, the critical pitting temperature of samples successfully arrived to the highest value obtained in this study.

Structural and electrical properties of conducting diamond nanowires.

PubMed

Sankaran, Kamatchi Jothiramalingam; Lin, Yen-Fu; Jian, Wen-Bin; Chen, Huang-Chin; Panda, Kalpataru; Sundaravel, Balakrishnan; Dong, Chung-Li; Tai, Nyan-Hwa; Lin, I-Nan

2013-02-01

Conducting diamond nanowires (DNWs) films have been synthesized by N₂-based microwave plasma enhanced chemical vapor deposition. The incorporation of nitrogen into DNWs films is examined by C 1s X-ray photoemission spectroscopy and morphology of DNWs is discerned using field-emission scanning electron microscopy and transmission electron microscopy (TEM). The electron diffraction pattern, the visible-Raman spectroscopy, and the near-edge X-ray absorption fine structure spectroscopy display the coexistence of sp³ diamond and sp² graphitic phases in DNWs films. In addition, the microstructure investigation, carried out by high-resolution TEM with Fourier transformed pattern, indicates diamond grains and graphitic grain boundaries on surface of DNWs. The same result is confirmed by scanning tunneling microscopy and scanning tunneling spectroscopy (STS). Furthermore, the STS spectra of current-voltage curves discover a high tunneling current at the position near the graphitic grain boundaries. These highly conducting regimes of grain boundaries form effective electron paths and its transport mechanism is explained by the three-dimensional (3D) Mott's variable range hopping in a wide temperature from 300 to 20 K. Interestingly, this specific feature of high conducting grain boundaries of DNWs demonstrates a high efficiency in field emission and pave a way to the next generation of high-definition flat panel displays or plasma devices.

High strength Sn-Mo-Nb-Zr alloy tubes and method of making same

DOEpatents

Cheadle, Brian A.

1977-01-01

Tubes for use in nuclear reactors fabricated from a quaternary alloy comprising 2.5-4.0 wt% Sn, 0.5-1.5 wt% Mo, 0.5-1.5 wt% Nb, balance essentially Zr. The tubes are fabricated by a process of hot extrusion, heat treatment, cold working to size and age hardening, so as to produce a microstructure comprising elongated .alpha. grains with an acicular transformed .beta. grain boundary phase.

The Effects of Grain Size and Texture on Dynamic Abnormal Grain Growth in Mo

NASA Astrophysics Data System (ADS)

Noell, Philip J.; Taleff, Eric M.

2016-10-01

This is the first report of abnormal grain morphologies specific to a Mo sheet material produced from a commercial-purity arc-melted ingot. Abnormal grains initiated and grew during plastic deformation of this material at temperatures of 1793 K and 1813 K (1520 °C and 1540 °C). This abnormal grain growth during high-temperature plastic deformation is termed dynamic abnormal grain growth, DAGG. DAGG in this material readily consumes nearly all grains near the sheet center while leaving many grains near the sheet surface unconsumed. Crystallographic texture, grain size, and other microstructural features are characterized. After recrystallization, a significant through-thickness variation in crystallographic texture exists in this material but does not appear to directly influence DAGG propagation. Instead, dynamic normal grain growth, which may be influenced by texture, preferentially occurs near the sheet surface prior to DAGG. The large grains thus produced near the sheet surface inhibit the subsequent growth of the abnormal grains produced by DAGG, which preferentially consume the finer grains near the sheet center. This produces abnormal grains that span the sheet center but leave unconsumed polycrystalline microstructure near the sheet surface. Abnormal grains are preferentially oriented with the < 110rangle approximately along the tensile axis. These results provide additional new evidence that boundary curvature is the primary driving force for DAGG in Mo.

Phase transformation kinetics in rolled U-10 wt. % Mo foil: Effect of post-rolling heat treatment and prior γ-UMo grain size

DOE PAGES

Jana, Saumyadeep; Overman, Nicole; Varga, Tamas; ...

2017-09-25

Here, the effect of sub-eutectoid heat treatment on the phase transformation behavior in rolled U-10 wt.% Mo (U10Mo) foils was systematically investigated. The as-cast 5 mm thick foils were initially homogenized at 900 °C for 48 h and were hot rolled to 2 mm and later cold rolled down to 0.2 mm. Three starting microstructures were evaluated: (i) hot + cold-rolled to 0.2 mm (as-rolled condition), (ii) hot + cold-rolled to 0.2 mm + annealed at 700 °C for 1 h, and (iii) hot + cold-rolled to 0.2 mm + annealed at 1000 °C for 60 h. Annealing of as-rolledmore » materials at 700 °C resulted in small grain size (15 ± 9 μm average grain size), while annealing at 1000 °C led to very large grains (156 ± 118 μm average grain size) in rolled U10Mo foils. Later the samples were subjected to sub-eutectoid heat-treatment temperatures of 550 °C, 500 °C, and 400 °C for different durations of time starting from 1 h up to 100 h. U10Mo rolled foils went through various degrees of decomposition when subjected to the sub-eutectoid heat-treatment step and formed a lamellar microstructure through a cellular reaction mostly along the previous γ-UMo grain boundaries. The least amount of cellular reaction was observed in the large-grain microstructure at all temperatures. Conversely, a substantial amount of cellular reaction was observed in both the as-rolled and the small-grain microstructure. After 100 h of heat treatment at 500 °C, the volume fraction of the lamellar phase was found to be 4%, 22%, and 82% in large-grain, as-rolled, and small-grain samples, respectively.« less

Phase transformation kinetics in rolled U-10 wt. % Mo foil: Effect of post-rolling heat treatment and prior γ-UMo grain size

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jana, Saumyadeep; Overman, Nicole; Varga, Tamas

Here, the effect of sub-eutectoid heat treatment on the phase transformation behavior in rolled U-10 wt.% Mo (U10Mo) foils was systematically investigated. The as-cast 5 mm thick foils were initially homogenized at 900 °C for 48 h and were hot rolled to 2 mm and later cold rolled down to 0.2 mm. Three starting microstructures were evaluated: (i) hot + cold-rolled to 0.2 mm (as-rolled condition), (ii) hot + cold-rolled to 0.2 mm + annealed at 700 °C for 1 h, and (iii) hot + cold-rolled to 0.2 mm + annealed at 1000 °C for 60 h. Annealing of as-rolledmore » materials at 700 °C resulted in small grain size (15 ± 9 μm average grain size), while annealing at 1000 °C led to very large grains (156 ± 118 μm average grain size) in rolled U10Mo foils. Later the samples were subjected to sub-eutectoid heat-treatment temperatures of 550 °C, 500 °C, and 400 °C for different durations of time starting from 1 h up to 100 h. U10Mo rolled foils went through various degrees of decomposition when subjected to the sub-eutectoid heat-treatment step and formed a lamellar microstructure through a cellular reaction mostly along the previous γ-UMo grain boundaries. The least amount of cellular reaction was observed in the large-grain microstructure at all temperatures. Conversely, a substantial amount of cellular reaction was observed in both the as-rolled and the small-grain microstructure. After 100 h of heat treatment at 500 °C, the volume fraction of the lamellar phase was found to be 4%, 22%, and 82% in large-grain, as-rolled, and small-grain samples, respectively.« less

Microstructure-Based Fatigue Life Prediction Methods for Naval Steel Structures

DTIC Science & Technology

1994-09-12

random variable (LRV) model proposed by Yang et al . (10] is useful. This model employs the simplest mathematical model for which the analytical solution...consider the work of Kunio, et al . [7], who found that cracks initiated in prior austenite grain boundaries for the low carbon martensitic steels...investigated. De los Rios, et al . [8], reported about the same result for a 0.4 wt.% C steel of mixed pearlite and ferrite microstructure with the ferrite

Oxidation behavior of grain boundary engineered alloy 690 in supercritical water environment

NASA Astrophysics Data System (ADS)

Xu, P.; Zhao, L. Y.; Sridharan, K.; Allen, T. R.

2012-03-01

Nickel-base alloy is an important structural material that is known for its exceptional high temperature oxidation resistance. Oxidation in this alloy at high temperatures occurs to a greater extent along the grain boundaries. Grain boundary engineering (GBE) was applied to modify the grain boundary characteristics of this alloy to affect its oxidation resistance. Specimens with both low level and high level cold works showed a high fraction of special grain boundaries, and were tested for supercritical water oxidation resistance at 500 °C and 24 MPa. Both GBE and as-received samples exhibited mass gain followed by mass loss during 10 weeks of exposure, but the normalized mass change was small and less than 0.12 mg/cm2. GBE samples showed better oxide layer retention compared to the as-received sample. XRD results indicate that nickel oxide, chromium oxide, and spinel oxide were the three main types of oxides that form on as-received and GBE alloy 690. Three distinct regions were identified on the oxidized surface: a flat region with oxide flakes aligning relatively parallel to the surface, a rough region with polygon-type oxide particles randomly distributed on the surface, and a region with aggregated oxide flakes perpendicular to the surface. The flat region of oxidation consisted of (1 1 1) orientated oxide spinel flakes formed on (1 1 1) oriented alloy 690 grains. The flat oxide region was thinner and showed better oxide adhesion compared to the rough region. Chromium oxidation was found only at random grain boundaries, leading to formation of thick Cr2O3 layer on the surface and chromium depletion underneath. None of this oxidation was found at low angle or special boundaries. The chromium oxidation was attributed to fast chromium diffusion through random boundaries and mechanically deformed regions such as scratches left after polishing. It is envisioned that the oxidation behavior of alloy 690 in supercritical water can be tailored by microstructure engineering that involves changes in grain orientation and grain boundary character distribution.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chu, Zhaodong; Yang, Mengjin; Schulz, Philip

Organic-inorganic perovskite solar cells have attracted tremendous attention because of their remarkably high power conversion efficiencies. To further improve device performance, it is imperative to obtain fundamental understandings on the photo-response and long-term stability down to the microscopic level. Here, we report the quantitative nanoscale photoconductivity imaging on two methylammonium lead triiodide thin films with different efficiencies by light-stimulated microwave impedance microscopy. The microwave signals are largely uniform across grains and grain boundaries, suggesting that microstructures do not lead to strong spatial variations of the intrinsic photo-response. In contrast, the measured photoconductivity and lifetime are strongly affected by bulk propertiesmore » such as the sample crystallinity. As visualized by the spatial evolution of local photoconductivity, the degradation process begins with the disintegration of grains rather than nucleation and propagation from visible boundaries between grains. In conclusion, our findings provide insights to improve the electro-optical properties of perovskite thin films towards large-scale commercialization.« less

A high-throughput technique for determining grain boundary character non-destructively in microstructures with through-thickness grains

DOE PAGES

Seita, Matteo; Volpi, Marco; Patala, Srikanth; ...

2016-06-24

Grain boundaries (GBs) govern many properties of polycrystalline materials. However, because of their structural variability, our knowledge of GB constitutive relations is still very limited. We present a novel method to characterise the complete crystallography of individual GBs non-destructively, with high-throughput, and using commercially available tools. This method combines electron diffraction, optical reflectance and numerical image analysis to determine all five crystallographic parameters of numerous GBs in samples with through-thickness grains. We demonstrate the technique by measuring the crystallographic character of about 1,000 individual GBs in aluminum in a single run. Our method enables cost- and time-effective assembly of crystallography–propertymore » databases for thousands of individual GBs. Furthermore, such databases are essential for identifying GB constitutive relations and for predicting GB-related behaviours of polycrystalline solids.« less

Multi-phase-field modeling of anisotropic crack propagation for polycrystalline materials

NASA Astrophysics Data System (ADS)

Nguyen, Thanh-Tung; Réthoré, Julien; Yvonnet, Julien; Baietto, Marie-Christine

2017-08-01

A new multi-phase-field method is developed for modeling the fracture of polycrystals at the microstructural level. Inter and transgranular cracking, as well as anisotropic effects of both elasticity and preferential cleavage directions within each randomly oriented crystal are taken into account. For this purpose, the proposed phase field formulation includes: (a) a smeared description of grain boundaries as cohesive zones avoiding defining an additional phase for grains; (b) an anisotropic phase field model; (c) a multi-phase field formulation where each preferential cleavage direction is associated with a damage (phase field) variable. The obtained framework allows modeling interactions and competition between grains and grain boundary cracks, as well as their effects on the effective response of the material. The proposed model is illustrated through several numerical examples involving a full description of complex crack initiation and propagation within 2D and 3D models of polycrystals.

Tensile and fracture properties of type 316 stainless steel after creep

NASA Astrophysics Data System (ADS)

Gan, D.

1982-12-01

The effects of creep on the mechanical properties of type 316 stainless steel were studied. Tensile and Charpy specimens were machined from the oversize specimens crept at 750 °C and 103 MPa. The ambient fracture energy was found to deteriorate rapidly after creep. The ambient yield stress was increased moderately, but the tensile ductility was severely reduced. The effects of intergranular carbides alone on mechanical properties were studied with specimens thermal aged without load. These carbides were shown to cause a moderate reduction in fracture energy and tensile ductility but had little effect on yield stress. Extensive grain boundary separations were observed on the fracture surfaces. SEM studies showed that these grain boundaries were covered with micro voids initiated by the dense intergranular carbides. Frequently, large dimples on grain boundary joined up and initiated shear fracture into the grain. In the crept specimens additional microstructural changes in the form of intragranular carbides and subgrain boundaries were observed. Both are responsible for the increase in yield stress and the further reduction in tensile ductility and fracture energy. The intragranular carbides also modified the size and density of the dimples on the fracture surfaces.

Effect of Boron Microalloying Element on Susceptibility to Hydrogen Embrittlement in High Strength Mooring Chain Steel

NASA Astrophysics Data System (ADS)

Li, H.; Cheng, X. Y.; Shen, H. P.; Su, L. C.; Zhang, S. Y.

The susceptibility to hydrogen embrittlement in high strength mooring chain steel with different boron content (0, 0.003 %, 0.008 %) were investigated by electrochemical hydrogen charging technique and tensile test. The results revealed that appropriate boron content can effectively depress hydrogen induced embrittlement. Precharged with a low current density, this effect seemed to be unobvious. It gradually became clearly with the increasing current density. The increase of resistance to the hydrogen embrittlement for 3B and 8B after adding appropriate boron was attributed to three facts. The first was that the segregation of boron atoms along grain boundaries reduced the grain boundary segregation of phosphorus, which prohibited hydrogen concentration at the grain boundaries, depressing the possibility of the intergranular fracture due to H. The second was that the segregation of boron increased intergranular cohesion, enhanced grain boundary strength, and refined the final microstructure. The third was that the addition of boron changed the state of hydrogen traps, leading to the small amount of diffusible hydrogen. That is to say, hydrogen transferred to these defects by dislocations was accordingly decreased, which led to the low sensitive of hydrogen induced cracking.

Behavior of grain boundary chemistry and precipitates upon thermal treatment of controlled purity alloy 690

NASA Astrophysics Data System (ADS)

Angeliu, Thomas M.; Was, Gary S.

1990-08-01

Grain boundary composition and carbide composition and structure were characterized for various microstructures of controlled purity alloy 690. Heat treatments produced varying degrees of grain boundary chromium depletion and precipitate distributions which were characterized via scanning transmission electron microscopy (STEM). Convergent beam electron diffraction revealed that the dominant carbide is M23C6, and energy dispersive X-ray analysis (EDAX) determined that the metallic content was about 90 at. pct chromium. A discontinuous precipitation reaction was observed and is attributed to a high degree of carbon supersaturation. Grain boundary composition measurements confirm that chromium depletion is controlled by volume diffusion of chromium to chromium-rich grain boundary carbides in the temperature range of 873 to 1073 K. Grain boundary chromium levels as low as 18.8 at. pct were obtained by thermal treatment at 873 K for 250 hours and 973 K for 1 hour. A thermodynamic and kinetic model developed for alloy 600 was modified to describe the development of the chromium depletion profile in alloy 690 during thermal treatment. Experimentally measured chromium profiles agree well with the model results for the dependence of the chromium depletion zone width and depth on various input parameters. The establishment of the model for alloy 690 allows the chromium depletion zone width and depth to be computed as a function of alloy composition, grain size, and temperature. The chromium depletion profiles and the precipitate structure and composition of controlled purity 690 are compared to those of controlled purity 600. A thermodynamic analysis of the carbide stability indicates that other factors, such as favorable orientation relationships, play an important role in controlling the precipitation of Cr23C6 in nickel-base alloys.

Fusion zone microstructure and porosity in electron beam welds of an α+β titanium alloy

NASA Astrophysics Data System (ADS)

Mohandas, T.; Banerjee, D.; Kutumba Rao, V. V.

1999-03-01

The effect of electron beam welding parameters on fusion zone (FZ) microstructure and porosity in a Ti -6.8 Al -3.42 Mo -1.9 Zr -0.21 Si alloy (Russian designation VT 9) has been investigated. It has been observed that the FZ grain width increased continuously with increase in heat input when the base metal was in the β heat-treated condition, while in the α+β heat-treated base metal welds, the FZ grain width increased only after a threshold energy input. The difference is attributed to both the weld thermal cycle and the pinning effect of equiaxed primary alpha on grain growth in the heat-affected zone (HAZ) of α+β heat-treated base metal. Postweld heat treatment (PWHT) in the subtransus and supertransus regions did not alter the columnar grain morphology in the FZ, possibly due to the lack of enough driving force for the formation of new grains by the breaking up of the columnar grains and grain boundary movement for grain growth. As the PWHTs were conducted in a furnace, the role of thermal gradients can be ruled out. Intragranular microstructure in the aswelded condition consisted of hexagonal martensite. The scale of the martensite laths depended on welding speed. The highest porosity was observed at intermediate welding speeds. At low speeds, a majority of pores formed at the fusion boundary, while at high speeds, occurrence of porosity was maximum at the weld center. The trends on porosity can be explained on the basis of solubility of hydrogen in titanium as a function of temperature and the influence of weld thermal cycle on nucleation, growth, and escape of hydrogen gas bubbles. The porosity at slow welding speeds is low because sufficient time exists for the nucleation, growth, and escape of hydrogen gas bubbles, while insufficient time exists for the nucleation of gas bubbles at high welding speeds. The effect of pickling of joint surface, vacuum annealing of the base metal, and successive remelting of the weld metal has also been investigated.

Influences of granular constraints and surface effects on the heterogeneity of elastic, superelastic, and plastic responses of polycrystalline shape memory alloys

DOE PAGES

Paranjape, Harshad M.; Paul, Partha P.; Sharma, Hemant; ...

2017-02-16

Deformation heterogeneities at the microstructural length-scale developed in polycrystalline shape memory alloys (SMAs) during superelastic loading are studied using both experiments and simulations. In situ X-ray diffraction, specifically the far-field high energy diffraction microscopy (ff-HEDM) technique, was used to non-destructively measure the grain-averaged statistics of position, crystal orientation, elastic strain tensor, and volume for hundreds of austenite grains in a superelastically loaded nickel-titanium (NiTi) SMA. These experimental data were also used to create a synthetic microstructure within a finite element model. The development of intragranular stresses were then simulated during tensile loading of the model using anisotropic elasticity. Driving forcesmore » for phase transformation and slip were calculated from these stresses. The grain-average responses of individual austenite crystals examined before and after multiple stress-induced transformation events showed that grains in the specimen interior carry more axial stress than the surface grains as the superelastic response "shakes down". Examination of the heterogeneity within individual grains showed that regions near grain boundaries exhibit larger stress variation compared to the grain interiors. As a result, this intragranular heterogeneity is more strongly driven by the constraints of neighboring grains than the initial stress state and orientation of the individual grains.« less

Influences of granular constraints and surface effects on the heterogeneity of elastic, superelastic, and plastic responses of polycrystalline shape memory alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Paranjape, Harshad M.; Paul, Partha P.; Sharma, Hemant

Deformation heterogeneities at the microstructural length-scale developed in polycrystalline shape memory alloys (SMAs) during superelastic loading are studied using both experiments and simulations. In situ X-ray diffraction, specifically the far-field high energy diffraction microscopy (ff-HEDM) technique, was used to non-destructively measure the grain-averaged statistics of position, crystal orientation, elastic strain tensor, and volume for hundreds of austenite grains in a superelastically loaded nickel-titanium (NiTi) SMA. These experimental data were also used to create a synthetic microstructure within a finite element model. The development of intragranular stresses were then simulated during tensile loading of the model using anisotropic elasticity. Driving forcesmore » for phase transformation and slip were calculated from these stresses. The grain-average responses of individual austenite crystals examined before and after multiple stress-induced transformation events showed that grains in the specimen interior carry more axial stress than the surface grains as the superelastic response "shakes down". Examination of the heterogeneity within individual grains showed that regions near grain boundaries exhibit larger stress variation compared to the grain interiors. As a result, this intragranular heterogeneity is more strongly driven by the constraints of neighboring grains than the initial stress state and orientation of the individual grains.« less

A study of fractography in the low-temperature brittle fracture of an 18Cr-18Mn-0.7N austenitic steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, S.C.; Hashida, T.; Takahashi, H.

1998-03-01

The fracture mode and crack propagation behavior of brittle fracture at 77 and 4 K in an 18Cr-18Mn-0.7N austenitic stainless were investigated using optical and scanning electron microscopy. The fracture path was examined by observing the side surface in a partially ruptured specimen. The relationship of the fracture facets to the microstructures were established by observing the fracture surface and the adjacent side surface simultaneously. Three kinds of fracture facets were identified at either temperature. The first is a smooth curved intergranular fracture facet with characteristic parallel lines on it. The second is a fairly planar facet formed by partingmore » along an annealing twin boundary, a real {l_brace}111{r_brace} plane. There are three sets of parallel lines on the facet and the lines in different sets intersect at 60 deg. The third is a lamellar transgranular fracture facet with sets of parallel steps on it. Fracture propagated by the formation of microcracks on a grain boundary, annealing twin boundary, and coalescence of these cracks. The observation suggests that the ease of crack initiation and propagation along the grain boundary and the annealing twin boundary may be the main reason for the low-temperature brittleness of this steel. A mechanism for grain boundary cracking, including annealing twin boundary parting, has been discussed based on the stress concentration induced by impinging planar deformation structures on the grain boundaries.« less

Monte Carlo modeling of recrystallization processes in α-uranium

DOE PAGES

Steiner, M. A.; McCabe, R. J.; Garlea, E.; ...

2017-08-01

In this study, starting with electron backscattered diffraction (EBSD) data obtained from a warm clock-rolled α-uranium deformation microstructure, a Potts Monte Carlo model was used to simulate static site-saturated recrystallization while testing a number of different conditions for the assignment of recrystallized nuclei within the microstructure. The simulations support observations that recrystallized nuclei within α-uranium form preferentially on non-twin high-angle grain boundary sites at 450 °C, and demonstrate that the most likely nucleation sites on these boundaries can be identified by the surrounding degree of Kernel Average Misorientation (KAM), which may be considered as a proxy for the local geometricallymore » necessary dislocation (GND) density.« less

Extreme grain size reduction in dolomite: microstructures and mechanisms.

NASA Astrophysics Data System (ADS)

Kennedy, L.; White, J. C.

2007-12-01

Pure dolomite sample were deformed at room temperature and under a variety of confining pressures (0 - 100MPa) to examine the processes of grain size reduction. The dolomite is composed of > 97 vol. % dolomite with accessory quartz, calcite, tremolite, and muscovite and has been metamorphosed to amphibolite facies and subsequently annealed. At the hand sample scale, the rock is isotropic, except for minor, randomly oriented tremolite porphyroblasts, and weakly aligned muscovite. At the thin section scale, coarser grains have lobate grain boundaries, exhibit minor to no undulose extinction and few deformation twins, although well- developed subgrains are present. Growth twins are common, as is the presence of well developed {1011} cleavage. Mean grain size 476 microns, and porosity is essentially zero (Austin and Kennedy, 2006). Samples contain diagonal to subvertical faults. Fractures are lined with an exceptionally fine-grained, powdered dolomite. Even experiments done at no confining pressure and stopped before sliding on the fracture surfaces occurred had significant powdered gouge developed along the surfaces. In this regard, fracturing of low porosity, pure dolomite, with metamorphic textures (e.g. lobate, interlocking grain boundaries) results in the development of fine-grained gouge. As expected the dolomite exhibited an increase in strength with increasing confining pressure, with a maximum differential stress of ~400MPa at 100 MPa confining pressure. At each chosen confining pressure, two experiments were performed and stopped at different stages along the load-displacement curve: just before yield stress and at peak stress. Microstructures at each stage were observed in order to determine the possible mechanisms for extreme grain size reduction. SEM work shows that in samples with little to no apparent displacement along microfractures, extreme grain size reduction still exists, suggesting that frictional sliding and subsequent cataclasis may not be the mechanism responsible for grain size reduction. Within individual dolomite clasts, apparent Mode I cracks are also lined with powedered gouge. Alternative mechanisms for grain size reduction are explored. Austin et al. 2005, Geological Society, London, Special Publications, 243, 51-66.3.

Effects of grain size and humidity on fretting wear in fine-grained alumina, Al{sub 2}O{sub 3}/TiC, and zirconia

DOE Office of Scientific and Technical Information (OSTI.GOV)

Krell, A.; Klaffke, D.

Friction and wear of sintered alumina with grain sizes between 0.4 and 3 {micro}m were measured in comparison with Al{sub 2}O{sub 3}/TiC composites and with tetragonal ZrO{sub 2} (3 mol% Y{sub 2}O{sub 3}). The dependence on the grain boundary toughness and residual microstresses is investigated, and a hierarchical order of influencing parameters is observed. In air, reduced alumina grain sizes improve the micromechanical stability of the grain boundaries and the hardness, and reduced wear is governed by microplastic deformation, with few pullout events. Humidity and water slightly reduce the friction of all of the investigated ceramics. In water, this effectmore » reduces the wear of coarser alumina microstructures. The wear of aluminas and of the Al{sub 2}O{sub 3}/TiC composite is similar; it is lower than observed in zirconia, where extended surface cracking occurs at grain sizes as small as 0.3 {micro}m.« less

The microstructures of SCS-6 and SCS-8 SiC reinforcing fibers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sattler, M.L.; Kinney, J.H.; Zywicz, E.

The microstructures of SCS-6 and SCS-8 SiC fibers have been examined and analyzed using high resolution transmission electron microscopy (HRTEM), microdiffraction, parallel electron energy loss spectroscopy (PEELS), x-ray diffraction and x-ray spectroscopy. The results of the study confirm findings from earlier studies wherein the microstructure of the fibers have been described as consisting of {beta}-SiC grown upon a monofilament turbostratic carbon core. The present study, however, provides much more detail regarding this microstructure. For example, PEELS spectroscopy and x-ray microscopy indicate that the composition of the SiC varies smoothly from SiC plus free C near the carbon core to SiCmore » at the midradial boundary. The SiC stoichiometry is roughly preserved from the midradial boundary to the exterior interface. HRTEM, microdiffraction, and dark field images provide evidence that the excess carbon is amorphous free carbon which is most likely situated at the grain boundaries of the SiC. The x-ray microscopy results are also consistent with the presence of two phases near the core which consist of SiC and free carbon having density less than graphite (2.25 g/cc). This complex microstructure may explain the recent observations of nonplanar failure in composites fabricated with SCS fibers.« less

Effect of Cooling Rate on Microstructure of Two Kinds of High Nb Containing Tial Alloys

NASA Astrophysics Data System (ADS)

Chai, L. H.; Feng, Z. Y.; Xiang, Z. L.; Cui, Y. S.; Zhou, F.; Chen, Z. Y.

2017-09-01

In this paper, high Nb-TiAl alloys with Cr and W additions were prepared by Vacuum induction melting method, and then were heat treated under three different cooling rates of slow cooling, furnace cooling and air cooling. The phase composition of the alloy was analyzed by X ray diffraction, and the microstructure of the alloy was observed by optical microscope (OM), scanning electron microscope (SEM) and energy dispersive analyzer. The results show that the microstructure of Ti45Al8Nb0.2Cr and Ti45Al8Nb0.2W are fully lamellar structure with the main phase composition of α+γ after 3 different heat treatment conditions. The grain size of the two alloys decreases with decreasing of cooling rate, and the grain size of the alloyed with Cr alloy is smaller than that of the alloyed with W alloy. Most of the original massive β phase at grain boundaries and lamellar interfaces dissolved after heat treatment, and the transformation of β phase is easier for Ti45Al8Nb0.2Cr.

A search for shocked quartz grains in the Allerød-Younger Dryas boundary layer

NASA Astrophysics Data System (ADS)

Hoesel, Annelies; Hoek, Wim Z.; Pennock, Gillian M.; Kaiser, Knut; Plümper, Oliver; Jankowski, Michal; Hamers, Maartje F.; Schlaak, Norbert; Küster, Mathias; Andronikov, Alexander V.; Drury, Martyn R.

2015-03-01

The Younger Dryas impact hypothesis suggests that multiple airbursts or extraterrestrial impacts occurring at the end of the Allerød interstadial resulted in the Younger Dryas cold period. So far, no reproducible, diagnostic evidence has, however, been reported. Quartz grains containing planar deformation features (known as shocked quartz grains), are considered a reliable indicator for the occurrence of an extraterrestrial impact when found in a geological setting. Although alleged shocked quartz grains have been reported at a possible Allerød-Younger Dryas boundary layer in Venezuela, the identification of shocked quartz in this layer is ambiguous. To test whether shocked quartz is indeed present in the proposed impact layer, we investigated the quartz fraction of multiple Allerød-Younger Dryas boundary layers from Europe and North America, where proposed impact markers have been reported. Grains were analyzed using a combination of light and electron microscopy techniques. All samples contained a variable amount of quartz grains with (sub)planar microstructures, often tectonic deformation lamellae. A total of one quartz grain containing planar deformation features was found in our samples. This shocked quartz grain comes from the Usselo palaeosol at Geldrop Aalsterhut, the Netherlands. Scanning electron microscopy cathodoluminescence imaging and transmission electron microscopy imaging, however, show that the planar deformation features in this grain are healed and thus likely to be older than the Allerød-Younger Dryas boundary. We suggest that this grain was possibly eroded from an older crater or distal ejecta layer and later redeposited in the European sandbelt. The single shocked quartz grain at this moment thus cannot be used to support the Younger Dryas impact hypothesis.

Reconstruction of 3d grain boundaries from rock thin sections, using polarised light

NASA Astrophysics Data System (ADS)

Markus Hammes, Daniel; Peternell, Mark

2016-04-01

Grain boundaries affect the physical and chemical properties of polycrystalline materials significantly by initiating reactions and collecting impurities (Birchenall, 1959), and play an essential role in recrystallization (Doherty et al. 1997). In particular, the shape and crystallographic orientation of grain boundaries reveal the deformation and annealing history of rocks (Kruhl and Peternell 2002, Kuntcheva et al. 2006). However, there is a lack of non-destructive and easy-to-use computer supported methods to determine grain boundary geometries in 3D. The only available instrument using optical light to measure grain boundary angles is still the polarising microscope with attached universal stage; operated manually and time-consuming in use. Here we present a new approach to determine 3d grain boundary orientations from 2D rock thin sections. The data is recorded by using an automatic fabric analyser microscope (Peternell et al., 2010). Due to its unique arrangement of 9 light directions the highest birefringence colour due to each light direction and crystal orientation (retardation) can be determined at each pixel in the field of view. Retardation profiles across grain boundaries enable the calculation of grain boundary angle and direction. The data for all positions separating the grains are combined and further processed. In combination with the lateral position of the grain boundary, acquired using the FAME software (Hammes and Peternell, in review), the data is used to reconstruct a 3d grain boundary model. The processing of data is almost fully automatic by using MATLAB®. Only minor manual input is required. The applicability was demonstrated on quartzite samples, but the method is not solely restricted on quartz grains and other birefringent polycrystalline materials could be used instead. References: Birchenall, C.E., 1959: Physical Metallurgy. McGraw-Hill, New York. Doherty, R.D., Hughes, D.A., Humphreys, F.J., Jonas, J.J., Juul Jensen, D., Kassner, M.E., King, W.E., McNelley, T.R., McQueen, H.J., Rollett, A.D., 1997: Current issues in recrystallization: a review. Materials Science and Engineering A 238, 219-274. Hammes, D.M., Peternell, M., in review. FAME: Software for analysing rock microstructures. Computers & Geoscience. Kruhl, J.H., Peternell, M., 2002. The equilibration of high-angle grain boundaries in dynamically recrystallized quartz: the effect of crystallography and temperature. Journal of Structural Geology 24, 1125-1137. Kuntcheva, B., Kruhl, J.H. & Kunze, K., 2006. Crystallographic orientation of high-angle grain boundaries in dynamically recrystallized quartz: First results. Tectonophysics 421, 331-346. Peternell, M., Hasalová, P., Wilson, J.L., Piaziolo, S., Schulmann, K., 2010. Evaluating quartz crystallographic preferred orientations and the role of deformation partitioning using EBSD and fabric analyser techniques. Journal of Structural Geology 32, 803-817.

Microstructure control of Al-Cu films for improved electromigration resistance

DOEpatents

Frear, Darrel R.; Michael, Joseph R.; Romig, Jr., Alton D.

1994-01-01

A process for the forming of Al-Cu conductive thin films with reduced electromigration failures is useful, for example, in the metallization of integrated circuits. An improved formation process includes the heat treatment or annealing of the thin film conductor at a temperature within the range of from 200.degree. C. to 300.degree. C. for a time period between 10 minutes and 24 hours under a reducing atmosphere such as 15% H.sub.2 in N.sub.2 by volume. Al-Cu thin films annealed in the single phase region of a phase diagram, to temperatures between 200.degree. C. and 300.degree. C. have .theta.-phase Al.sub.2 Cu precipitates at the grain boundaries continuously become enriched in copper, due, it is theorized, to the formation of a thin coating of .theta.-phase precipitate at the grain boundary. Electromigration behavior of the aluminum is, thus, improved because the .theta.-phase precipitates with copper hinder aluminum diffusion along the grain boundaries. Electromigration, then, occurs mainly within the aluminum grains, a much slower process.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Khafizov, M.; Pakarinen, J.; He, L.

We report on imaging subsurface grain microstructure using picosecond ultrasonics. This approach relies on elastic anisotropy of crystalline materials where ultrasonic velocity depends on propagation direction relative to the crystal axes. Picosecond duration ultrasonic pulses are generated and detected using ultrashort light pulses. In materials that are transparent or semitransparent to the probe wavelength, the probe monitors GHz Brillouin oscillations. The frequency of these oscillations is related to the ultrasonic velocity and the optical index of refraction. Ultrasonic waves propagating across a grain boundary experience a change in velocity due to a change in crystallographic orientation relative to the ultrasonicmore » propagation direction. This change in velocity is manifested as a change in the Brillouin oscillation frequency. Using the ultrasonic propagation velocity, the depth of the interface can be determined from the location in time of the transition in oscillation frequency. An image of the grain boundary is obtained by scanning the beam along the surface. We demonstrate this volumetric imaging capability using a polycrystalline UO 2 sample. As a result, cross section liftout analysis of the grain boundaries using electron microscopy were used to verify our imaging results.« less

Grain wall boundaries in centimeter-scale continuous monolayer WS2 film grown by chemical vapor deposition.

PubMed

Jia, Zhiyan; Hu, Wentao; Xiang, Jianyong; Wen, Fusheng; Nie, Anmin; Mu, Congpu; Zhao, Zhisheng; Xu, Bo; Tian, Yongjun; Liu, Zhongyuan

2018-06-22

Centimeter-scale continuous monolayer WS 2 film with large tensile strain has been successfully grown on oxidized silicon substrate by chemical vapor deposition, in which monolayer grains can be more than 200 μm in size. Monolayer WS 2 grains are observed to merge together via not only traditional grain boundaries but also non-traditional ones, which are named as grain walls (GWs) due to their nanometer-scale widths. The GWs are revealed to consist of two or three layers. Though not a monolayer, the GWs exhibit significantly enhanced fluorescence and photoluminescence. This enhancement may be attributed to abundant structural defects such as stacking faults and partial dislocations in the GWs, which are clearly observable in atomically resolved high resolution transmission electron microscopy and scanning transmission electron microscopy images. Moreover, GW-based phototransistor is found to deliver higher photocurrent than that based on monolayer film. These features of GWs provide a clue to microstructure engineering of monolayer WS 2 for specific applications in (opto)electronics.

Grain wall boundaries in centimeter-scale continuous monolayer WS2 film grown by chemical vapor deposition

NASA Astrophysics Data System (ADS)

Jia, Zhiyan; Hu, Wentao; Xiang, Jianyong; Wen, Fusheng; Nie, Anmin; Mu, Congpu; Zhao, Zhisheng; Xu, Bo; Tian, Yongjun; Liu, Zhongyuan

2018-06-01

Centimeter-scale continuous monolayer WS2 film with large tensile strain has been successfully grown on oxidized silicon substrate by chemical vapor deposition, in which monolayer grains can be more than 200 μm in size. Monolayer WS2 grains are observed to merge together via not only traditional grain boundaries but also non-traditional ones, which are named as grain walls (GWs) due to their nanometer-scale widths. The GWs are revealed to consist of two or three layers. Though not a monolayer, the GWs exhibit significantly enhanced fluorescence and photoluminescence. This enhancement may be attributed to abundant structural defects such as stacking faults and partial dislocations in the GWs, which are clearly observable in atomically resolved high resolution transmission electron microscopy and scanning transmission electron microscopy images. Moreover, GW-based phototransistor is found to deliver higher photocurrent than that based on monolayer film. These features of GWs provide a clue to microstructure engineering of monolayer WS2 for specific applications in (opto)electronics.

Friction Freeform Fabrication of Superalloy Inconel 718: Prospects and Problems

NASA Astrophysics Data System (ADS)

Dilip, J. J. S.; Janaki Ram, G. D.

2014-01-01

Friction Freeform Fabrication is a new solid-state additive manufacturing process. The present investigation reports a detailed study on the prospects of this process for additive part fabrication in superalloy Inconel 718. Using a rotary friction welding machine and employing alloy 718 consumable rods in solution treated condition, cylindrical-shaped multi-layer friction deposits (10 mm diameter) were successfully produced. In the as-deposited condition, the deposits showed very fine grain size with no grain boundary δ phase. The deposits responded well to direct aging and showed satisfactory room-temperature tensile properties. However, their stress rupture performance was unsatisfactory because of their layered microstructure with very fine grain size and no grain boundary δ phase. The problem was overcome by heat treating the deposits first at 1353 K (1080 °C) (for increasing the grain size) and then at 1223 K (950 °C) (for precipitating the δ phase). Overall, the current study shows that Friction Freeform Fabrication is a very useful process for additive part fabrication in alloy 718.

Comparison between diffraction contrast tomography and high-energy diffraction microscopy on a slightly deformed aluminium alloy.

PubMed

Renversade, Loïc; Quey, Romain; Ludwig, Wolfgang; Menasche, David; Maddali, Siddharth; Suter, Robert M; Borbély, András

2016-01-01

The grain structure of an Al-0.3 wt%Mn alloy deformed to 1% strain was reconstructed using diffraction contrast tomography (DCT) and high-energy diffraction microscopy (HEDM). 14 equally spaced HEDM layers were acquired and their exact location within the DCT volume was determined using a generic algorithm minimizing a function of the local disorientations between the two data sets. The microstructures were then compared in terms of the mean crystal orientations and shapes of the grains. The comparison shows that DCT can detect subgrain boundaries with disorientations as low as 1° and that HEDM and DCT grain boundaries are on average 4 µm apart from each other. The results are important for studies targeting the determination of grain volume. For the case of a polycrystal with an average grain size of about 100 µm, a relative deviation of about ≤10% was found between the two techniques.

The Influence of Grain Boundary Fluids on the Recrystallization Behavior in Calcite: A Comparison of "dry" and "wet" Marble Mylonites

NASA Astrophysics Data System (ADS)

Schenk, O.; Urai, J.; Evans, B.

2003-12-01

Carbonate rocks are able to accumulate large amounts of strain and deform crystal-plastically even at low p-T conditions and thus, marble sequences are often the site of strain localization in the upper crust during late-stage deformation in mountain building processes. In this study we sought to identify the effect of fluids on grain boundary morphology and recrystallization processes in marble mylonites during shear zone evolution, as fluids play a major role in the flow behavior of many rock materials during deformation (e.g. quartz, olivine, halite, feldspar). We compared calcite marble mylonites from two geological settings: (a) Schneeberg Complex, Southern Tyrole, Italy and (b) Naxos Metamorphic Core Complex, Greece. The shear zones of the selected areas are suitable for comparison, because they consist of similar lithology and the marble mylonites resemble each other in chemical composition. In addition, calcite-dolomite solvus geothermometry and TEM observations indicate similar p-T conditions for the shear zones formation. However, the two settings are different in the availability of fluids during the shear zone evolution: In the Schneeberg mylonites, both the alteration of minerals during retrograde metamorphism of neighboring micaschists and the existence of veins suggest that fluids were present during mylonitization. The absence of these features in the Naxos samples indicates that fluids were not present during deformation of these mylonites. This difference is also supported by the signature of stable isotopes. Microstructural investigations using optical and scanning electron microscopes on broken and planar surfaces did not indicate major differences between wet and dry mylonites: Grain boundaries of both types of samples display pores with shapes controlled by crystallography, and pore morphologies that are similar to observations from crack and grain-boundary healing experiments. Grain size reduction was predominantly the result of subgrain rotation recrystallization. However, the coarse grains inside the wet protomylonites (Schneeberg) are characterized by intracrystalline shear zones. With the exception of the intracrystalline shear zones, there were no obvious microstructural signatures that were obvious indicators of the presence of fluids, at least for these two field examples.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ning, Yongquan, E-mail: luckyning@nwpu.edu.cn; Huang, Shibo; Fu, M.W.

Microstructural characterization, formation mechanism and fracture behavior of the needle δ phase in Fe–Ni–Cr type superalloys with high Nb content (GH4169, equivalent to Inconel 718) have been quantitatively investigated in this research. The typical microstructures of δ phases with the stick, mixed and needle shapes obviously present in Inconel 718 after the isothermal upsetting at the temperature of 980–1060 °C with the initial strain rate of 10{sup −3}–10{sup −1} s{sup −1}. It is found that the shape of the δ phase has a great effect on the mechanical properties of the alloy, viz., the stick δ phase behaves good plasticitymore » and the needle δ phase has good strength. In addition, the needle δ phase can be used to control the grain size as it can prevent grain growth. The combined effect of the localized necking and microvoid coalescence leads to the final ductile fracture of the GH4169 components with the needle δ phase. Both dislocation motion and atom diffusion are the root-cause for the needle δ phase to be firstly separated at grain boundary and then at sub-boundary. The formation mechanism of the needle δ phase is the new finding in this research. Furthermore, it is the primary mechanism for controlling the needle δ phase in Fe–Ni–Cr type superalloys with high Nb content. - Highlights: • Shape of the δ phase takes great effect on mechanical property. • Needle δ phase plays a great role to prevent grain growth. • Needle δ phase can enhance the fracture strength. • Microstructure mechanism of the needle δ phase has been investigated. • Fracture behavior of the needle δ phase has been studied.« less

Microstructural stability and thermomechanical processing of boron modified beta titanium alloys

NASA Astrophysics Data System (ADS)

Cherukuri, Balakrishna

One of the main objectives during primary processing of titanium alloys is to reduce the prior beta grain size. Producing an ingot with smaller prior beta grain size could potentially eliminate some primary processing steps and thus reduce processing cost. Trace additions of boron have been shown to decrease the as-cast grain size in alpha + beta titanium alloys. The primary focus of this dissertation is to investigate the effect of boron on microstructural stability and thermomechanical processing in beta titanium alloys. Two metastable beta titanium alloys: Ti-15Mo-2.6Nb-3Al-0.2Si (Beta21S) and Ti-5Al-5V-5Mo-3Cr (Ti5553) with 0.1 wt% B and without boron additions were used in this investigation. Significant grain refinement of the as-cast microstructure and precipitation of TiB whiskers along the grain boundaries was observed with boron additions. Beta21S and Beta21S-0.1B alloys were annealed above the beta transus temperature for different times to investigate the effect of boron on grain size stability. The TiB precipitates were very effective in restricting the beta grain boundary mobility by Zener pinning. A model has been developed to predict the maximum grain size as a function of TiB size, orientation, and volume fraction. Good agreement was obtained between model predictions and experimental results. Beta21S alloys were solution treated and aged for different times at several temperatures below the beta transus to study the kinetics of alpha precipitation. Though the TiB phase did not provide any additional nucleation sites for alpha precipitation, the grain refinement obtained by boron additions resulted in accelerated aging. An investigation of the thermomechanical processing behavior showed different deformation mechanisms above the beta transus temperature. The non-boron containing alloys showed a non-uniform and fine recrystallized necklace structure at grain boundaries whereas uniform intragranular recrystallization was observed in boron containing alloys. Micro-voids were observed at the ends of the TiB needles at high temperature, slow strain rates as a result of decohesion at the TiB/matrix interfaces. At low temperatures and faster strain rates micro voids were also formed due to fracture of TiB needles. Finite element analysis on void formation in TiB containing alloys were in agreement with experimental observations. Microhardness and tensile testing of as-cast + forged and aged Beta21S and Ti5553 alloys with and without boron did not show any significant differences in mechanical properties. The primary benefits of boron modified alloys are in as-cast condition.

Microstructure and Dielectric Properties of LPCVD/CVI-SiBCN Ceramics Annealed at Different Temperatures

PubMed Central

Li, Jianping; Zhao, Mingxi; Liu, Yongsheng; Chai, Nan; Ye, Fang; Qin, Hailong; Cheng, Laifei; Zhang, Litong

2017-01-01

SiBCN ceramics were introduced into porous Si3N4 ceramics via a low-pressure chemical vapor deposition and infiltration (LPCVD/CVI) technique, and then the composite ceramics were heat-treated from 1400 °C to 1700 °C in a N2 atmosphere. The effects of annealing temperatures on microstructure, phase evolution, dielectric properties of SiBCN ceramics were investigated. The results revealed that α-Si3N4 and free carbon were separated below 1700 °C, and then SiC grains formed in the SiBCN ceramic matrix after annealing at 1700 °C through a phase-reaction between free carbon and α-Si3N4. The average dielectric loss of composites increased from 0 to 0.03 due to the formation of dispersive SiC grains and the increase of grain boundaries. PMID:28773015

Effect of microstructure on the corrosion of CVD-SiC exposed to supercritical water

NASA Astrophysics Data System (ADS)

Tan, L.; Allen, T. R.; Barringer, E.

2009-10-01

Silicon carbide (SiC) is an important engineering material being studied for potential use in multiple nuclear energy systems including high-temperature gas-cooled reactors and water-cooled reactors. The corrosion behavior of SiC exposed to supercritical water (SCW) is critical for examining its applications in nuclear reactors. Although the hydrothermal corrosion of SiC has been the subject of many investigations, the study on the microstructural effects on the corrosion is limited. This paper presents the effect of residual strain, grain size, grain boundary types, and surface orientations on the corrosion of chemical vapor deposited (CVD) β-SiC exposed to SCW at 500 °C and 25 MPa. Weight loss occurred on all the samples due to localized corrosion. Residual strains associated with small grains showed the most significant effect on the corrosion compared to the other factors.

Microstructural Analysis of Severe Plastic Deformed Twin Roll Cast AZ31 for the Optimization of Superplastic Properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Young, John P.; Askari, Hesam A.; Heiden, Michael J.

2013-07-08

In recent years magnesium alloys have attracted significant attention as potential candidates to replace many of the heavier metals used in some automotive applications. However, the limited formability of magnesium and its alloys at room temperature has driven interest in the superplastic forming magnesium as an alternative shaping method. Severe plastic deformation techniques have become a well studied method of refining the grain size and modifying the microstructural characteristics of many magnesium alloys to achieve greater superplastic properties. In this study twin roll cast (TRC) AZ31 magnesium alloy was subjected to equal channel angular pressing (ECAP) and friction stir weldingmore » (FSW). The influence of these severe plastic deformation processes on the grain size, texture and grain boundary character distribution was investigated to identify the optimum severe plastic deformation process for the superplastic forming of AZ31.« less

Theoretical modeling of cellular and dendritic solidification microstructures

NASA Astrophysics Data System (ADS)

Song, Younggil

In this dissertation, we use three-dimensional (3D) phase-field (PF) modeling to investigate (i) 3D solid-liquid interface dynamics observed in microgravity experiments, and (ii) array patterns in a thin-sample geometry. In addition, using the two-dimensional (2D) dendritic-needle-network (DNN) model, we explore (iii) secondary sidebranching dynamics. Recently, solidification experiments are carried out in the DSI (Directional Solidification Insert) of the DECLIC (Device for the study of Critical LIquids and Crystallization) facility aboard the International Space Station (ISS). Thus, the directional solidification experiments are achieved under limited convective currents, and the experimental observations reveal unique dynamics of 3D microstructure in a purely diffusive growth regime. In this directional solidification setup, a temperature field between heat sources could evolve due to two main factors: (i) heat transfer within an adiabatic zone and (ii) latent heat rejection at the interface. These two thermal effects are phenomenologically characterized using a time-dependent thermal shift. In addition, we could quantitatively account for these thermal factors using a numerical calculation of the evolution of temperature field. We introduce these phenomenological and quantitative thermal representations into the PF model. The performed simulations using different thermal descriptions are compared to the experimental measurements from the initial planar interface dynamics to the final spacing selection. The DECLIC-DSI experimental observations exhibit complex grain boundary (GB) dynamics between large grains with a small misorientation. In the observations, several large grains with a small misorientation with respect to the temperature gradient are formed during solidification. Specifically, at a convergent GB, a localized group of misoriented cells penetrates into a nearby grain, which yields the morphological instability of grain boundaries. Remarkably, while the invasion process starts with a group of cells, the leader cell can detach itself from the group and grow continuously as a misoriented solitary cell in the other grain with a different misorientation. We use PF simulations to investigate the GB morphology and dynamics of a solitary cell. Solidification experiments on earth are typically performed in a thin-sample geometry to avoid fluid convection. Thus, we consider various influences on cellular and dendritic array patterns in thin samples. First, we explore the influence of crystal orientation. When a grain in a thin-sample geometry is misoriented with respect to the temperature gradient, primary cells and dendrites drift laterally in both experiments and simulations. At the same time, grain boundaries are systematically formed at the edges of the misoriented grain. The misoriented primary branches move away from the divergent grain boundary. At this boundary, cells/dendrites are generated continuously, and their spacings are larger than the dynamically selected spacings. Primary branches run into the other convergent GB, which leads to their elimination. Thus, at a stationary state, a spacing distribution is uniform with the spacing selected at the divergent GB until it decreases near the convergent GB. We perform simulations to illustrate the global evolutions of a primary spacing. In addition, we suggest a simple geometrical model and a nonlinear advection equation for the dynamics of the primary spacing evolution, which can predict the slow evolution of a primary spacing in a quasi-2D array. Experimental observations point out that the primary spacing selection could be affected by the sample thickness; however, the detailed description for the link between the primary spacing selection and a sample thickness is still missing. Here, we use PF simulations to investigate the primary cellular and dendritic spacing selection mechanisms under the influence of a sample thickness. A thin-sample geometry can limit thermal and solutal convective currents effectively. However, as the sample thickness increases, the convective currents can influence the solid- liquid interface dynamics. Then, the microstructure selection mechanisms can be different from the classical theories that are valid in a diffusive regime. We propose a simple approach for the PF model to demonstrate the microstructure selection when liquid convection is present. These simulations are compared to experimental results. Columnar microstructures with cells and dendrites typically form polycrystalline materials during directional solidification. Then, convergent and divergent grain boundaries form systematically between grains, which are misoriented with respect to the temperature gradient. Moreover, the GB is dynamically selected during the competition between two nearby misoriented grains. In order to investigate the GB orientation selection, we carry out 3D PF simulations in a thin-sample geometry. These simulations reveal the influence of the 3D GB bi-crystallography on grain competition. The results highlight the importance of considering the orientation of the orthogonal planes containing secondary branches in addition to the growth direction of primary branches. Finally, we propose three growth steps to demonstrate the secondary sidebranching growth dynamics under isothermal dendritic growth condition. (Abstract shortened by ProQuest.).

Evaluation of microstructure stability at the interfaces of Al-6061 welds fabricated using ultrasonic additive manufacturing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sridharan, Niyanth S.; Gussev, Maxim N.; Parish, Chad M.

Here, ultrasonic additive manufacturing (UAM) is a solid-state additive manufacturing process that uses fundamental principles of ultrasonic welding and sequential layering of tapes to fabricate complex three-dimensional (3-D) components. One of the factors limiting the use of this technology is the poor tensile strength along the z-axis. Recent work has demonstrated the improvement of the z-axis properties after post-processing treatments. The abnormally high stability of the grains at the interface during post-weld heat treatments is, however, not yet well understood. In this work we use multiscale characterization to understand the stability of the grains during post-weld heat treatments. Aluminum alloymore » (6061) builds, fabricated using ultrasonic additive manufacturing, were post-weld heat treated at 180, 330 and 580 °C. The grains close to the tape interfaces are stable during post-weld heat treatments at high temperatures (i.e., 580 °C). This is in contrast to rapid grain growth that takes place in the bulk. Transmission electron microscopy and atom-probe tomography display a significant enrichment of oxygen and magnesium near the stable interfaces. Based on the detailed characterization, two mechanisms are proposed and evaluated: nonequilibrium nano-dispersed oxides impeding the grain growth due to grain boundary pinning, or grain boundary segregation of magnesium and oxygen reducing the grain boundary energy.« less

Evaluation of microstructure stability at the interfaces of Al-6061 welds fabricated using ultrasonic additive manufacturing

DOE PAGES

Sridharan, Niyanth S.; Gussev, Maxim N.; Parish, Chad M.; ...

2018-03-06

Here, ultrasonic additive manufacturing (UAM) is a solid-state additive manufacturing process that uses fundamental principles of ultrasonic welding and sequential layering of tapes to fabricate complex three-dimensional (3-D) components. One of the factors limiting the use of this technology is the poor tensile strength along the z-axis. Recent work has demonstrated the improvement of the z-axis properties after post-processing treatments. The abnormally high stability of the grains at the interface during post-weld heat treatments is, however, not yet well understood. In this work we use multiscale characterization to understand the stability of the grains during post-weld heat treatments. Aluminum alloymore » (6061) builds, fabricated using ultrasonic additive manufacturing, were post-weld heat treated at 180, 330 and 580 °C. The grains close to the tape interfaces are stable during post-weld heat treatments at high temperatures (i.e., 580 °C). This is in contrast to rapid grain growth that takes place in the bulk. Transmission electron microscopy and atom-probe tomography display a significant enrichment of oxygen and magnesium near the stable interfaces. Based on the detailed characterization, two mechanisms are proposed and evaluated: nonequilibrium nano-dispersed oxides impeding the grain growth due to grain boundary pinning, or grain boundary segregation of magnesium and oxygen reducing the grain boundary energy.« less

Spark plasma sintering of ceramic matrix composite based on alumina, reinforced by carbon nanotubes

NASA Astrophysics Data System (ADS)

Leonov, A. A.; Khasanov, A. O.; Danchenko, V. A.; Khasanov, O. L.

2017-12-01

Alumina composites reinforced with 3 vol.% multi-walled carbon nanotubes (MWCNTs) were prepared by spark plasma sintering (SPS). The influence of sintering temperature (1400-1600 °C) on the composites microstructure and mechanical properties was investigated. Microstructure observations of the composite shows that some CNTs site along alumina grains boundary, while others embed into the alumina grains and shows that CNTs bonded strongly with the alumina matrix contributing to fracture toughness and microhardness increase. MWCNTs reinforcing mechanisms including CNT pull-out and crack deflection were directly observed by scanning electron microscope (SEM). For Al2O3/CNT composite sintered at 1600 °C, fracture toughness and microhardness are 4.93 MPa·m1/2 and 23.26 GPa respectively.

Investigation on microstructure characterization and property of rapidly solidified Mg-Zn-Ca-Ce-La alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhou Tao, E-mail: tzhou1118@163.com; Chen Zhenhua, E-mail: chenzhenhua45@hotmail.com; Yang Mingbo, E-mail: yangmingbo@cqit.edu.cn

2012-01-15

Rapidly solidified (RS) Mg-Zn-Ca-Ce-La (wt.%) alloys have been produced via atomizing the alloy melt and subsequent splat-quenching on the water-cooled copper twin-rollers in the form of flakes. Microstructure characterization, phase compositions and thermal stability of the alloys have been systematically investigated. The results showed that with addition of RE (Ce and La) to the Mg-6Zn-5Ca alloy, the stable intermetallic compounds i.e. the Mg{sub x}Zn{sub y}RE{sub z} phase with a few Ca (about 3 at.%), shortened as the T Prime phase, were formed at the expense of the binary Mg-Zn and Ca{sub 2}Mg{sub 6}Zn{sub 3} phases, which was possibly beneficial tomore » the enhanced thermal stability of the alloy. In the Mg-6Zn-5Ca-3Ce-0.5La alloy, the composition of the T Prime phase in the grain interior was different from that at the grain boundaries, in which the segregation of the La elements was found, and the atomic percentage ratio of Zn to Ce in the T Prime phase within the grains was close to 2. Moreover, the stable Mg{sub 2}Ca phases were detected around the T Prime phases at the grain boundaries in the alloy. - Research Highlights: Black-Right-Pointing-Pointer The phase constitution of RS Mg-6Zn-5Ca alloy can be improved by RE additions. Black-Right-Pointing-Pointer In the Mg-Zn-Ca-Ce-La alloys, the Mg{sub x}Zn{sub y}RE{sub z} phase with a few Ca (T Prime phase) is formed. Black-Right-Pointing-Pointer The formation of the T Prime phase leads to the loss of the Mg-Zn and Ca{sub 2}Mg{sub 6}Zn{sub 3} phases. Black-Right-Pointing-Pointer The composition of the T Prime phase differs from the grain interior to the grain boundary.« less

Metallurgical Mechanisms Controlling Mechanical Properties of Aluminum Alloy 2219 Produced by Electron Beam Freeform Fabrication

NASA Technical Reports Server (NTRS)

Domack, Marcia S.; Tainger, Karen M.

2006-01-01

The electron beam freeform fabrication (EBF3) layer-additive manufacturing process has been developed to directly fabricate complex geometry components. EBF3 introduces metal wire into a molten pool created on the surface of a substrate by a focused electron beam. Part geometry is achieved by translating the substrate with respect to the beam to build the part one layer at a time. Tensile properties demonstrated for electron beam deposited aluminum and titanium alloys are comparable to wrought products, although the microstructures of the deposits exhibit cast features. Understanding the metallurgical mechanisms controlling mechanical properties is essential to maximizing application of the EBF3 process. Tensile mechanical properties and microstructures were examined for aluminum alloy 2219 fabricated over a range of EBF3 process variables. Unique microstructures were observed within the deposited layers and at interlayer boundaries, which varied within the deposit height due to microstructural evolution associated with the complex thermal history experienced during subsequent layer deposition. Microstructures exhibited irregularly shaped grains with interior dendritic structures, described based on overall grain size, morphology, distribution, and dendrite spacing, and were correlated with deposition parameters. Fracture features were compared with microstructural elements to define fracture paths and aid in definition of basic processing-microstructure-property correlations.

Dynamic Recrystallization Behavior and Corrosion Resistance of a Dual-Phase Mg-Li Alloy

PubMed Central

Liu, Gang; Xie, Wen; Wei, Guobing; Yang, Yan; Liu, Junwei; Xu, Tiancai; Xie, Weidong; Peng, Xiaodong

2018-01-01

The hot deformation and dynamic recrystallization behavior of the dual-phase Mg-9Li-3Al-2Sr-2Y alloy had been investigated using a compression test. The typical dual-phase structure was observed, and average of grain size of as-homogenized alloy is about 110 µm. It mainly contains β-Li, α-Mg, Al4Sr and Al2Y phases. The dynamic recrystallization (DRX) kinetic was established based on an Avrami type equation. The onset of the DRX process occurred before the peak of the stress–strain flow curves. It shows that the DRX volume fraction increases with increasing deformation temperature or decreasing strain rate. The microstructure evolution during the hot compression at various temperatures and strain rates had been investigated. The DRX grain size became larger with the increasing testing temperature or decreasing strain rate because the higher temperature or lower strain rate can improve the migration of DRX grain boundaries. The fully recrystallized microstructure can be achieved in a small strain due to the dispersed island-shape α-Mg phases, continuous the Al4Sr phases and spheroidal Al2Y particles, which can accelerate the nucleation. The continuous Al4Sr phases along the grain boundaries are very helpful for enhancing the corrosion resistance of the duplex structured Mg-Li alloy, which can prevent the pitting corrosion and filiform corrosion. PMID:29522473

Dynamic Recrystallization Behavior and Corrosion Resistance of a Dual-Phase Mg-Li Alloy.

PubMed

Liu, Gang; Xie, Wen; Wei, Guobing; Yang, Yan; Liu, Junwei; Xu, Tiancai; Xie, Weidong; Peng, Xiaodong

2018-03-09

The hot deformation and dynamic recrystallization behavior of the dual-phase Mg-9Li-3Al-2Sr-2Y alloy had been investigated using a compression test. The typical dual-phase structure was observed, and average of grain size of as-homogenized alloy is about 110 µm. It mainly contains β-Li, α-Mg, Al₄Sr and Al₂Y phases. The dynamic recrystallization (DRX) kinetic was established based on an Avrami type equation. The onset of the DRX process occurred before the peak of the stress-strain flow curves. It shows that the DRX volume fraction increases with increasing deformation temperature or decreasing strain rate. The microstructure evolution during the hot compression at various temperatures and strain rates had been investigated. The DRX grain size became larger with the increasing testing temperature or decreasing strain rate because the higher temperature or lower strain rate can improve the migration of DRX grain boundaries. The fully recrystallized microstructure can be achieved in a small strain due to the dispersed island-shape α-Mg phases, continuous the Al₄Sr phases and spheroidal Al₂Y particles, which can accelerate the nucleation. The continuous Al₄Sr phases along the grain boundaries are very helpful for enhancing the corrosion resistance of the duplex structured Mg-Li alloy, which can prevent the pitting corrosion and filiform corrosion.

Investigation of mechanical and microstructural properties of Zircaloy-4 under different experimental conditions

DOE PAGES

Silva, Chinthaka M.; Leonard, Keith J.; Van Abel, Eric; ...

2017-12-09

Here two types of Zircaloy-4 (alpha-annealed and beta-quenched) were investigated in their different forms. It was found that mechanical properties of Zircaloy-4 are affected significantly by welding and hydrogen-charging followed by neutron irradiation. Evaluation of microstructural properties of samples showed that these changes are mainly due to the formation of secondary phases such as hydrides—mostly along grain boundaries, dislocation channeling and their disruptions, and the increase in the type dislocation loops.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jana, S.; Devaraj, A.; Kovarik, L.

Transformation kinetics of metastable body-centered cubic γ-UMo phase in U-10 wt.percent Mo alloy during annealing at sub-eutectoid temperatures of 500C and 400C has been determined as a function of time using detailed microstructural characterization by scanning electron microscopy, X-ray diffraction analysis, scanning transmission electron microscopy, and atom probe tomography. Based on the results, we found that the phase transformation is initiated by cellular transformation at both the temperatures, which results in formation of a lamellar microstructure along prior γ-UMo grain boundaries.

Investigation of mechanical and microstructural properties of Zircaloy-4 under different experimental conditions

NASA Astrophysics Data System (ADS)

Silva, Chinthaka M.; Leonard, Keith J.; Van Abel, Eric; Geringer, J. Wilna; Bryan, Chris D.

2018-02-01

Two types of Zircaloy-4 (alpha-annealed and beta-quenched) were investigated in their different forms. It was found that mechanical properties of Zircaloy-4 are affected significantly by welding and hydrogen-charging followed by neutron irradiation. Evaluation of microstructural properties of samples showed that these changes are mainly due to the formation of secondary phases such as hydrides-mostly along grain boundaries, dislocation channeling and their disruptions, and the increase in the type dislocation loops.

Microscale mechanical characterization of materials for extreme environments

NASA Astrophysics Data System (ADS)

Ozerinc, Sezer

Nanocrystalline metals are promising materials for applications that require outstanding strength and stability in extreme environments. Further improvements in the desirable mechanical properties of these materials require a better understanding of the relationship between their microstructure and grain boundary deformation behavior. Previous molecular dynamics simulations suggested that solute additions to grain boundaries can enhance the strength of nanocrystalline metals, but there has been a lack of experimental studies investigating this prediction. This dissertation presents mechanical and microstructural characterization of nanocrystalline Cu alloys and demonstrate that addition of Nb solutes to grain boundaries greatly enhances the strength of Cu. The measured hardness of Cu90Nb10 alloy is 5.6 GPa which is more than double the hardness of nanocrystalline pure Cu. Microstructural characterization through transmission electron microscopy and energy-dispersive X-ray spectroscopy on these alloys indicates a strong correlation between the grain boundary composition and the hardness. Variation of measured hardness with measured grain boundary composition is in very good agreement with previous molecular dynamics simulation predictions. The results of this work provide experimental evidence that grain boundary doping enhances the strength of nanocrystalline Cu far beyond that predicted by classical Hall-Petch strengthening and decreasing grain boundary energy through solute additions is the key to reaching theoretical strength in nanocrystalline metals. Irradiation induced creep is a deformation mechanism that takes place under combined stress and particle bombardment. Effective characterization of this phenomenon on nanostructured materials is crucial for the assessment of their potential use in next generation nuclear power plants. Direct measurements of irradiation induced creep under MeV-heavy ion bombardment have not been feasible until recently due to the requirements of micron-sized specimens, muN-level force sensitivity, and nm-level displacement sensitivity. A recently developed mechanical characterization technique, micropillar compression, has enabled the testing of miniaturized specimens; however, there has been no demonstration of the application of this technique to irradiation induced creep measurements. This dissertation presents the development of an in situ measurement apparatus for compression testing of micron-sized cylindrical specimens under MeV-heavy ion bombardment. The apparatus has a force resolution of 1 muN and a displacement resolution of 1 nm. The apparatus measured irradiation induced creep in four different amorphous materials and the findings clarified the significance of different creep mechanisms in these materials. In amorphous metals and amorphous Si, the measured irradiation induced fluidity is ≈ 3 dpa-1GPa-1 (dpa: displacements per atom). The measured fluidity is in excellent agreement with previous molecular dynamics simulation predictions, providing experimental evidence for point defect mediated plastic flow under ion bombardment. For amorphous SiO2, stress relaxation through thermal spikes further contribute to the creep response, resulting in higher fluidities up to ≈ 83 dpa-1GPa -1. Finally, this dissertation presents the further development of the creep testing apparatus for high temperature measurements. The apparatus demonstrated good thermal and mechanical stability and measured irradiation induced creep of nanocrystalline Cu at 200°C. Resulting irradiation induced fluidity is ≈ 10% of the fluidity of the amorphous metals, in agreement with previous measurements on free-standing films. Understanding the creep behavior of nanostructured metals under heavy ion bombardment at elevated temperatures is important for identifying the governing creep mechanisms in these materials. The developed apparatus provides a new and effective method of accelerated mechanical characterization of such promising materials for their potential use in future nuclear applications.

3D additive manufactured 316L components microstructural features and changes induced by working life cycles

NASA Astrophysics Data System (ADS)

Pace, M. L.; Guarnaccio, A.; Dolce, P.; Mollica, D.; Parisi, G. P.; Lettino, A.; Medici, L.; Summa, V.; Ciancio, R.; Santagata, A.

2017-10-01

The ability of processing through laser beams different kinds of metallic powders for direct production of 3D components with complex geometries has been gaining an impressive and growing attention for specific industrial applications. The process which can be distinguished as Selective Laser Sintering or Selective Laser Melting is even considered, more generally, as Additive Manufacturing where layer by layer material is built by the interaction between a laser beam and a powder bed. The rapid heating of the powder due to the laser beam energy transfer process followed by a rapid cooling rate induces within the manufactured material a cellular structure with fine sub-grains, which are in the range of few hundreds of micrometers. These metastable structures, which are smaller than the grain size in conventionally manufactured 316L stainless steel components, can undertake towards a recrystallization process due to either heat or mechanical treatments. For instance, when sub-grain boundaries of the cells are enriched with Mo and higher concentration of dislocation, dynamical processes occur generating local residual stresses. In these circumstances the segregation of Mo in cell boundaries is out of thermodynamic equilibrium conditions so that microstructures and phases are metastable. In the range of 1100-1400 °C heat treatments a complete dissolution of Mo in the Fe matrix with a gradual disappearance of sub-microns cell is observed feeding the growth of larger austenitic sub-grains formation. It follows a higher degree of Mo dissolution in the material matrix and a decrease of dislocation's concentration (Saeidi et al., 2015) [1]. In the work here presented we point out which are the microstructural features of stainless steel 316L components realized by Additive Manufacturing. Furthermore, the occurrence of a microstructural evolution is presented after experiencing to fatigue of 80000 cycles some door joints obtained by this technique. A decrease of dislocation's number, an increase of twinning due to the growth of grains and to the release of local stresses can be hypothesized following that an important role could be played by the presence of dislocations in cell boundaries as well as oxides nano-inclusion formed in-situ during the Additive Manufacturing process (Saeidi et al., 2015) [2]. From these outcomes it is going to be presented how the 3D components produced by Additive Manufacturing could change and improve their features for potential industrial applications during life cycles and enhance such a behavior by taking carefully into account the laser parameters and its scanning speed.

A Model for Predicting Grain Boundary Cracking in Polycrystalline Viscoplastic Materials Including Scale Effects

DOE Office of Scientific and Technical Information (OSTI.GOV)

Allen, D.H.; Helms, K.L.E.; Hurtado, L.D.

1999-04-06

A model is developed herein for predicting the mechanical response of inelastic crystalline solids. Particular emphasis is given to the development of microstructural damage along grain boundaries, and the interaction of this damage with intragranular inelasticity caused by dislocation dissipation mechanisms. The model is developed within the concepts of continuum mechanics, with special emphasis on the development of internal boundaries in the continuum by utilizing a cohesive zone model based on fracture mechanics. In addition, the crystalline grains are assumed to be characterized by nonlinear viscoplastic mechanical material behavior in order to account for dislocation generation and migration. Due tomore » the nonlinearities introduced by the crack growth and viscoplastic constitution, a numerical algorithm is utilized to solve representative problems. Implementation of the model to a finite element computational algorithm is therefore briefly described. Finally, sample calculations are presented for a polycrystalline titanium alloy with particular focus on effects of scale on the predicted response.« less

Modeling and Studying the Effect of Texture and Elastic Anisotropy of Copper Microstructure in Nanoscale Interconnects on Reliability in Integrated Circuits

NASA Astrophysics Data System (ADS)

Basavalingappa, Adarsh

Copper interconnects are typically polycrystalline and follow a lognormal grain size distribution. Polycrystalline copper interconnect microstructures with a lognormal grain size distribution were obtained with a Voronoi tessellation approach. The interconnect structures thus obtained were used to study grain growth mechanisms, grain boundary scattering, scattering dependent resistance of interconnects, stress evolution, vacancy migration, reliability life times, impact of orientation dependent anisotropy on various mechanisms, etc. In this work, the microstructures were used to study the impact of microstructure and elastic anisotropy of copper on thermal and electromigration induced failure. A test structure with copper and bulk moduli values was modeled to do a comparative study with the test structures with textured microstructure and elastic anisotropy. By subjecting the modeled test structure to a thermal stress by ramping temperature down from 400 °C to 100 °C, a significant variation in normal stresses and pressure were observed at the grain boundaries. This variation in normal stresses and hydrostatic stresses at the grain boundaries was found to be dependent on the orientation, dimensions, surroundings, and location of the grains. This may introduce new weak points within the metal line where normal stresses can be very high depending on the orientation of the grains leading to delamination and accumulation sites for vacancies. Further, the hydrostatic stress gradients act as a driving force for vacancy migration. The normal stresses can exceed certain grain orientation dependent critical threshold values and induce delamination at the copper and cap material interface, thereby leading to void nucleation and growth. Modeled test structures were subjected to a series of copper depositions at 250 °C followed by copper etch at 25 °C to obtain initial stress conditions. Then the modeled test structures were subjected to 100,000 hours ( 11.4 years) of simulated thermal stress at an elevated temperature of 150 °C. Vacancy migration due to concentration gradients, thermal gradients, and mechanical stress gradients were considered under the applied thermal stress. As a result, relatively high concentrations of vacancies were observed in the test structure due to a driving force caused by the pressure gradients resulting from the elastic anisotropy of copper. The grain growth mechanism was not considered in these simulations. Studies with two grain analysis demonstrated that the stress gradients developed will be severe when (100) grains are adjacent to (111) grains, therefore making them the weak points for potentially reliability failures. Ilan Blech discovered that electromigration occurs above a critical product of the current density and metal length, commonly referred as Blech condition. Electromigration stress simulations in this work were carried out by subjecting test structures to scaled current densities to overcome the Blech condition of (jL)crit for small dimensions of test structure and the low temperature stress condition used. Vacancy migration under the electromigration stress conditions was considered along with the vacancy migration induced stress evolution. A simple void growth model was used which assumes voids start to form when vacancies reach a critical level. Increase of vacancies in a localized region increases the resistance of the metal line. Considering a 10% increase in resistance as a failure criterion, the distributions of failure times were obtained for given electromigration stress conditions. Bimodal/multimodal failure distributions were obtained as a result. The sigma values were slightly lower than the ones commonly observed from experiments. The anisotropy of the elastic moduli of copper leads to the development of significantly different stress values which are dependent on the orientation of the grains. This results in some grains having higher normal stress than the others. This grain orientation dependent normal stress can reach a critical stress necessary to induce delamination at the copper and cap interface. Time taken to reach critical stress was considered as time to fail and distributions of failure times were obtained for structures with different grain orientations in the microstructure for different critical stress values. The sigma values of the failure distributions thus obtained for different constant critical stress values had a strong dependence of on the critical stress. It is therefore critical to use the appropriate critical stress value for the delamination of copper and cap interface. The critical stress necessary to overcome the local adhesion of the copper and the cap material interface is dependent on grain orientation of the copper. Simulations were carried out by considering grain orientation dependent critical normal stress values as failure criteria. The sigma value thus obtained with selected critical stress values were comparable to sigma values commonly observed from experiments.

A Multiscale Computational Model Combining a Single Crystal Plasticity Constitutive Model with the Generalized Method of Cells (GMC) for Metallic Polycrystals.

PubMed

Ghorbani Moghaddam, Masoud; Achuthan, Ajit; Bednarcyk, Brett A; Arnold, Steven M; Pineda, Evan J

2016-05-04

A multiscale computational model is developed for determining the elasto-plastic behavior of polycrystal metals by employing a single crystal plasticity constitutive model that can capture the microstructural scale stress field on a finite element analysis (FEA) framework. The generalized method of cells (GMC) micromechanics model is used for homogenizing the local field quantities. At first, the stand-alone GMC is applied for studying simple material microstructures such as a repeating unit cell (RUC) containing single grain or two grains under uniaxial loading conditions. For verification, the results obtained by the stand-alone GMC are compared to those from an analogous FEA model incorporating the same single crystal plasticity constitutive model. This verification is then extended to samples containing tens to hundreds of grains. The results demonstrate that the GMC homogenization combined with the crystal plasticity constitutive framework is a promising approach for failure analysis of structures as it allows for properly predicting the von Mises stress in the entire RUC, in an average sense, as well as in the local microstructural level, i.e. , each individual grain. Two-three orders of saving in computational cost, at the expense of some accuracy in prediction, especially in the prediction of the components of local tensor field quantities and the quantities near the grain boundaries, was obtained with GMC. Finally, the capability of the developed multiscale model linking FEA and GMC to solve real-life-sized structures is demonstrated by successfully analyzing an engine disc component and determining the microstructural scale details of the field quantities.

A Multiscale Computational Model Combining a Single Crystal Plasticity Constitutive Model with the Generalized Method of Cells (GMC) for Metallic Polycrystals

PubMed Central

Ghorbani Moghaddam, Masoud; Achuthan, Ajit; Bednarcyk, Brett A.; Arnold, Steven M.; Pineda, Evan J.

2016-01-01

A multiscale computational model is developed for determining the elasto-plastic behavior of polycrystal metals by employing a single crystal plasticity constitutive model that can capture the microstructural scale stress field on a finite element analysis (FEA) framework. The generalized method of cells (GMC) micromechanics model is used for homogenizing the local field quantities. At first, the stand-alone GMC is applied for studying simple material microstructures such as a repeating unit cell (RUC) containing single grain or two grains under uniaxial loading conditions. For verification, the results obtained by the stand-alone GMC are compared to those from an analogous FEA model incorporating the same single crystal plasticity constitutive model. This verification is then extended to samples containing tens to hundreds of grains. The results demonstrate that the GMC homogenization combined with the crystal plasticity constitutive framework is a promising approach for failure analysis of structures as it allows for properly predicting the von Mises stress in the entire RUC, in an average sense, as well as in the local microstructural level, i.e., each individual grain. Two–three orders of saving in computational cost, at the expense of some accuracy in prediction, especially in the prediction of the components of local tensor field quantities and the quantities near the grain boundaries, was obtained with GMC. Finally, the capability of the developed multiscale model linking FEA and GMC to solve real-life-sized structures is demonstrated by successfully analyzing an engine disc component and determining the microstructural scale details of the field quantities. PMID:28773458

Effects of HfB2 and HfN Additions on the Microstructures and Mechanical Properties of TiB2-Based Ceramic Tool Materials

PubMed Central

An, Jing; Song, Jinpeng; Liang, Guoxing; Gao, Jiaojiao; Xie, Juncai; Cao, Lei; Wang, Shiying; Lv, Ming

2017-01-01

The effects of HfB2 and HfN additions on the microstructures and mechanical properties of TiB2-based ceramic tool materials were investigated. The results showed that the HfB2 additive not only can inhibit the TiB2 grain growth but can also change the morphology of some TiB2 grains from bigger polygons to smaller polygons or longer ovals that are advantageous for forming a relatively fine microstructure, and that the HfN additive had a tendency toward agglomeration. The improvement of flexural strength and Vickers hardness of the TiB2-HfB2 ceramics was due to the relatively fine microstructure; the decrease of fracture toughness was ascribed to the formation of a weaker grain boundary strength due to the brittle rim phase and the poor wettability between HfB2 and Ni. The decrease of the flexural strength and Vickers hardness of the TiB2-HfN ceramics was due to the increase of defects such as TiB2 coarse grains and HfN agglomeration; the enhancement of fracture toughness was mainly attributed to the decrease of the pore number and the increase of the rim phase and TiB2 coarse grains. The toughening mechanisms of TiB2-HfB2 ceramics mainly included crack bridging and transgranular fracture, while the toughening mechanisms of TiB2-HfN ceramics mainly included crack deflection, crack bridging, transgranular fracture, and the core-rim structure. PMID:28772821

Comparative evaluation of cast aluminum alloys for automotive cylinder heads: Part I Microstructure evolution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Roy, Shibayan; Allard, Jr, Lawrence Frederick; Rodriguez, Andres

The present study stages a comparative evaluation of microstructure and associated mechanical and thermal response for common cast aluminum alloys that are used for manufacturing automotive cylinder heads. The systems considered are Al-Cu (206-T6), Al-Si-Cu (319-T7), and Al-Si (356-T6, A356-T6, and A356 + 0.5Cu-T6). The focus of the present manuscript is on the evaluation of microstructure at various length scales after aging, while the second manuscript will deal with the mechanical and thermal response of these alloys due to short-term (aging) and long-term (pre-conditioning) heat treatments. At the grain-scale, the Al-Cu alloy possessed an equiaxed microstructure as opposed to themore » dendritic structure for the Al-Si-Cu or Al-Si alloys which is related to the individual solidification conditions for these alloy systems. The composition and morphology of intermetallic precipitates within the grain and at the grain/dendritic boundary are dictated by the alloy chemistry, solidification, and heat treatment conditions. At the nanoscale, these alloys contain various metastable strengthening precipitates (GPI and θ''θ'' in Al-Cu alloy, θ'θ' in Al-Si-Cu alloy, and β'β' in Al-Si alloys) with varying size, morphology, coherency, and thermal stability.« less

Comparative evaluation of cast aluminum alloys for automotive cylinder heads: Part I Microstructure evolution

DOE PAGES

Roy, Shibayan; Allard, Jr, Lawrence Frederick; Rodriguez, Andres; ...

2017-03-06

The present study stages a comparative evaluation of microstructure and associated mechanical and thermal response for common cast aluminum alloys that are used for manufacturing automotive cylinder heads. The systems considered are Al-Cu (206-T6), Al-Si-Cu (319-T7), and Al-Si (356-T6, A356-T6, and A356 + 0.5Cu-T6). The focus of the present manuscript is on the evaluation of microstructure at various length scales after aging, while the second manuscript will deal with the mechanical and thermal response of these alloys due to short-term (aging) and long-term (pre-conditioning) heat treatments. At the grain-scale, the Al-Cu alloy possessed an equiaxed microstructure as opposed to themore » dendritic structure for the Al-Si-Cu or Al-Si alloys which is related to the individual solidification conditions for these alloy systems. The composition and morphology of intermetallic precipitates within the grain and at the grain/dendritic boundary are dictated by the alloy chemistry, solidification, and heat treatment conditions. At the nanoscale, these alloys contain various metastable strengthening precipitates (GPI and θ''θ'' in Al-Cu alloy, θ'θ' in Al-Si-Cu alloy, and β'β' in Al-Si alloys) with varying size, morphology, coherency, and thermal stability.« less

Development of re-crystallized W-1.1%TiC with enhanced room-temperature ductility and radiation performance

NASA Astrophysics Data System (ADS)

Kurishita, H.; Matsuo, S.; Arakawa, H.; Sakamoto, T.; Kobayashi, S.; Nakai, K.; Takida, T.; Kato, M.; Kawai, M.; Yoshida, N.

2010-03-01

Ultra-fine grained (UFG) W-TiC compacts fabricated by powder metallurgical methods utilizing mechanical alloying (MA) are very promising for use in irradiation environments. However, the assurance of room-temperature ductility and enhancement in surface resistances to low-energy hydrogen irradiation are unsettled issues. As an approach to solution to these, microstructural modification by hot plastic working has been applied to UFG W-TiC processed by MA in a purified Ar or H 2 atmosphere and hot isostatic pressing (HIP). Hot plastically worked compacts have been subjected to 3-point bend tests at room temperature and TEM microstructural examinations. It is found that the microstructural modification allows us to convert UFG W-1.1%TiC to compacts exhibiting a very high fracture strength and appreciable ductility at room temperature. The compacts of W-1.1%TiC/Ar (MA atmosphere: Ar) and W-1.1%TiC/H 2 (MA atmosphere: H 2) exhibit re-crystallized structures with approximately 0.5 and 1.5 μm in grain size, respectively. It is shown that the enhancement of fracture resistance by microstructural modifications is attributed to significant strengthening of weak grain boundaries in the re-crystallized state. As a result the modified compacts exhibit superior surface resistance to low-energy deuteron irradiation.

Comparative Evaluation of Cast Aluminum Alloys for Automotive Cylinder Heads: Part I—Microstructure Evolution

NASA Astrophysics Data System (ADS)

Roy, Shibayan; Allard, Lawrence F.; Rodriguez, Andres; Watkins, Thomas R.; Shyam, Amit

2017-05-01

The present study stages a comparative evaluation of microstructure and associated mechanical and thermal response for common cast aluminum alloys that are used for manufacturing automotive cylinder heads. The systems considered are Al-Cu (206-T6), Al-Si-Cu (319-T7), and Al-Si (356-T6, A356-T6, and A356 + 0.5Cu-T6). The focus of the present manuscript is on the evaluation of microstructure at various length scales after aging, while the second manuscript will deal with the mechanical and thermal response of these alloys due to short-term (aging) and long-term (pre-conditioning) heat treatments. At the grain-scale, the Al-Cu alloy possessed an equiaxed microstructure as opposed to the dendritic structure for the Al-Si-Cu or Al-Si alloys which is related to the individual solidification conditions for these alloy systems. The composition and morphology of intermetallic precipitates within the grain and at the grain/dendritic boundary are dictated by the alloy chemistry, solidification, and heat treatment conditions. At the nanoscale, these alloys contain various metastable strengthening precipitates (GPI and θ^'' in Al-Cu alloy, θ^' in Al-Si-Cu alloy, and β^' in Al-Si alloys) with varying size, morphology, coherency, and thermal stability.

Failure investigations of failed valve plug SS410 steel due to cracking

NASA Astrophysics Data System (ADS)

Kalyankar, V. D.; Deshmukh, D. D.

2017-12-01

Premature and sudden in service failure of a valve plug due to crack formation, applied in power plant has been investigated. The plug was tempered and heat treated, the crack was originated at centre, developed along the axis and propagates radially towards outer surface of plug. The expected life of the component is 10-15 years while, the component had failed just after the installation that is, within 3 months of its service. No corrosion products were observed on the crack interface and on the failed surface; hence, causes of corrosion failure are neglected. This plug of level separator control valve, is welded to the stem by means of plasma-transferred arc welding and as there is no crack observed at the welding zone, the failure due to welding residual stresses are also neglected. The failed component discloses exposed surface of a crack interface that originated from centre and propagates radially. The micro-structural observation, hardness testing, and visual observation are carried out of the specimen prepared from the failed section and base portion. The microstructure from the cracked interface showed severe carbide formation along the grain boundaries. From the microstructural analysis of the failed sample, it is observed that there is a formation of acicular carbides along the grain boundaries due to improper tempering heat treatment.

Simulated HAZ continuous cooling transformation diagram of a bogie steel of high-speed railway

NASA Astrophysics Data System (ADS)

Liu, Yue; Chen, Hui; Liu, Yan; Hang, Zongqiu

2017-07-01

Simulated HAZ continuous cooling transformation (SH-CCT) diagram presents the start and end points of phase transformation and the relationships of the microstructures of HAZ, temperature and cooling rates. It is often used to assess the weldability of materials. In this paper, a weathering steel Q345C which is widely used in the bogies manufacturing was studied. The cooling times from 800∘C to 500∘C (t8/5) were from 3 s to 6000 s, aiming to study the microstructures under different cooling rates. Different methods such as color metallography were used to obtain the metallography images. The results show that ferrite nucleates preferentially at the prior austenite grain boundaries and grows along the grain boundaries with a lath-like distribution when t8/5 is 300 s. Austenite transforms into ferrite, pearlite and bainite with decreasing t8/5. Pearlite disappears completely when t8/5 = 150 s. Martensite gradually appears when t8/5 decreases to 30 s. The hardness increases with decreasing t8/5. The SH-CCT diagram indicates that the welding input and t8/5 should be taken into consideration when welding. This work provides the relationships of welding parameters and microstructures.

Effect of sintering conditions on the electrical-transport properties of the SrZrO3-based protonic ceramic electrolyser membrane

NASA Astrophysics Data System (ADS)

Heras-Juaristi, Gemma; Pérez-Coll, Domingo; Mather, Glenn C.

2016-11-01

The effects of sintering temperature and addition of 4 mol.% ZnO as sintering additive on the crystal structure, microstructure and electrical properties of SrZr0.9Y0.1O3-δ are reported. The presence of ZnO as sintering aid brings about high densification at 1300 °C (relative density ∼97%); gas-tightness is not achieved for ZnO-free samples sintered below 1600 °C. Bulk conductivity (σB) is considerably higher in wet and dry O2 on doping with ZnO, but only slight variations of σB with sintering temperature are observed for the Zn-containing phases. Similarly, the apparent grain-boundary conductivities are much greater for the Zn-doped samples. The grain-boundary volume and accompanying resistances are much reduced on sintering at 1500 °C with ZnO addition in comparison to Zn-modified samples sintered below 1500 °C, with only minor changes in grain-boundary relaxation frequency observed. Conversely, in comparison to the undoped sample with sintering temperature of 1600 °C, there is an enormous improvement in the specific grain-boundary conductivity of two orders of magnitude for the ZnO-containing samples. Analysis on the basis of the core space-charge-layer model relates the enhancement of the grain-boundary transport to a higher concentration of charge carriers in the space-charge layer and associated lower potential barrier heights.

Microstructural Evolution of Al-1Fe (Weight Percent) Alloy During Accumulative Continuous Extrusion Forming

NASA Astrophysics Data System (ADS)

Wang, Xiang; Guan, Ren-Guo; Tie, Di; Shang, Ying-Qiu; Jin, Hong-Mei; Li, Hong-Chao

2018-04-01

As a new microstructure refining method, accumulative continuous extrusion forming (ACEF) cannot only refine metal matrix but also refine the phases that exist in it. In order to detect the refinements of grain and second phase during the process, Al-1Fe (wt pct) alloy was processed by ACEF, and the microstructural evolution was analyzed by electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). Results revealed that the average grain size of Al-1Fe (wt pct) alloy decreased from 13 to 1.2 μm, and blocky Al3Fe phase with an average length of 300 nm was granulated to Al3Fe particle with an average diameter of 200 nm, after one pass of ACEF. Refinement of grain was attributed to continuous dynamic recrystallization (CDRX), and the granulation of Al3Fe phase included the spheroidization resulting from deformation heat and the fragmentation caused by the coupling effects of strain and thermal effect. The spheroidization worked in almost the entire deformation process, while the fragmentation required strain accumulation. However, fragmentation contributed more than spheroidization. Al3Fe particle stimulated the formation of substructure and retarded the migration of recrystallized grain boundary, but the effect of Al3Fe phase on refinement of grain could only be determined by the contrastive investigation of Al-1Fe (wt pct) alloy and pure Al.

Fusion boundary microstructure evolution in aluminum alloys

NASA Astrophysics Data System (ADS)

Kostrivas, Anastasios Dimitrios

2000-10-01

A melting technique was developed to simulate the fusion boundary of aluminum alloys using the GleebleRTM thermal simulator. Using a steel sleeve to contain the aluminum, samples were heated to incremental temperatures above the solidus temperature of a number of alloys. In alloy 2195, a 4wt%Cu-1wt%Li alloy, an equiaxed non-dendritic zone (EQZ) could be formed by heating in the temperature range from approximately 630 to 640°C. At temperatures above 640°C, solidification occurred by the normal epitaxial nucleation and growth mechanism. Fusion boundary behavior was also studied in alloys 5454-H34, 6061-T6, and 2219-T8. Additionally, experimental alloy compositions were produced by making bead on plate welds using an alloy 5454-H32 base metal and 5025 or 5087 filler metals. These filler metals contain zirconium and scandium additions, respectively, and were expected to influence nucleation and growth behavior. Both as-welded and welded/heat treated (540°C and 300°C) substrates were tested by melting simulation, resulting in dendritic and EQZ structures depending on composition and substrate condition. Orientation imaging microscopy (OIM(TM)) was employed to study the crystallographic character of the microstructures produced and to verify the mechanism responsible for EQZ formation. OIM(TM) proved that grains within the EQZ have random orientation. In all other cases, where the simulated microstructures were dendritic in nature, it was shown that epitaxy was the dominant mode of nucleation. The lack of any preferred crystallographic orientation relationship in the EQZ supports a theory proposed by Lippold et al that the EQZ is the result of heterogeneous nucleation within the weld unmixed zone. EDS analysis of the 2195 on STEM revealed particles with ternary composition consisted of Zr, Cu and Al and a tetragonal type crystallographic lattice. Microdiffraction line scans on EQZ grains in the alloy 2195 showed very good agreement between the measured Cu composition within the interior of the non-dendritic grains and the corresponding value the Scheil equation predicts for the first solid to form upon solidification for a binary Al-Cu alloy with identical Cu composition. In the context of the alloys, compositions and substrate conditions examined a mechanistic model for EQZ zone formation is proposed, helpful in adjusting base metal compositions and/or substrate conditions to control fusion boundary microstructure.

Improved magnetic properties and growth anisotropy of chemically modified Sr ferrites

NASA Astrophysics Data System (ADS)

Lee, Jung W.; Cho, Yong S.; Amarakoon, Vasantha R. W.

1999-04-01

Magnetic properties and microstructural characteristics of SrOṡ5.9Fe2O3 chemically modified with Si and Ca were investigated by changing experimental parameters such as additive composition, the ratio of Ca/Si, and sintering condition. A novel particulate coating method utilizing sol-gel reactions was used to uniformly incorporate the additives of Si and Ca. This method was very successful in obtaining homogeneous grain growth and fine grains. A sample containing the gel additives of 0.6 wt % SiO2 and 0.7 wt % CaO and sintered at 1200 °C for 4 h was found to significantly suppress abnormal grain growth, resulting in submicron-sized grains and high density. A distinct grain boundary phase containing Si and Ca was observed by increasing the sintering temperature to 1250 °C. The resultant microstructural characteristics favorably affected magnetic properties. For example, the chemically modified sample exhibited a higher coercivity of 3530 Oe compared to a value of 2050 Oe obtained for the sample without the additives. On the other hand, an increase in the ratio of Ca/Si or in sintering temperature tended to induce a large anisotropy during grain growth.

Mechanical Behavior and Microcrack Development in Nominally Dry Synthetic Salt-rock During Cyclic Loading

NASA Astrophysics Data System (ADS)

Ding, J.; Chester, F. M.; Chester, J. S.; Zhu, C.; Shen, X.; Arson, C. F.

2016-12-01

Synthetic salt-rock is produced through uniaxial consolidation of sieved granular salt (0.3-0.355 mm grain diam.) at 75-107 MPa pressure and 100-200 0 C for 15 min duration, to produce low porosity (3%-6%) aggregates. Based on microstructural observations, consolidation mechanisms are grain rearrangement, intragranular plastic flow, and minor microfracture and recrystallization. Following consolidation, the salt-rock is deformed by cyclic, triaxial loading at room temperature and 4 MPa confining pressure to investigate microfracture development, closure and healing effects on elastic properties and flow strength. Load cycles are performed within the elastic regime, up to yielding, and during steady ductile flow. The mechanical properties are determined using an internal load cell and strain gages bonded to the samples. Elastic properties vary systematically during deformation reflecting cracking and pore and grain shape changes. Between triaxial load cycles, samples are held at isostatic loads for durations up to one day to determine healing rates and strength recovery; a change in mechanical behavior is observed when significant healing is induced. The microstructures of all samples are characterized before and after cyclic loading using optical microscopy. The consolidation and cyclic triaxial tests, and optical microscopy investigations, are conducted in a controlled low-humidity environment to ensure nominally dry conditions. The microstructures of samples from different stages of cyclic triaxial deformation indicate that intracrystalline plasticity, accompanied by minor recovery by recrystallization, is dominant; but, grain-boundary crack opening also becomes significant. Grain-boundary microcracks have preferred orientations that are sub-parallel to the load axis. The stress-strain behavior correlates with microcrack fabrics and densities during cyclic loading. These experiments are used to both inform and test continuum damage mechanics models of salt-rock deformation in the semibrittle domain, as well as to help design and optimize salt-rock storage facilities.

Pressure Dependence of Magnesite Flow Strength

NASA Astrophysics Data System (ADS)

Millard, J. W.; Holyoke, C. W., III; McDaniel, C.; Raterron, P.; Kronenberg, A. K.; Tokle, L.

2017-12-01

Recent experiments by Holyoke et al. (2014) indicate that magnesite is weak compared with olivine, leading to strain localization into magnesite-bearing horizons of downgoing subducting slabs, potentially leading to intermediate (200-400 km) deep focus earthquakes DFEs. Flow strengths (σ) of magnesite were determined as functions of strain rate and temperature (T), but not of pressure (P). In order to determine the pressure dependence of magnesite deforming by dislocation creep and low temperature plasticity (LTP), we performed triaxial deformation experiments on natural, coarse-grained (80 μm) magnesite aggregates at T = 900oC, strain rate of 2*10-5/s and P from 3.2 to 7.9 GPa in the D-DIA at Beamline 6-BMB at the Advanced Photon Source at Argonne National Lab. Strengths of magnesite aggregates increase as a function of pressure, from σ=0.85 GPa (at P = 3.2 GPa) to 1.69 GPa (at P = 7.9 GPa). Microstructures developed at P ≤ 6.2 GPa include grain flattening and sweeping undulatory extinction, and dynamic recrystallization at grain boundaries (by bulge nucleation), consistent with dislocation creep. Microstructures generated at P ≥ 6.7 GPa include some twins and kink bands, grain flattening and patchy undulatory extinction, and bulging recrystallization at grain boundaries. These microstructures indicate contributions to strain of both LTP and dislocation creep mechanisms. The pressure dependence can be described by a thermally activated enthalpy, where s increases with P by way of an activation volume V*. Based on both D-DIA and Griggs apparatus results (of Holyoke et al., 2014), V* = 8.5 (± 0.5) × 10-6 m3 mol-1. This value is comparable to V* determined for creep of olivine (9.5 (± 7) × 10-6 m3 mol-1 Durham et al., 2009), indicating that the strength difference between magnesite and olivine will continue to be significant at high pressures, and lead to strain localization at all subduction zone depths.

Influence of Cr and Y Addition on Microstructure, Mechanical Properties, and Corrosion Resistance of SPSed Fe-Based Alloys

NASA Astrophysics Data System (ADS)

Muthaiah, V. M. Suntharavel; Mula, Suhrit

2018-03-01

Present work investigates the microstructural stability during spark plasma sintering (SPS) of Fe-Cr-Y alloys, its mechanical properties and corrosion behavior for its possible applications in nuclear power plant and petrochemical industries. The SPS was carried out for the Fe-7Cr-1Y and Fe-15Cr-1Y alloys at 800 °C, 900 °C, and 1000 °C due to their superior thermal stability as reported in Muthaiah et al. [Mater Charact 114:43-53, 2016]. Microstructural analysis through TEM and electron back scattered diffraction confirmed that the grain sizes of the sintered samples depicted a dual size grain distribution with >50 pct grains within a range of 200 nm and remaining grains in the range 200 nm to 2 µm. The best combination of hardness, wear resistance, and corrosion behavior was achieved for the samples sintered at 1000 °C. The high hardness (9.6 GPa), minimum coefficient of friction (0.25), and extremely low wear volume (0.00277 × 10-2 mm3) and low corrosion rate (3.43 mpy) are discussed in the light of solid solution strengthening, grain size strengthening, grain boundary segregation, excellent densification due to diffusion bonding, and precipitation hardening due to uniformly distributed nanosize Fe17Y2 phase in the alloy matrix. The SEM analysis of the worn surface and corroded features corroborated well with the wear resistance and corrosion behavior of the corresponding samples.

Microstructure and Porosity of Laser Welds in Cast Ti-6Al-4V with Addition of Boron

NASA Astrophysics Data System (ADS)

Tolvanen, Sakari; Pederson, Robert; Klement, Uta

2018-03-01

Addition of small amounts of boron to cast Ti-6Al-4V alloy has shown to render a finer microstructure and improved mechanical properties. For such an improved alloy to be widely applicable for large aerospace structural components, successful welding of such castings is essential. In the present work, the microstructure and porosity of laser welds in a standard grade cast Ti-6Al-4V alloy as well as two modified alloy versions with different boron concentrations have been investigated. Prior-β grain reconstruction revealed the prior-β grain structure in the weld zones. In fusion zones of the welds, boron was found to refine the grain size significantly and rendered narrow elongated grains. TiB particles in the prior-β grain boundaries in the cast base material restricted grain growth in the heat-affected zone. The TiB particles that existed in the as cast alloys decreased in size in the fusion zones of welds. The hardness in the weld zones was higher than in the base material and boron did not have a significant effect on hardness of the weld zones. The fusion zones were smaller in the boron-modified alloys as compared with Ti-6Al-4V without boron. Computed tomography X-ray investigations of the laser welds showed that pores in the FZ of the boron modified alloys were confined to the lower part of the welds, suggesting that boron addition influences melt pool flow.

Textural evidence of the significance of compaction in the formation of adcumulates in the Skaergaard intrusion, East Greenland

NASA Astrophysics Data System (ADS)

Vukmanovic, Zoja; Holness, Marian; Mariani, Elisabetta

2017-04-01

It has been argued that the upwards decrease in incompatible element concentration in the Skaergaard Layered Series is due to an upwards increasing significance of compaction driven by gravitational loading. The suggested mechanisms for compaction are dislocation creep and dissolution-reprecipitation creep. Localised elongate zones of strong modal banding in the upper part of the Layered Series, known as trough bands, have also been interpreted as the result of localised recrystallization during compaction. In this study we examine the microstructures of Skaergaard gabbros to determine whether their fabrics (foliations and lineations) preserve a record of compaction. The most common microstructures formed by dislocation creep are low angle boundaries and, as a result of ongoing recovery processes, new grains. The (010)[001] slip system in plagioclase is commonly observed to be a "soft" orientation, creating a crystallographic preferred orientation (CPO) defined by the alignment of (010) planes, with [001] parallel to lineation. Previous work on dissolution-reprecipitation creep, shows a CPO with (010) planes aligned parallel to the principal compressive stress, and preferential mineral growth on (010) planes to form an SPO defined by grains elongated perpendicular to (010). In the Skaergaard Layered Series, the shape of cumulus plagioclase grains (as viewed in thin section) changes systematically up through the stratigraphy from highly tabular to equant. Foliations, defined both by a plagioclase SPO (with tabular grains aligned horizontally) and an associated CPO ((010) parallel to foliation), are strongest lower in the stratigraphy and reduce in strength upwards. Evidence for crystal plasticity is limited to bending of some plagioclase crystals and small numbers of low angle boundaries in all phases. There are no signs of recovery associated with dislocation creep. Compositional zoning is present on all plagioclase growth faces in the lower part of the stratigraphy, inconsistent with preferential dissolution-reprecipitation during compression. There are no fabrics or microstructures that can be attributed to solution-reprecipitation, and evidence for only minor microstructural modification by dislocation creep throughout the entire stratigraphy. The trough bands are characterised by strong lineation of elongate grains, an almost complete absence of microstructures caused by deformation, and euhedral plagioclase grains with concentric compositional zoning. These observations rule out recrystallization driven by compaction, and support the hypothesis that the modal banding in the trough bands is a result of grain sorting by magmatic flow. Our observations suggest that the Skaergaard fabrics throughout the Layered Series, are primary and formed at or close to the magma-mush interface as a consequence of particle re-arrangement by magmatic current, with only minor deformation-related fabric modification deeper in the mush. The Skaergaard adcumulates cannot therefore be attributed to compaction.

Embrittlement of Intercritically Reheated Coarse Grain Heat-Affected Zone of ASTM4130 Steel

NASA Astrophysics Data System (ADS)

Li, Liying; Han, Tao; Han, Bin

2018-04-01

In this investigation, a thermal welding simulation technique was used to investigate the microstructures and mechanical properties of the intercritically reheated coarse grain heat-affected zone (IR CGHAZ) of ASTM4130 steel. The effect of post weld heat treatment (PWHT) on the toughness of IR CGHAZ was also analyzed. The toughness of IR CGHAZ was measured by means of Charpy impact, and it is found that IR CGHAZ has the lowest toughness which is much lower than that of the base metal regardless of whether PWHT is applied or not. The as-welded IR CGHAZ is mainly composed of ferrite, martensite, and many blocky M-A constituents distributing along grain boundaries and subgrain boundaries in a near-connected network. Also, the prior austenite grains are still as coarse as those in the coarse grain heat-affected zone (CGHAZ). The presence of the blocky M-A constituents and the coarsened austenite grains result in the toughness deterioration of the as-welded IR CGHAZ. Most of the blocky M-A constituents are decomposed to granular bainite due to the effect of the PWHT. However, PWHT cannot refine the prior austenite grains. Thus, the low toughness of IR CGHAZ after PWHT can be attributed to two factors, i.e., the coarsened austenite grains, and the presence of the remaining M-A constituents and granular bainite, which are located at grain boundaries and subgrain boundaries in a near-connected network. The absorbed energy of the IR CGHAZ was increased by about 3.75 times, which means that the PWHT can effectively improve the toughness but it cannot be recovered to the level of base metal.

Microstructure Evolution and Mechanical Behavior of Ultrafine Ti-6Al-4V During Low Temperature Superplastic Deformation (Postprint)

DTIC Science & Technology

2016-09-13

through the deformed β matrix . A total elongation of 1000% and strain-rate-sensitivity exponent m = 0.48 were obtained at 550 °C and 2 × 10−4 s−1...two orders of magnitude faster than the corresponding static behaviors due to enhanced diffusion through the deformed b matrix . A total elongation of...various metallic materials, including titanium alloys, is usually the result of concurrent grain- or interphase-boundary sliding, grain- matrix

The microstructure of laterally seeded silicon-on-oxide

NASA Astrophysics Data System (ADS)

Pinizzotto, R. F.; Lam, H. W.; Vaandrager, B. L.

1982-03-01

The production of large scale integrated circuits in thin silicon films on insulating substrates is currently of much interest in the electronics industry. One of the most promising techniques of forming this composite structure is by lateral seeding. We have used optical microscopy and transmission electron microscopy to characterize the microstructure of silicon-on-oxide formed by scanning CW laser induced lateral epitaxy. The primary defects are dislocations. Dislocation rearrangement leads to the formation of both small angle boundaries (stable, regular dislocation arrays) and grain boundaries. The grains were found to be misoriented to the <100> direction perpendicular to the film plane by ≤ 4° and to the <100> directions in the plane of the film by ≤ 2°. Internal reflection twins are a common defect. Microtwinning was found to occur at the vertical step caused by the substrate-oxide interface if the substrate to oxide step height was > 120 nm. The microstructure is continuous across successive scan lines. Microstructural defects are found to initiate at the same topographical location in different oxide pads. We propose that this is due to the meeting of two crystallization growth fronts. The liquid silicon between the fronts causes large stresses in this area because of the 9% volume increase during solidification. The defects observed in the bulk may form by a similar mechanism or by dislocation generation at substrate-oxide interface irregularities. The models predict that slower growth leads to improved material quality. This has been observed experimentally.

An automated method of quantifying ferrite microstructures using electron backscatter diffraction (EBSD) data.

PubMed

Shrestha, Sachin L; Breen, Andrew J; Trimby, Patrick; Proust, Gwénaëlle; Ringer, Simon P; Cairney, Julie M

2014-02-01

The identification and quantification of the different ferrite microconstituents in steels has long been a major challenge for metallurgists. Manual point counting from images obtained by optical and scanning electron microscopy (SEM) is commonly used for this purpose. While classification systems exist, the complexity of steel microstructures means that identifying and quantifying these phases is still a great challenge. Moreover, point counting is extremely tedious, time consuming, and subject to operator bias. This paper presents a new automated identification and quantification technique for the characterisation of complex ferrite microstructures by electron backscatter diffraction (EBSD). This technique takes advantage of the fact that different classes of ferrite exhibit preferential grain boundary misorientations, aspect ratios and mean misorientation, all of which can be detected using current EBSD software. These characteristics are set as criteria for identification and linked to grain size to determine the area fractions. The results of this method were evaluated by comparing the new automated technique with point counting results. The technique could easily be applied to a range of other steel microstructures. © 2013 Published by Elsevier B.V.

Effects of the Strain Rate and Temperature on the Microstructural Evolution of Twin-Rolled Cast Wrought AZ31B Alloys Sheets

NASA Astrophysics Data System (ADS)

Rodriguez, A. K.; Kridli, G.; Ayoub, G.; Zbib, H.

2013-10-01

This article investigates the effects of the strain rate and temperature on the microstructural evolution of twin-rolled cast wrought AZ31B sheets. This was achieved through static heating and through tensile test performed at strain rates from 10-4 to 10-1 s-1 and temperatures between room temperature (RT) and 300 °C. While brittle fracture with high stresses and limited elongation was observed at the RT, ductile behavior was obtained at higher temperatures with low strain rates. The strain rate sensitivity and activation energy calculations indicate that grain boundary diffusion and lattice diffusion are the two rate-controlling mechanisms at warm and high temperatures, respectively. An analysis of the evolution of the microstructure provided some indications of the most probable deformation mechanisms in the material: twinning operates at lower temperatures, and dynamic recrystallization dominates at higher temperatures. The static evolution of the microstructure was also studied, proving a gradual static grain growth of the AZ31B with annealing temperature and time.

Microstructural and Textural Differences Induced by Water and Furnace Cooling in Commercially Pure Zr Annealed in the α + β Region

NASA Astrophysics Data System (ADS)

Chai, Linjiang; Wang, Tingting; Ren, Yi; Song, Bo; Guo, Ning; Chen, Liangyu

2018-07-01

In this work, a commercially pure Zr sheet with a typical bimodal basal texture was annealed in an α + β region and then subjected to different coolings (in water and furnace). Microstructures and textures of both the as-received and the heat-treated specimens were investigated by electron channeling contrast imaging and electron backscatter diffraction techniques. Results show that a duplex microstructure consisting of untransformed bulk α grains and twinned martensitic plates is produced in the water-cooled specimen, which possesses a weakened texture compared to the initial one. For the specimen cooled in furnace, however, a uniform microstructure fully comprised of coarser equiaxed grains with a strengthened texture is obtained. Analyses reveal that the rapid cooling in water could suppress variant selection behaviors during β → α transformation and allow α plates with scattered orientations to be nucleated inside β phases, contributing to the weakened texture. In contrast, during slow cooling in furnace, β boundaries would act as preferred nucleation sites of α embryos, resulting in a strong variant selection that accounts for the intensified texture.

Microstructural and Textural Differences Induced by Water and Furnace Cooling in Commercially Pure Zr Annealed in the α + β Region

NASA Astrophysics Data System (ADS)

Chai, Linjiang; Wang, Tingting; Ren, Yi; Song, Bo; Guo, Ning; Chen, Liangyu

2018-03-01

In this work, a commercially pure Zr sheet with a typical bimodal basal texture was annealed in an α + β region and then subjected to different coolings (in water and furnace). Microstructures and textures of both the as-received and the heat-treated specimens were investigated by electron channeling contrast imaging and electron backscatter diffraction techniques. Results show that a duplex microstructure consisting of untransformed bulk α grains and twinned martensitic plates is produced in the water-cooled specimen, which possesses a weakened texture compared to the initial one. For the specimen cooled in furnace, however, a uniform microstructure fully comprised of coarser equiaxed grains with a strengthened texture is obtained. Analyses reveal that the rapid cooling in water could suppress variant selection behaviors during β → α transformation and allow α plates with scattered orientations to be nucleated inside β phases, contributing to the weakened texture. In contrast, during slow cooling in furnace, β boundaries would act as preferred nucleation sites of α embryos, resulting in a strong variant selection that accounts for the intensified texture.

Atomistic modeling of helium segregation to grain boundaries in tungsten and its effect on de-cohesion

NASA Astrophysics Data System (ADS)

Martínez, Enrique; Uberuaga, Blas P.; Wirth, Brian D.

2017-08-01

Due to their low sputtering yield, low intrinsic tritium retention, high melting point, and high thermal conductivity, W and W alloys are promising candidates for the divertor region in a magnetic fusion device. Transmutation reactions under neutron irradiation lead to the formation of He and H particles that potentially degrade material performance and might lead to failure. High He fluxes ultimately lead to the formation and bursting of bubbles that induce swelling, a strong decrease in toughness, and a nanoscale microstructure that potentially degrades the plasma. Understanding the behavior of He in polycrystalline W is thus of significant importance as one avenue for controlling the material properties under operating conditions. This paper studies the interaction of substitutional He atoms with various grain boundaries in pure W and the effect of the He presence on the system response to external loading. We observe that He segregates to all the interfaces tested and decreases the cohesion of the system at the grain boundary. Upon tension, the presence of He significantly decreases the yield stress, which depends considerably on the bubble pressure. Increasing pressure reduces cohesion, as expected. More complex stress states result in more convoluted behavior, with He hindering grain boundary sliding upon simple shear.

The effect of metal microstructure on the initial attachment of Escherichia coli to 1010 carbon steel.

PubMed

Javed, M A; Stoddart, P R; McArthur, S L; Wade, S A

2013-09-01

Metallurgical features have been shown to play an important role in the attachment of microorganisms to metal surfaces. In the present study, the influence of the microstructure of as-received (AR) and heat-treated (HT) 1010 carbon steel on the initial attachment of bacteria was investigated. Heat treatment was carried out with the aim of increasing the grain size of the carbon steel coupons. Mirror-polished carbon steel coupons were immersed in a minimal medium inoculated with Escherichia coli (ATCC 25922) to investigate the early (15, 30 and 60 min) and relatively longer-term (4 h) stages of bacterial attachment. The results showed preferential colonisation of bacteria on the grain boundaries of the steel coupons. The bacterial attachment to AR steel coupons was relatively uniform compared to the HT steel coupons where an increased number of localised aggregates of bacteria were found. Quantitative analysis showed that the ratio of the total number of isolated (i.e., single) bacteria to the number of bacteria in aggregates was significantly higher on the AR coupons than the HT coupons. Longer-term immersion studies showed production of extracellular polymeric substances by the bacteria and corrosion at the grain boundaries on both types of steel coupon tested.

Kinetics and formation mechanisms of intragranular ferrite in V-N microalloyed 600 MPa high strength rebar steel

NASA Astrophysics Data System (ADS)

Zhang, Jing; Wang, Fu-ming; Li, Chang-rong

2016-04-01

To systematically investigate the kinetics and formation mechanisms of intragranular ferrite (IGF), isothermal heat treatment in the temperature range of 450°C to 600°C with holding for 30 s to 300 s, analysis of the corresponding microstructures, and observation of the precipitated particles were conducted in V-N microalloyed 600 MPa high strength rebar steel. The potency of V(C,N) for IGF nucleation was also analyzed statistically. The results show that the dominant microstructure transforms from bainite (B) and acicular ferrite (AF) to grain boundary ferrite (GBF), intragranular polygonal ferrite (IPF), and pearlite (P) as the isothermal temperature increases from 450°C to 600°C. When the holding time at 600°C is extended from 30 s to 60 s, 120 s, and 300 s, the GBF content ranges from 6.0vol% to 6.5vol% and the IPF content increases from 0.5vol% to 2.8vol%, 13.1vol%, and 13.5vol%, respectively, because the ferrite transformation preferentially occurs at the grain boundaries and then occurs at the austenite grains. Notably, V(C,N) particles are the most effective nucleation site for the formation of IPF, accounting for 51% of the said formation.

Microstructures and mechanical properties of Cu-Sn alloy subjected to elevated-temperature heat deformation

NASA Astrophysics Data System (ADS)

Hui, Jun; Feng, Zaixin; Fan, Wenxin; Wang, Pengfei

2018-04-01

Cu-Sn alloy was subjected to elevated-temperature isothermal compression with 0.01 s‑1 strain rate and 500 ∼ 700 °C temperature range. The thermal compression curve reflected a competing process of work hardening versus dynamic recovery (DRV) and recrystallization, which exhibited an obvious softening trend. Meanwhile, high-temperature deformation and microstructural features in different regions of the alloy was analyzed through EBSD. The results show that grains grow as the temperature rises, competition among recrystallization, substructural, and deformation regions tends to increase with the increase of temperature, and distribution frequency of recrystallization regions gradually increases and then drops suddenly at 650 °C. At 500 ∼ 550 °C, preferentially oriented texturing phenomenon occurs, low angle boundaries(LABs) are gradually transformed into high angle boundaries (HABs) and the Σ (CSL) boundaries turn gradually into Σ3 boundaries. In tensile test of tin bronze, elongation at break increases slowly, whereas yield strength (YS) and ultimate tensile strength (TS) decrease gradually.

Ultra-thin grain-oriented silicon steel sheet fabricated by a novel way: Twin-roll strip casting and two-stage cold rolling

NASA Astrophysics Data System (ADS)

Wang, Yin-Ping; Liu, Hai-Tao; Song, Hong-Yu; Liu, Jia-Xin; Shen, Hui-Ying; Jin, Yang; Wang, Guo-Dong

2018-04-01

0.05-0.15 mm-thick ultra-thin grain-oriented silicon steel sheets were successfully produced by a novel processing route including strip casting, hot rolling, normalizing, two-stage cold rolling with intermediate annealing, primary recrystallization annealing and secondary recrystallization annealing. The evolutions of microstructure, texture and inhibitor along the processing were briefly investigated. The results showed that the initial Goss orientation originated due to the heterogenous nucleation of δ-ferrite grains during solidification. Because of the lack of shear deformation, only a few Goss grains were observed in the hot rolled sheet. After the first cold rolling and intermediate annealing, Goss texture was enhanced and distributed in the whole thickness. A small number of Goss grains having a high fraction of high energy boundaries exhibited in the primary recrystallization annealed sheet. A large number of fine and dispersed MnS and AlN and a few co-precipitates MnS and AlN with the size range of 10-70 nm were also observed. Interestingly, a well-developed secondary recrystallization microstructure characterized by 10-60 mm grains and a sharp Goss texture were finally produced in the 0.05-0.15 mm-thick ultra-thin sheets. A magnetic induction B8 of 1.72-1.84 T was obtained. Another new finding was that a few {2 3 0}〈0 0 1〉 and {2 1 0}〈1 2 7〉 grains also can grow up abnormally because of the high fraction of high energy boundaries and the size and number advantage, respectively. These non-Goss grains finally deteriorated the magnetic properties of the ultra-thin sheets. In addition, low surface energies of {hk0} planes may also contribute to the abnormal growth of Goss, {2 3 0}〈0 0 1〉 and {2 1 0}〈1 2 7〉 grains.

Three-Dimensional Characterization of Microstructure by Electron Back-Scatter Diffraction

DTIC Science & Technology

2007-03-28

Costa LDF, Cesar RM, Cesar J. 2000. Shape Analysis and Classification: Theory and Practice. Boca Raton, FL: CRC Press. 660 pp. 7. Williams RE. 1968...The distribution of grain boundaries in magnesia as a function of five macroscopic parameters. Acta Mater. 51:3663–74 27. Schaeben H, Apel M, Frank T

Microstructures and performance of CaO-based ceramic cores with different particle size distributions for investment casting

NASA Astrophysics Data System (ADS)

Zhou, P. P.; Wu, G. Q.; Tao, Y.; Cheng, X.; Zhao, J. Q.; Nan, H.

2018-02-01

A series of calcium-based ceramic cores for casting titanium alloy were prepared by mixing different amounts of coarse and fine powders through injection molding. The effects of particle size on the microstructures and properties of the ceramic cores were investigated using quantitative and statistical analysis methods. It is found that the shrinkage and room-temperature strength of the ceramic cores were enhanced as increasing the contents of fine particles. Moreover, the creep resistance of the ceramic cores increased initially and then decreased. The increase in the fine particle content of the cores reduced the number and mean diameter of pores after sintering. The grain boundary density decreased firstly and then increased. The flexural strength of the ceramic cores at room temperature decreased with increasing porosity of ceramic cores, whereas the creep resistance increased with decreasing grain boundary density. A core exhibiting the optimal property was obtained when mixing 65 wt% of coarse powders (75-150 μm) and 35 wt% of fine powders (25-48 μm).

Strain localization in ultramylonitic calcite marbles by dislocation creep-accommodated grain boundary sliding

NASA Astrophysics Data System (ADS)

Rogowitz, Anna; Grasemann, Bernhard; Clancy White, Joseph

2015-04-01

Strain localization in monomineralic rocks is often associated with brittle precursors, resulting in stress and strain concentration, followed by grain size reduction and activation of grain-size-sensitive deformation mechanisms such as diffusion creep, grain boundary sliding and cataclastic flow. The aforementioned mechanisms typically tend to produce a random crystallographic orientation or a decrease in intensity of a pre-existing texture. However, reports of fine grained polycrystalline materials showing a preferred crystallographic orientation indicate a need for subsequent grain re-organization by either static annealing or the activation of additional deformation mechanisms in conjunction with grain boundary sliding. We present observations from an almost pure calcite marble layer from Syros Island (Cyclades, Greece) deformed in lower greenschist facies conditions. The presence of a crack (i.e. cross-cutting element) that rotated during shear resulted in the formation of a flanking structure. At the location of maximum displacement (120 cm) along the cross-cutting element, the marble is extremely fine grained (3 µm) leading to anticipation of deformation by grain-size-sensitive mechanisms. Detailed microstructural analysis of the highly strained (80 < gamma < 1000) calcite ultramylonite by optical microscopy, electron backscatter diffraction and scanning transmission electron microscopy show that recrystallization by bulging results in small, strain-free grains. The change in grain size appears to be concomitant with increased activity of independent grain boundary sliding as indicated by a random misorientation angle distribution. At the same time, dislocation multiplication through Frank-Read sources produces high mean dislocation density (~ 5x10^13 m^-2) as well as a weak primary CPO; the latter all argue that grain boundary sliding was accommodated by dislocation activity. Theoretical and experimental determined relationships (paleowattmeter, paleopiezometer, dislocation density) have been used to estimate the flow stress conditions. All of the applied relationships indicate differential stresses in a range between 80 and 200 MPa. Plotted in a deformation mechanism map for calcite, the data show that the ultramylonite was deformed at maximum strain rates of 10^-9 s^-1. Our study shows that the switch from dominantly dislocation creep to grain boundary sliding accommodated by dislocation activity corresponds to strain softening and can be an important strain localization process in calcite rocks, even at high strain rate (10^-9 s^-1) and low temperature (300 °C).

High temperature compounds for turbine vanes

NASA Technical Reports Server (NTRS)

Rhodes, W. H.; Cannon, R. M., Jr.

1972-01-01

Fabrication and microstructure control studies were conducted on SiC, Si3N4, and composites based on these compounds. Charpy mode impact testing to 2400 F established that beta-spodumene, lithium aluminum silicate, coated Si3N4, Si3N4 derived from alpha-Si3N4 powder, and SiC containing 5-25 v/o chopped C fibers had the most promising strengths. Several other composite systems had excellent microstructures and could prove interesting materials in the future. Stress-rupture testing on Si3N4 established that increasing 2000 F - 100 hour strengths were obtained for increasing grain size to at least 5 micrometers, increasing density and possibly increasing phase purity. These parameters became less important at 2400 F where it is thought a grain boundary phase controls strength.

Effect of doping ions on the structural defect and the electrical behavior of CaCu{sub 3}Ti{sub 4}O{sub 12} ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xue, Renzhong; Department of Technology and Physics, Zhengzhou University of Light Industry, Zhengzhou 450002; Zhao, Gaoyang, E-mail: zhaogy@xaut.edu.cn

Graphical abstract: The dielectric constant decreases with Ta doping, increases with Y doping and keeps almost constant with Zr doping compared with that of pure CCTO. - Highlights: • Y and Ta doping cause different defect types and concentration. • Defect influences the grain boundary mobility and results in different grain size. • Y doping increases the dielectric constant and decreases the nonlinear property. • Ta doping decreases the dielectric constant and enhances the nonlinear property. • Zr doped sample has nearly the defect type and dielectric properties as CaCu{sub 3}Ti{sub 4}O{sub 12}. - Abstract: The microstructure, dielectric and electricalmore » properties of CaCu{sub 3}Ti{sub 4−x}R{sub x}O{sub 12} (R = Y, Zr, Ta; x = 0 and 0.005) ceramics were investigated by XRD, Raman spectra, SEM and dielectric spectrum measurements. Positron annihilation measurements have been performed to investigate the influence of doping on the defects. The results show that all samples form a single crystalline phase. Y and Ta doping cause different defect types and increase the defect size and concentration, which influence the mobility of grain boundary and result in the different grain size. Y doping increases the dielectric constant and decreases the nonlinear property while Ta doping lead to an inverse result. Zr-doped sample has nearly the defect type, grain morphology and dielectric properties as pure CaCu{sub 3}Ti{sub 4}O{sub 12}. The effects of microstructure including the grain morphology and the vacancy defects on the mechanism of the dielectric and electric properties by doping are discussed.« less

Precipitate strengthening of nanostructured aluminium alloy.

PubMed

Wawer, Kinga; Lewandowska, Malgorzata; Kurzydlowski, Krzysztof J

2012-11-01

Grain boundaries and precipitates are the major microstructural features influencing the mechanical properties of metals and alloys. Refinement of the grain size to the nanometre scale brings about a significant increase in the mechanical strength of the materials because of the increased number of grain boundaries which act as obstacles to sliding dislocations. A similar effect is obtained if nanoscale precipitates are uniformly distributed in coarse grained matrix. The development of nanograin sized alloys raises the important question of whether or not these two mechanisms are "additive" and precipitate strengthening is effective in nanostructured materials. In the reported work, hydrostatic extrusion (HE) was used to obtain nanostructured 7475 aluminium alloy. Nanosized precipitates were obtained by post-HE annealing. It was found that such annealing at the low temperatures (100 degrees C) results in a significant increase in the microhardness (HV0.2) and strength of the nanostructured 7475 aluminium alloy. These results are discussed in terms of the interplay between the precipitation and deformation of nanocrystalline metals.

Quantification of Microtexture at Weld Nugget of Friction Stir-Welded Carbon Steel

NASA Astrophysics Data System (ADS)

Husain, Md M.; Sarkar, R.; Pal, T. K.; Ghosh, M.; Prabhu, N.

2017-05-01

Friction stir welding of C-Mn steel was carried out under 800-1400 rpm tool rotation. Tool traversing speed of 50 mm/min remained same for all joints. Effect of thermal state and deformation on texture and microstructure at weld nugget was investigated. Weld nugget consisted of ferrite + bainite/Widmanstatten ferrite with different matrix grain sizes depending on peak temperature. A texture around ( ϕ 2 = 0°, φ = 30°, ϕ 2 = 45°) was developed at weld nugget. Grain boundary misorientation at weld nugget indicated that continuous dynamic recrystallization influenced the development of fine equiaxed grain structure. Pole figures and orientation distribution function were used to determine crystallographic texture at weld nugget and base metal. Shear texture components D1, D2 and F were present at weld nugget. D1 shear texture was more prominent among all. Large number of high-angle grain boundaries ( 60-70%) was observed at weld nugget and was the resultant of accumulation of high amount of dislocation, followed by subgrain formation.

Spark Plasma Sintering of a Gas Atomized Al7075 Alloy: Microstructure and Properties

PubMed Central

Molnárová, Orsolya; Málek, Přemysl; Lukáč, František; Chráska, Tomáš

2016-01-01

The powder of an Al7075 alloy was prepared by gas atomization. A combination of cellular, columnar, and equiaxed dendritic-like morphology was observed in individual powder particles with continuous layers of intermetallic phases along boundaries. The cells are separated predominantly by high-angle boundaries, the areas with dendritic-like morphology usually have a similar crystallographic orientation. Spark plasma sintering resulted in a fully dense material with a microstructure similar to that of the powder material. The continuous layers of intermetallic phases are replaced by individual particles located along internal boundaries, coarse particles are formed at the surface of original powder particles. Microhardness measurements revealed both artificial and natural ageing behavior similar to that observed in ingot metallurgy material. The minimum microhardness of 81 HV, observed in the sample annealed at 300 °C, reflects the presence of coarse particles. The peak microhardness of 160 HV was observed in the sample annealed at 500 °C and then aged at room temperature. Compression tests confirmed high strength combined with sufficient plasticity. Annealing even at 500 °C does not significantly influence the distribution of grain sizes—about 45% of the area is occupied by grains with the size below 10 µm. PMID:28774126

Hidden secrets of deformation: Impact-induced compaction within a CV chondrite

NASA Astrophysics Data System (ADS)

Forman, L. V.; Bland, P. A.; Timms, N. E.; Collins, G. S.; Davison, T. M.; Ciesla, F. J.; Benedix, G. K.; Daly, L.; Trimby, P. W.; Yang, L.; Ringer, S. P.

2016-10-01

The CV3 Allende is one of the most extensively studied meteorites in worldwide collections. It is currently classified as S1-essentially unshocked-using the classification scheme of Stöffler et al. (1991), however recent modelling suggests the low porosity observed in Allende indicates the body should have undergone compaction-related deformation. In this study, we detail previously undetected evidence of impact through use of Electron Backscatter Diffraction mapping to identify deformation microstructures in chondrules, AOAs and matrix grains. Our results demonstrate that forsterite-rich chondrules commonly preserve crystal-plastic microstructures (particularly at their margins); that low-angle boundaries in deformed matrix grains of olivine have a preferred orientation; and that disparities in deformation occur between chondrules, surrounding and non-adjacent matrix grains. We find heterogeneous compaction effects present throughout the matrix, consistent with a highly porous initial material. Given the spatial distribution of these crystal-plastic deformation microstructures, we suggest that this is evidence that Allende has undergone impact-induced compaction from an initially heterogeneous and porous parent body. We suggest that current shock classifications (Stöffler et al., 1991) relying upon data from chondrule interiors do not constrain the complete shock history of a sample.

Temperature stability of coercivity in mischmetal-Fe-Co-B melt-spun ribbons

NASA Astrophysics Data System (ADS)

Li, Rui; Zhang, Hong-Rui; Liu, Yao; Zuo, Shu-Lan; Xiong, Jie-Fu; Zuo, Wen-Liang; Zhao, Tong-Yun; Hu, Feng-Xia; Sun, Ji-Rong; Shen, Bao-Gen

2018-05-01

Coercivity temperature coefficient (β) of the permanent magnet depends on its intrinsic magnetic properties and microstructure. In this paper, the relationship between β and the temperature stabilities of magnetocrystalline anisotropy field (H a ) and saturation magnetization (M s ) as well as the microstructure is discussed. Regarding two concerned microstructural factors: grain size and grain boundary, coercivity thermal-stabilities of MM13.5Fe79.5B7 (MM-mischmetal: unseparated La-Ce-Pr-Nd alloy) and MMxFe94‑xB6 (x = 12, 13, 14, 15, 16, 19) melt-spun ribbons, respectively, are investigated. High β values near the theoretical limit are obtained either by decreasing grain size or by reducing MM percentage. In addition, coercivities above room temperature of MM13.5Fe79.5‑yCoyB7 (y = 0, 3, 6, 9, 12, 15) melt-spun ribbons are measured. The detailed influences of Co substitutions on β are analyzed, and the weak temperature dependence of M s is proved to the reason for the observed decrease of β. These findings suggest that proper strategy to minimize local stray fields is the key to enhance coercivity thermal-stability of 2:14:1 structure magnet.

Recrystallization and Grain Growth Kinetics in Binary Alpha Titanium-Aluminum Alloys

NASA Astrophysics Data System (ADS)

Trump, Anna Marie

Titanium alloys are used in a variety of important naval and aerospace applications and often undergo thermomechanical processing which leads to recrystallization and grain growth. Both of these processes have a significant impact on the mechanical properties of the material. Therefore, understanding the kinetics of these processes is crucial to being able to predict the final properties. Three alloys are studied with varying concentrations of aluminum which allows for the direct quantification of the effect of aluminum content on the kinetics of recrystallization and grain growth. Aluminum is the most common alpha stabilizing alloying element used in titanium alloys, however the effect of aluminum on these processes has not been previously studied. This work is also part of a larger Integrated Computational Materials Engineering (ICME) effort whose goal is to combine both computational and experimental efforts to develop computationally efficient models that predict materials microstructure and properties based on processing history. The static recrystallization kinetics are measured using an electron backscatter diffraction (EBSD) technique and a significant retardation in the kinetics is observed with increasing aluminum concentration. An analytical model is then used to capture these results and is able to successfully predict the effect of solute concentration on the time to 50% recrystallization. The model reveals that this solute effect is due to a combination of a decrease in grain boundary mobility and a decrease in driving force with increasing aluminum concentration. The effect of microstructural inhomogeneities is also experimentally quantified and the results are validated with a phase field model for recrystallization. These microstructural inhomogeneities explain the experimentally measured Avrami exponent, which is lower than the theoretical value calculated by the JMAK model. Similar to the effect seen in recrystallization, the addition of aluminum also significantly slows downs the grain growth kinetics. This is generally attributed to the solute drag effect due to segregation of solute atoms at the grain boundaries, however aluminum segregation is not observed in these alloys. The mechanism for this result is explained and is used to validate the prediction of an existing model for solute drag.

Thermal stability comparison of nanocrystalline Fe-based binary alloy pairs

DOE PAGES

Clark, Blythe G.; Hattar, Khalid Mikhiel; Marshall, Michael Thomas; ...

2016-03-24

Here, the widely recognized property improvements of nanocrystalline (NC) materials have generated significant interest, yet have been difficult to realize in engineering applications due to the propensity for grain growth in these interface-dense systems. While traditional pathways to thermal stabilization can slow the mobility of grain boundaries, recent theories suggest that solute segregation in NC alloy can reduce the grain boundary energy such that thermodynamic stabilization is achieved. Following the predictions of Murdock et al., here we compare for the first time the thermal stability of a predicted NC stable alloy (Fe-10at.% Mg) with a predicted non-NC stable alloy (Fe-10at.%more » Cu) using the same processing and characterization methodologies. Results indicate improved thermal stability of the Fe-Mg alloy in comparison to the Fe-Cu, and observed microstructures are consistent with those predicted by Monte Carlo simulations.« less

Influence of interface point defect on the dielectric properties of Y doped CaCu3Ti4O12 ceramics

NASA Astrophysics Data System (ADS)

Deng, Jianming; Sun, Xiaojun; Liu, Saisai; Liu, Laijun; Yan, Tianxiang; Fang, Liang; Elouadi, Brahim

2016-04-01

CaCu3Ti4-xYxO12 (0≤x≤0.12) ceramics were fabricated with conventional solid-state reaction method. Phase structure and microstructure of prepared ceramics were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The impedance and modulus tests both suggested the existence of two different relaxation behavior, which were attributed to bulk and grain boundary response. In addition, the conductivity and dielectric permittivity showed a step-like behavior under 405K. Meanwhile, frequency independence of dc conduction became dominant when above 405K. In CCTO ceramic, rare earth element Y3+ ions as an acceptor were used to substitute Ti sites, decreasing the concentration of oxygen vacancy around grain-electrode and grain boundary. The reason to the reduction of dielectric behavior in low frequencies range was associated with the Y doping in CCTO ceramic.