[Influence on microstructure of dental zirconia ceramics prepared by two-step sintering].

PubMed

Jian, Chao; Li, Ning; Wu, Zhikai; Teng, Jing; Yan, Jiazhen

2013-10-01

To investigate the microstructure of dental zirconia ceramics prepared by two-step sintering. Nanostructured zirconia powder was dry compacted, cold isostatic pressed, and pre-sintered. The pre-sintered discs were cut processed into samples. Conventional sintering, single-step sintering, and two-step sintering were carried out, and density and grain size of the samples were measured. Afterward, T1 and/or T2 of two-step sintering ranges were measured. Effects on microstructure of different routes, which consisted of two-step sintering and conventional sintering were discussed. The influence of T1 and/or T2 on density and grain size were analyzed as well. The range of T1 was between 1450 degrees C and 1550 degrees C, and the range of T2 was between 1250 degrees C and 1350 degrees C. Compared with conventional sintering, finer microstructure of higher density and smaller grain could be obtained by two-step sintering. Grain growth was dependent on T1, whereas density was not much related with T1. However, density was dependent on T2, and grain size was minimally influenced. Two-step sintering could ensure a sintering body with high density and small grain, which is good for optimizing the microstructure of dental zirconia ceramics.

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.

Influence of friction stir processing on the room temperature fatigue cracking mechanisms of A356 aluminum alloy

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

Nelaturu, Phalgun; Jana, Saumyadeep; Mishra, Rajiv S.

Here, failure by fatigue is a common problem associated with cast aluminum alloys due to defects like shrinkage porosities, non-metallic inclusions, etc. Friction stir processing (FSP) has recently emerged as an effective technique for local modification of microstructure. This study investigates the fatigue crack initiation and growth mechanisms in cast and FSPed A356 aluminum alloy. Two sets of parameters were used to friction stir the cast alloy resulting in the complete modification the cast microstructure to a wrought microstructure. Both the FSPed microstructures exhibited severe abnormal grain growth (AGG) after heat treatment leading to a multimodal grain size distribution –more » the grain sizes ranging from a few microns to a few millimeters. One of the FSP conditions displayed an excellent improvement in fatigue life by an order of magnitude, while the other condition displayed an unexpectedly large scatter in fatigue lives. Detailed study of the fractured fatigue specimens by electron back scattered diffraction (EBSD) revealed that both, fatigue crack initiation and propagation, were intimately tied to the grain size as well as the grain misorientations in the microstructure.« less

Influence of friction stir processing on the room temperature fatigue cracking mechanisms of A356 aluminum alloy

DOE PAGES

Nelaturu, Phalgun; Jana, Saumyadeep; Mishra, Rajiv S.; ...

2018-01-11

Here, failure by fatigue is a common problem associated with cast aluminum alloys due to defects like shrinkage porosities, non-metallic inclusions, etc. Friction stir processing (FSP) has recently emerged as an effective technique for local modification of microstructure. This study investigates the fatigue crack initiation and growth mechanisms in cast and FSPed A356 aluminum alloy. Two sets of parameters were used to friction stir the cast alloy resulting in the complete modification the cast microstructure to a wrought microstructure. Both the FSPed microstructures exhibited severe abnormal grain growth (AGG) after heat treatment leading to a multimodal grain size distribution –more » the grain sizes ranging from a few microns to a few millimeters. One of the FSP conditions displayed an excellent improvement in fatigue life by an order of magnitude, while the other condition displayed an unexpectedly large scatter in fatigue lives. Detailed study of the fractured fatigue specimens by electron back scattered diffraction (EBSD) revealed that both, fatigue crack initiation and propagation, were intimately tied to the grain size as well as the grain misorientations in the microstructure.« less

The Effect of Microstructure on Fretting Fatigue Behavior of Nickel Alloy IN-100

DTIC Science & Technology

2007-03-01

microstructure there are grains with an average size of 6 microns. (Milligan et al) [16] The large globular particles are Ni3Al ( Padula , Milligan et al.) [17...had better crack propagation resistance. Padula , Milligan et al. [17] in studied of the effect of grain size and precipitate distribution on the...threshold of endurance strength with an increase in grain size. Finally Padula could not find a calculation method of CK1Δ that matched his data even

Numerical Study of Variation of Mechanical Properties of a Binary Aluminum Alloy with Respect to Its Grain Shapes †

PubMed Central

Sharifi, Hamid; Larouche, Daniel

2014-01-01

To study the variation of the mechanical behavior of binary aluminum copper alloys with respect to their microstructure, a numerical simulation of their granular structure was carried out. The microstructures are created by a repeated inclusion of some predefined basic grain shapes into a representative volume element until reaching a given volume percentage of the α-phase. Depending on the grain orientations, the coalescence of the grains can be performed. Different granular microstructures are created by using different basic grain shapes. Selecting a suitable set of basic grain shapes, the modeled microstructure exhibits a realistic aluminum alloy microstructure which can be adapted to a particular cooling condition. Our granular models are automatically converted to a finite element model. The effect of grain shapes and sizes on the variation of elastic modulus and plasticity of such a heterogeneous domain was investigated. Our results show that for a given α-phase fraction having different grain shapes and sizes, the elastic moduli and yield stresses are almost the same but the ultimate stress and elongation are more affected. Besides, we realized that the distribution of the θ phases inside the α phases is more important than the grain shape itself. PMID:28788607

Effect of Powder Grain Size on Microstructure and Magnetic Properties of Hexagonal Barium Ferrite Ceramic

NASA Astrophysics Data System (ADS)

Shao, Li-Huan; Shen, Si-Yun; Zheng, Hui; Zheng, Peng; Wu, Qiong; Zheng, Liang

2018-05-01

Compact hexagonal barium ferrite (BaFe12O19, BaM) ceramics with excellent magnetic properties have been prepared from powder with the optimal grain size. The dependence of the microstructure and magnetic properties of the ceramics on powder grain size was studied in detail. Single-phase hexagonal barium ferrite powder with grain size of 177 nm, 256 nm, 327 nm, and 454 nm was obtained by calcination under different conditions. Scanning electron microscopy revealed that 327-nm powder was beneficial for obtaining homogeneous grain size and compact ceramic. In addition, magnetic hysteresis loops and complex permeability spectra demonstrated that the highest saturation magnetization (67.2 emu/g) and real part of the permeability (1.11) at 1 GHz were also obtained using powder with grain size of 327 nm. This relationship between the powder grain size and the properties of the resulting BaM ceramic could be significant for development of microwave devices.

The Smallest Lunar Grains: Analytical TEM Characterization of the Sub-micron Size Fraction of a Mare Soil

NASA Technical Reports Server (NTRS)

Thompson, M.; Christoffersen, R.

2010-01-01

The chemical composition, mineralogical type, and morphology of lunar regolith grains changes considerably with decreasing size, and below the approx.25 m size range the correlation between these parameters and remotely-sensed lunar surface properties connected to space weathering increases significantly. Although trends for these parameters across grain size intervals greater than 20 m are now well established, the 0 to 20 m size interval remains relatively un-subdivided with respect to variations in grain modal composition, chemistry and microstructure. Of particular interest in this size range are grains in the approximate < 1 m diameter class, whose fundamental properties are now the focus of lunar research pertaining to electrostatic grain transport, dusty plasmas, and lunar dust effects on crew health and exploration systems. In this study we have used analytical transmission electron microscopy (TEM) to characterize the mineralogy, microstructure and major element composition of grains below the 1 m size threshold in lunar soil 10084.

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.

Plastic Flow and Microstructure Evolution during Thermomechanical Processing of a PM Nickel-Base Superalloy

NASA Astrophysics Data System (ADS)

Semiatin, S. L.; McClary, K. E.; Rollett, A. D.; Roberts, C. G.; Payton, E. J.; Zhang, F.; Gabb, T. P.

2013-06-01

Plastic flow and microstructure evolution during sub- and supersolvus forging and subsequent supersolvus heat treatment of the powder-metallurgy superalloy LSHR (low-solvus, high-refractory) were investigated to develop an understanding of methods that can be used to obtain a moderately coarse gamma grain size under well-controlled conditions. To this end, isothermal, hot compression tests were conducted over broad ranges of temperature [(1144 K to 1450 K) 871 °C to 1177 °C] and constant true strain rate (0.0005 to 10 s-1). At low temperatures, deformation was generally characterized by flow softening and dynamic recrystallization that led to a decrease in grain size. At high subsolvus temperatures and low strain rates, steady-state flow or flow hardening was observed. These latter behaviors were ascribed to superplastic deformation and microstructure evolution characterized by a constant grain size or concomitant dynamic grain growth, respectively. During supersolvus heat treatment following subsolvus deformation, increases in grain size whose magnitude was a function of the prior deformation conditions were noted. A transition in flow behavior from superplastic to nonsuperplastic and the development during forging at a high subsolvus temperature of a wide (possibly bi- or multimodal) gamma-grain-size distribution having some large grains led to a substantially coarser grain size during supersolvus annealing in comparison to that produced under all other forging conditions.

Modeling of the static recrystallization for 7055 aluminum alloy by cellular automaton

NASA Astrophysics Data System (ADS)

Zhang, Tao; Lu, Shi-hong; Zhang, Jia-bin; Li, Zheng-fang; Chen, Peng; Gong, Hai; Wu, Yun-xin

2017-09-01

In order to simulate the flow behavior and microstructure evolution during the pass interval period of the multi-pass deformation process, models of static recovery (SR) and static recrystallization (SRX) by the cellular automaton (CA) method for the 7055 aluminum alloy were established. Double-pass hot compression tests were conducted to acquire flow stress and microstructure variation during the pass interval period. With the basis of the material constants obtained from the compression tests, models of the SR, incubation period, nucleation rate and grain growth were fitted by least square method. A model of the grain topology and a statistical computation of the CA results were also introduced. The effects of the pass interval time, temperature, strain, strain rate and initial grain size on the microstructure variation for the SRX of the 7055 aluminum alloy were studied. The results show that a long pass interval time, large strain, high temperature and large strain rate are beneficial for finer grains during the pass interval period. The stable size of the static recrystallized grain is not concerned with the initial grain size, but mainly depends on the strain rate and temperature. The SRX plays a vital role in grain refinement, while the SR has no effect on the variation of microstructure morphology. Using flow stress and microstructure comparisons of the simulated and experimental CA results, the established CA models can accurately predict the flow stress and microstructure evolution during the pass interval period, and provide guidance for the selection of optimized parameters for the multi-pass deformation process.

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

Computer modelling of grain microstructure in three dimensions

NASA Astrophysics Data System (ADS)

Narayan, K. Lakshmi

We present a program that generates the two-dimensional micrographs of a three dimensional grain microstructure. The code utilizes a novel scanning, pixel mapping technique to secure statistical distributions of surface areas, grain sizes, aspect ratios, perimeters, number of nearest neighbors and volumes of the randomly nucleated particles. The program can be used for comparing the existing theories of grain growth, and interpretation of two-dimensional microstructure of three-dimensional samples. Special features have been included to minimize the computation time and resource requirements.

Fatigue Resistance of the Grain Size Transition Zone in a Dual Microstructure Superalloy Disk

NASA Technical Reports Server (NTRS)

Gabb, T. P.; Kantzos, P. T.; Telesman, J.; Gayda, J.; Sudbrack, C. K.; Palsa, B. S.

2010-01-01

Mechanical property requirements vary with location in nickel-based superalloy disks. To maximize the associated mechanical properties, heat treatment methods have been developed for producing tailored microstructures. In this study, a specialized heat treatment method was applied to produce varying grain microstructures from the bore to the rim portions of a powder metallurgy processed nickel-based superalloy disk. The bore of the contoured disk consisted of fine grains to maximize strength and fatigue resistance at lower temperatures. The rim microstructure of the disk consisted of coarse grains for maximum resistance to creep and dwell crack growth at high temperatures up to 704 C. However, the fatigue resistance of the grain size transition zone was unclear, and needed to be evaluated. This zone was located as a band in the disk web between the bore and rim. Specimens were extracted parallel and transverse to the transition zone, and multiple fatigue tests were performed at 427 and 704 C. Mean fatigue lives were lower at 427 C than for 704 C. Specimen failures often initiated at relatively large grains, which failed on crystallographic facets. Grain size distributions were characterized in the specimens, and related to the grains initiating failures as well as location within the transition zone. Fatigue life decreased with increasing maximum grain size. Correspondingly, mean fatigue resistance of the transition zone was slightly higher than that of the rim, but lower than that of the bore. The scatter in limited tests of replicates was comparable for all transition zone locations examined.

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.

Trends in Solidification Grain Size and Morphology for Additive Manufacturing of Ti-6Al-4V

NASA Astrophysics Data System (ADS)

Gockel, Joy; Sheridan, Luke; Narra, Sneha P.; Klingbeil, Nathan W.; Beuth, Jack

2017-12-01

Metal additive manufacturing (AM) is used for both prototyping and production of final parts. Therefore, there is a need to predict and control the microstructural size and morphology. Process mapping is an approach that represents AM process outcomes in terms of input variables. In this work, analytical, numerical, and experimental approaches are combined to provide a holistic view of trends in the solidification grain structure of Ti-6Al-4V across a wide range of AM process input variables. The thermal gradient is shown to vary significantly through the depth of the melt pool, which precludes development of fully equiaxed microstructure throughout the depth of the deposit within any practical range of AM process variables. A strategy for grain size control is demonstrated based on the relationship between melt pool size and grain size across multiple deposit geometries, and additional factors affecting grain size are discussed.

Dual Microstructure Heat Treatment of a Nickel-Base Disk Alloy Assessed

NASA Technical Reports Server (NTRS)

Gayda, John

2002-01-01

Gas turbine engines for future subsonic aircraft will require nickel-base disk alloys that can be used at temperatures in excess of 1300 F. Smaller turbine engines, with higher rotational speeds, also require disk alloys with high strength. To address these challenges, NASA funded a series of disk programs in the 1990's. Under these initiatives, Honeywell and Allison focused their attention on Alloy 10, a high-strength, nickel-base disk alloy developed by Honeywell for application in the small turbine engines used in regional jet aircraft. Since tensile, creep, and fatigue properties are strongly influenced by alloy grain size, the effect of heat treatment on grain size and the attendant properties were studied in detail. It was observed that a fine grain microstructure offered the best tensile and fatigue properties, whereas a coarse grain microstructure offered the best creep resistance at high temperatures. Therefore, a disk with a dual microstructure, consisting of a fine-grained bore and a coarse-grained rim, should have a high potential for optimal performance. Under NASA's Ultra-Safe Propulsion Project and Ultra-Efficient Engine Technology (UEET) Program, a disk program was initiated at the NASA Glenn Research Center to assess the feasibility of using Alloy 10 to produce a dual-microstructure disk. The objectives of this program were twofold. First, existing dual-microstructure heat treatment (DMHT) technology would be applied and refined as necessary for Alloy 10 to yield the desired grain structure in full-scale forgings appropriate for use in regional gas turbine engines. Second, key mechanical properties from the bore and rim of a DMHT Alloy 10 disk would be measured and compared with conventional heat treatments to assess the benefits of DMHT technology. At Wyman Gordon and Honeywell, an active-cooling DMHT process was used to convert four full-scale Alloy 10 disks to a dual-grain microstructure. The resulting microstructures are illustrated in the photomicrographs. The fine grain size in the bore can be contrasted with the coarse grain size in the rim. Testing (at NASA Glenn) of coupons machined from these disks showed that the DMHT approach did indeed produce a high-strength, fatigue resistant bore and a creep-resistant rim. This combination of properties was previously unobtainable using conventional heat treatments, which produced disks with a uniform grain size. Future plans are in place to spin test a DMHT disk under the Ultra Safe Propulsion Project to assess the viability of this technology at the component level. This testing will include measurements of disk growth at a high temperature as well as the determination of burst speed at an intermediate temperature.

Characterization of ultra-fine grained aluminum produced by accumulative back extrusion (ABE)

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

Alihosseini, H., E-mail: hamid.alihossieni@gmail.com; Materials Science and Engineering Department, Engineering School, Amirkabir University, Tehran; Faraji, G.

2012-06-15

In the present work, the microstructural evolutions and microhardness of AA1050 subjected to one, two and three passes of accumulative back extrusion (ABE) were investigated. The microstructural evolutions were characterized using transmission electron microscopy. The results revealed that applying three passes of accumulative back extrusion led to significant grain refinement. The initial grain size of 47 {mu}m was refined to the grains of 500 nm after three passes of ABE. Increasing the number of passes resulted in more decrease in grain size, better microstructure homogeneity and increase in the microhardness. The cross-section of ABEed specimen consisted of two different zones:more » (i) shear deformation zone, and (ii) normal deformation zone. The microhardness measurements indicated that the hardness increased from the initial value of 31 Hv to 67 Hv, verifying the significant microstructural refinement via accumulative back extrusion. - Highlights: Black-Right-Pointing-Pointer A significant grain refinement can be achieved in AA1050, Al alloy by applying ABE. Black-Right-Pointing-Pointer Microstructural homogeneity of ABEed samples increased by increasing the number of ABE cycles. Black-Right-Pointing-Pointer A substantial increase in the hardness, from 31 Hv to 67 Hv, was recorded.« less

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

Modeling of the Coupling of Microstructure and Macrosegregation in a Direct Chill Cast Al-Cu Billet

NASA Astrophysics Data System (ADS)

Heyvaert, Laurent; Bedel, Marie; Založnik, Miha; Combeau, Hervé

2017-10-01

The macroscopic multiphase flow and the growth of the solidification microstructures in the mushy zone of a direct chill (DC) casting are closely coupled. These couplings are the key to the understanding of the formation of the macrosegregation and of the non-uniform microstructure of the casting. In the present paper we use a multiphase and multiscale model to provide a fully coupled picture of the links between macrosegregation and microstructure in a DC cast billet. The model describes nucleation from inoculant particles and growth of dendritic and globular equiaxed crystal grains, fully coupled with macroscopic transport phenomena: fluid flow induced by natural convection and solidification shrinkage, heat, mass, and solute mass transport, motion of free-floating equiaxed grains, and of grain refiner particles. We compare our simulations to experiments on grain-refined and non-grain-refined industrial size billets from literature. We show that a transition between dendritic and globular grain morphology triggered by the grain refinement is the key to the explanation of the differences between the macrosegregation patterns in the two billets. We further show that the grain size and morphology are strongly affected by the macroscopic transport of free-floating equiaxed grains and of grain refiner particles.

Nanostructure formation during accumulative roll bonding of commercial purity titanium

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

Karimi, Mohsen, E-mail: m.karimi@shahroodut.ac.ir

2016-12-15

In this investigation, commercial purity titanium (CP–Ti) was subjected to accumulative roll bonding (ARB) process up to 8 cycles (equivalent strain of 6.4) at the ambient temperature. Transmission electron microscopy (TEM) and X–ray diffraction line profile analysis (XRDLPA) were utilized to investigate the microstructure and grain size evolution. Both characterization techniques could clarify the non–uniform microstructure in the early stages and the uniform microstructure in the final stages of the process. The effectiveness of ARB for the fabrication of the nano–grained structure in CP–Ti was revealed. It was found that the SFE is not the only factor affecting grain refinement,more » as compared with other studies on ARB of FCC materials. Influence of other factors such as the melting temperature and the crystalline structure of the material was determined on the grain refinement. - Highlights: •Nano–grained commercial purity titanium was produced by accumulative roll bonding. •TEM and XRDLPA were used for the characterization of the microstructure. •Important factors affecting the grain size of ARBed materials were discussed.« less

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

Effects of microrolling parameters on the microstructure and deformation behavior of pure copper

NASA Astrophysics Data System (ADS)

Jing, Yi; Zhang, Hong-mei; Wu, Hao; Li, Lian-jie; Jia, Hong-bin; Jiang, Zheng-yi

2018-01-01

Microrolling experiments and uniaxial tensile tests of pure copper under different annealing conditions were carried out in this paper. The effects of grain size and reduction on non-uniform deformation, edge cracking, and microstructure were studied. The experimental results showed that the side deformation became more non-uniform, resulting in substantial edge bulge, and the uneven spread increased with increasing grain size and reduction level. When the reduction level reached 80% and the grain size was 65 μm, slight edge cracks occurred. When the grain size was 200 μm, the edge cracks became wider and deeper. No edge cracks occurred when the grain size was 200 μm and the reduction level was less than 60%; edge cracks occurred when the reduction level was increased to 80%. As the reduction level increased, the grains were gradually elongated and appeared as a sheet-like structure along the rolling direction; a fine lamellar structure was obtained when the grain size was 20 μm and the reduction level was less than 60%.

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.

Effect of Bimodal Grain Size Distribution on Scatter in Toughness

NASA Astrophysics Data System (ADS)

Chakrabarti, Debalay; Strangwood, Martin; Davis, Claire

2009-04-01

Blunt-notch tests were performed at -160 °C to investigate the effect of a bimodal ferrite grain size distribution in steel on cleavage fracture toughness, by comparing local fracture stress values for heat-treated microstructures with uniformly fine, uniformly coarse, and bimodal grain structures. An analysis of fracture stress values indicates that bimodality can have a significant effect on toughness by generating high scatter in the fracture test results. Local cleavage fracture values were related to grain size distributions and it was shown that the largest grains in the microstructure, with an area percent greater than approximately 4 pct, gave rise to cleavage initiation. In the case of the bimodal grain size distribution, the large grains from both the “fine grain” and “coarse grain” population initiate cleavage; this spread in grain size values resulted in higher scatter in the fracture stress than in the unimodal distributions. The notch-bend test results have been used to explain the difference in scatter in the Charpy energies for the unimodal and bimodal ferrite grain size distributions of thermomechanically controlled rolled (TMCR) steel, in which the bimodal distribution showed higher scatter in the Charpy impact transition (IT) region.

Comparative Mineralogy, Microstructure and Compositional Trends in the Sub-Micron Size Fractions of Mare and Highland Lunar Soils

NASA Technical Reports Server (NTRS)

Thompson, M. S.; Christoffersen, R.; Noble, S. K.; Keller, L. P.

2012-01-01

The morphology, mineralogy, chemical composition and optical properties of lunar soils show distinct correlations as a function of grain size and origin [1,2,3]. In the <20 m size fraction, there is an increased correlation between lunar surface properties observed through remote sensing techniques and those attributed to space weathering phenomenae [1,2]. Despite the establishment of recognizable trends in lunar grains <20 in size [1,2,3], the size fraction < 10 m is characterized as a collective population of grains without subdivision. This investigation focuses specifically on grains in the <1 m diameter size fraction for both highland and mare derived soils. The properties of these materials provide the focus for many aspects of lunar research including the nature of space weathering on surface properties, electrostatic grain transport [4,5] and dusty plasmas [5]. In this study, we have used analytical transmission and scanning transmission electron microscopy (S/TEM) to characterize the mineralogy type, microstructure and major element compositions of grains in this important size range in lunar soils.

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.

A study on the influence of microstructure on small fatigue cracks

NASA Astrophysics Data System (ADS)

Castelluccio, Gustavo M.

In spite of its significance in industrial applications, the prediction of the influence of microstructure on the early stages of crack formation and growth in engineering alloys remains underdeveloped. The formation and early growth of fatigue cracks in the high cycle fatigue regime lasts for much of the fatigue life, and it is strongly influenced by microstructural features such as grain size, twins and morphological and crystallographic texture. However, most fatigue models do not predict the in uence of the microstructure on early stages of crack formation, or they employ parameters that should be calibrated with experimental data from specimens with microstructures of interest. These post facto strategies are adequate to characterize materials, but they are not fully appropriate to aid in the design of fatigue-resistant engineering alloys. This thesis considers finite element computational models that explicitly render the microstructure of selected FCC metallic systems and introduces a fatigue methodology that estimates transgranular and intergranular fatigue growth for microstructurally small cracks. The driving forces for both failure modes are assessed by means of fatigue indicators, which are used along with life correlations to estimate the fatigue life. Furthermore, cracks with meandering paths are modeled by considering crack growth on a grain-by-grain basis with a damage model embedded analytically to account for stress and strain redistribution as the cracks extend. The methodology is implemented using a crystal plasticity constitutive model calibrated for studying the effect of microstructure on early fatigue life of a powder processed Ni-base RR1000 superalloy at elevated temperature under high cycle fatigue conditions. This alloy is employed for aircraft turbine engine disks, which undergo a thermomechanical production process to produce a controlled bimodal grain size distribution. The prediction of the fatigue life for this complex microstructure presents particular challenges that are discussed and addressed. The conclusions of this work describe the mechanistic of microstructural small crack. In particular, the fatigue crack growth driving force has been characterized as it evolves within grains and crosses to other grains. Furthermore, the computational models serve as a tool to assess the effects of microstructural features on early stages of fatigue crack formation and growth, such as distributions of grain size and twins.

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.

A study of spectrum fatigue crack propagation in two aluminum alloys. 2: Influence of microstructures

NASA Technical Reports Server (NTRS)

Telesman, J.; Antolovich, S. D.

1985-01-01

The important metallurgical factors that influence both constant amplitude and spectrum crack growth behavior in aluminum alloys were investigated. The effect of microstructural features such as grain size, inclusions, and dispersoids was evaluated. It was shown that a lower stress intensities, the I/M 7050 alloy showed better fatigue crack propagation (FCP) resistance than P/M 7091 alloy for both constant amplitude and spectrum testing. It was suggested that the most important microstructural variable accounting for superior FCP resistance of 7050 alloy is its large grain size. It was further postulated that the inhomogenous planar slip and large grain size of 7050 limit dislocation interactions and thus increase slip reversibility which improves FCP performance. The hypothesis was supported by establishing that the cyclic strain hardening exponent for the 7091 alloy is higher than that of 7050.

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.

Spatial distribution of quartz recrystallization microstructures across the Aar massif (Swiss Central Alps)

NASA Astrophysics Data System (ADS)

Peters, M.; Herwegh, M.

2012-04-01

In the Aar massif, main foliation and major deformation structures were developed during NW-SE compression associated with the Alpine orogeny (Steck 1968). To be precise, shearing at the brittle to ductile transition may have initiated at different stages between 22-20 Ma and 14-12 Ma, followed by purely brittle deformation at around 10 Ma (Rolland et al. 2009). In light of the onset of dynamic recrystallization in quartz, Bambauer et al. (2009) defined a quartz recrystallization isograd in the northern part of the Aar massif. To the south, the grain size of recrystallized grains increases due to an increase of metamorphic temperatures from N to S. The aim of the current project is to carry out quantitative analysis on changes of the dynamic and static recrystallization behavior of quartz. Across the Aar massif, two general types of microstructures have to be discriminated: (i) weakly to moderately deformed host rocks and (ii) intensely deformed mylonites to ultramylonites out of high strain shear zones. In (i), volume fraction and size of recrystallized quartz grains increase towards the S showing grain size changes from around 5 µm up to ca. 200 µm. Southern microstructures are characterized by complete recrystallization. In terms of recrystallization processes, a transition from bulging recrystallization in the N to subgrain rotation recrystallization in the S occurs. Such a change in dynamic recrystallization processes combined with a grain size increase points towards reduced differential stresses with increasing temperature. This temperature gradient is also corroborated by a switch in the active glide systems in quartz from basal to rhomb dominated glide. In contrast to the granitic host rocks, the mylonites and ultramylonites (ii) show smaller recrystallized grain sizes due to enhanced strain rates. However, they also reveal a general increase of recrystallized grain sizes from N to S. In the S, microstructures from (i) and (ii) show equidimensional grains with 120° triple junctions and straight grain boundaries. Such microstructures are typical for static annealing. For that reason, we propose a post-deformational temperature pulse mainly affecting the southern part of the Aar massif. This annealing stage might correlate with the fluid pulse between 12-10 Ma suggested by Challandes et al. (2008). We will present constraints on the grade of deformation based on grain size data and CPO analyses, supporting the hypothesis that various deformation stages are well preserved in statically recrystallized structures.

Ductility Improvement of an AZ61 Magnesium Alloy through Two-Pass Submerged Friction Stir Processing

PubMed Central

Luo, Xicai; Cao, Genghua; Zhang, Wen; Qiu, Cheng; Zhang, Datong

2017-01-01

Friction stir processing (FSP) has been considered as a novel technique to refine the grain size and homogenize the microstructure of metallic materials. In this study, two-pass FSP was conducted under water to enhance the cooling rate during processing, and an AZ61 magnesium alloy with fine-grained and homogeneous microstructure was prepared through this method. Compared to the as-cast material, one-pass FSP resulted in grain refinement and the β-Mg17Al12 phase was broken into small particles. Using a smaller stirring tool and an overlapping ratio of 100%, a finer and more uniform microstructure with an average grain size of 4.6 μm was obtained through two-pass FSP. The two-pass FSP resulted in a significant improvement in elongation of 37.2% ± 4.3%, but a slight decrease in strength compared with one-pass FSP alloy. Besides the microstructure refinement, the texture evolution in the stir zone is also considered responsible for the ductility improvement. PMID:28772614

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.

Forging of Advanced Disk Alloy LSHR

NASA Technical Reports Server (NTRS)

Gabb, Timothy P.; Gayda, John; Falsey, John

2005-01-01

The powder metallurgy disk alloy LSHR was designed with a relatively low gamma precipitate solvus temperature and high refractory element content to allow versatile heat treatment processing combined with high tensile, creep and fatigue properties. Grain size can be chiefly controlled through proper selection of solution heat treatment temperatures relative to the gamma precipitate solvus temperature. However, forging process conditions can also significantly influence solution heat treatment-grain size response. Therefore, it is necessary to understand the relationships between forging process conditions and the eventual grain size of solution heat treated material. A series of forging experiments were performed with subsequent subsolvus and supersolvus heat treatments, in search of suitable forging conditions for producing uniform fine grain and coarse grain microstructures. Subsolvus, supersolvus, and combined subsolvus plus supersolvus heat treatments were then applied. Forging and subsequent heat treatment conditions were identified allowing uniform fine and coarse grain microstructures.

Effects of thermomechanical processing on the microstructure and mechanical properties of a Ti-V-N steel

NASA Astrophysics Data System (ADS)

Dogan, B.; Collins, L. E.; Boyd, J. D.

1988-05-01

Based on studies of austenite deformation behavior and continuous-cooling-transformation behavior of a Ti-V microalloyed steel by cam plastometer and quench-deformation dilatometer, respectively, plate rolling schedules were designed to produce (i) recrystallized austenite, (ii) unrecrystallized austenite, (iii) deformed ferrite + unrecrystallized austenite. The effects of austenite condition and cooling rate on the final microstructure and mechanical properties were investigated. To rationalize the variation in final ferrite grain size with different thermomechanical processing schedules, it is necessary to consider the kinetics of ferrite grain growth in addition to the density of ferrite nucleation sites. The benefit of dilatometer studies in determining the optimum deformation schedule and cooling rate for a given steel is domonstrated. A wide range of tensile and impact properties results from the different microstructures studied. Yield strength is increased by increasing the amount of deformed ferrite, bainite, or martensite, and by decreasing the ferrite grain size. Impact toughness is most strongly influenced by ferrite grain size and occurrence of rolling plane delaminations.

Effective grain size and charpy impact properties of high-toughness X70 pipeline steels

NASA Astrophysics Data System (ADS)

Hwang, Byoungchul; Kim, Yang Gon; Lee, Sunghak; Kim, Young Min; Kim, Nack J.; Yoo, Jang Yong

2005-08-01

The correlation of microstructure and Charpy V-notch (CVN) impact properties of a high-toughness API X70 pipeline steel was investigated in this study. Six kinds of steel were fabricated by varying the hot-rolling conditions, and their microstructures, effective grain sizes, and CVN impact properties were analyzed. The CVN impact test results indicated that the steels rolled in the single-phase region had higher upper-shelf energies (USEs) and lower energy-transition temperatures (ETTs) than the steels rolled in the two-phase region because their microstructures were composed of acicular ferrite (AF) and fine polygonal ferrite (PF). The decreased ETT in the steels rolled in the single-phase region could be explained by the decrease in the overall effective grain size due to the presence of AF having a smaller effective grain size. On the other hand, the absorbed energy of the steels rolled in the two-phase region was considerably lower because a large amount of dislocations were generated inside PFs during rolling. It was further decreased when coarse martensite or cementite was formed during the cooling process.

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

Dynamic Grain Growth in Forsterite Aggregates Experimentally Deformed to High Strain

NASA Astrophysics Data System (ADS)

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

2004-12-01

The dynamics of the outer Earth are largely controlled by olivine rheology. From previous work it has become clear that if olivine rocks are deformed to high strain, substantial weakening may occur before steady state mechanical behaviour is approached. This weakening appears directly related to progressive modification of the grain size distribution through competing effects of dynamic recrystallization and syn-deformational grain growth. However, most of our understanding of these processes in olivine comes from tests on coarse-grained materials that were reduced in grain size during straining by grain size insensitive (dislocation) creep mechanisms. The aim of the present study was to investigate microstructure evolution of fine-grained olivine rocks that coarsen in grain size while deforming by grain size sensitive (GSS) creep. We used fine-grained (~1 μ m) olivine aggregates (i.e., forsterite/Mg2SiO4), containing ~0.5 wt% water and 10 vol% enstatite (MgSiO3). Two types of experiments were carried out: 1) Hot isostatic pressing (HIP) followed by axial compression to varying strains up to a maximum of ~45%, at 600 MPa confining pressure and a temperature of 950°C, 2) HIP treatment without axial deformation. Microstructures were characterized by analyzing full grain size distributions and texture using SEM/EBSD. Our stress-strain curves showed continuous hardening. When samples were temporally unloaded for short time intervals, no difference in flow stress was observed before and after the interruption in straining. Strain rate sensitivity analysis showed a low value of ~1.5 for the stress exponent n. Measured grain sizes show an increase with strain up to a value twice that of the starting value. HIP-only samples showed only minor increase in grain size. A random LPO combined with the low n ~1.5 suggests dominant GSS creep controlled by grain boundary sliding. These results indicate that dynamic grain growth occurs in forsterite aggregates deforming by GSS creep, and we relate the continuous strain hardening to this process. A dynamic grain growth model involving an increase in cellular defect fraction seems best applicable to the grain growth observed in this study. We suggest that the employment of this model to fine-grained olivine rocks can further improve our understanding of the microstructural evolution of this material and related rheological behaviour.

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.

Cryomilled and spark plasma sintered titanium: the evolution of microstructure

NASA Astrophysics Data System (ADS)

Kozlík, Jiří; Becker, Hanka; Harcuba, Petr; Stráský, Josef; Janeček, Milos

2017-05-01

Bulk ultra-fine grained (UFG) commercially pure Ti was prepared by cryogenic milling in liquid argon and subsequent spark plasma sintering (SPS). During cryogenic milling, individual powder particles are repetitively severely deformed by attrition forces. Powder particles were not significantly refined, but due to severe repetitive plastic deformation, ultra-fine grained microstructure emerges within each powder particle. Cryogenic milling can be therefore considered as a specific severe plastic deformation (SPD) method. Compactization of cryomilled powder by SPS technique (also referred to as field assisted sintering technique - FAST) requires significantly lower sintering temperatures and shorter sintering times for successful compaction when compared to any other sintering technique. This is crucial for maintaining the UFG microstructure due to its limited thermal stability. Several specimens were prepared by varying processing parameters, in particular the sintering temperature. The microstructure of powders and compacted samples was observed by scanning electron microscopy (SEM). Increased sintering temperature results in recrystallization and grain growth. A trade-off relationship between the density of compacted material and grain size was identified. Microhardness of the material was found to depend on residual porosity rather than grain size. This contribution presents cryogenic milling and spark plasma sintering as a viable alternative for achieving UFG microstructure in commercially pure Ti.

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

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.

Stress Distribution During Deformation of Polycrystalline Aluminum by Molecular-Dynamics and Finite-Element Modeling

NASA Technical Reports Server (NTRS)

Yamakov, V.; Saether, E.; Phillips, D.; Glaessgen, E. H.

2004-01-01

In this paper, a multiscale modelling strategy is used to study the effect of grain-boundary sliding on stress localization in a polycrystalline microstructure with an uneven distribution of grain size. The development of the molecular dynamics (MD) analysis used to interrogate idealized grain microstructures with various types of grain boundaries and the multiscale modelling strategies for modelling large systems of grains is discussed. Both molecular-dynamics and finite-element (FE) simulations for idealized polycrystalline models of identical geometry are presented with the purpose of demonstrating the effectiveness of the adapted finite-element method using cohesive zone models to reproduce grain-boundary sliding and its effect on the stress distribution in a polycrystalline metal. The yield properties of the grain-boundary interface, used in the FE simulations, are extracted from a MD simulation on a bicrystal. The models allow for the study of the load transfer between adjacent grains of very different size through grain-boundary sliding during deformation. A large-scale FE simulation of 100 grains of a typical microstructure is then presented to reveal that the stress distribution due to grain-boundary sliding during uniform tensile strain can lead to stress localization of two to three times the background stress, thus suggesting a significant effect on the failure properties of the metal.

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.

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.

System and methods to determine and monitor changes in microstructural properties

DOEpatents

Turner, Joseph Alan [Lincoln, NE

2011-05-17

A system and methods with which changes in microstructure properties such as grain size, grain elongation, texture, and porosity of materials can be determined and monitored over time to assess conditions such as stress and defects. The present invention includes a database of data, wherein a first set of data is used for comparison with a second set of data to determine the conditions of the material microstructure.

Grain size and shape evolution of experimentally deformed sediments: the role of slip rate

NASA Astrophysics Data System (ADS)

Balsamo, Fabrizio; Storti, Fabrizio; De Paola, Nicola

2016-04-01

Sediment deformation within fault zones occurs with a broad spectrum of mechanisms which, in turn, depend on intrinsic material properties (porosity, grain size and shape, etc.) and external factors (burial depth, fluid pressure, stress configuration, etc.). Fieldworks and laboratory measurements conducted in the last years in sediments faulted at shallow depth showed that cataclasis and grain size reduction can occur very close to the Earth surface (<1-2 km), and that fault displacement is one of the parameters controlling the amount of grain size, shape, and microtextural modifications in fault cores. In this contribution, we present a new set of microstructural observations combined with grain size and shape distribution data obtained from quart-feldspatic loose sediments (mean grain diameter 0.2 mm) experimentally deformed at different slip rates from subseismic (0.01 mm/s, 0.1 mm/s, 1 mm/s, 1 cm/s, and 10 cm/s) to coseismic slip rates (1 m/s). The experiments were originally performed at sigma n=14 MPa, with the same amount of slip (1.3 m), to constrain the frictional properties of such sediments at shallow confining pressures (<1 km). After the experiments, the granular materials deformed in the 0.1-1 mm-thick slip zones were prepared for both grain size distribution analyses and microstructural and textural analyses in thin sections. Grain size distribution analyses were obtained with a Malvern Mastersizer 3000 particle size laser-diffraction analyser, whereas grain shape data (angularity) were obtained by using image analysis technique on selected SEM-photomicrographs. Microstructural observations were performed at different scales with a standard optical microscope and with a SEM. Results indicate that mean grain diameter progressively decreases with increasing slip rates up to ~20-30 m, and that granulometric curves systematically modify as well, shifting toward finer grain sizes. Obtained fractal dimensions (D) indicate that D increases from ~2.3 up to >3 moving from subseismic to coseismic slip rates. Grain angularity also changes with increasing slip rates, being particles more smoothed and rounded in sediments deformed at coseismic slip rates. As a whole, our results indicate that both grain size and shape distributions of experimentally deformed sediments progressively changes from subseismic to coseismic slip rate, thus helping to understand the deformation mechanisms in natural fault zones and to predict frictional and permeability properties of faults affecting shallow sediments.

The effects of nucleation and solidification mechanisms on the microstructure and thermomechanical response of tin silver copper solder joints

NASA Astrophysics Data System (ADS)

Arfaei, Babak

This work examines the nucleation mechanism of Sn in SnAgCu alloys and its effect on the microstructure of those solder joints. The nucleation rate of Sn in a SAC alloy was obtained by simultaneous calorimetric examination of the isothermal solidification of 88 flip chip Sn-Ag-Cu solder joints. Qualitative agreement with classic nucleation theory was observed, although it was concluded that the spherical cap model cannot be applied to explain the structure of nucleus. It was shown that the solidification temperature significantly affects the microstructure; samples that undercooled less than approximately 40oC revealed one or three large Sn grains, while interlaced twinning was observed in the samples that solidified at lower temperatures. In order to better understand the effect of microstructure on the thermomechanical properties of solder joints, a study of the dependence of room temperature shear fatigue lifetime on Sn grain number and orientation was conducted. This study examined the correlations of variations in fatigue life of solder balls with the microstructure of Sn-Ag-Cu solder. The mean fatigue lifetime was found to be significantly longer for samples with multiple Sn grains than for samples with single Sn grains. For single grain samples, correlations between Sn grain orientation (with respect to the loading direction) and lifetime were observed, providing insight on early failures in SnAgCu solder joints. Correlations between the lifetimes of single Sn grained, SAC205 solder joints with differences in Ag3Sn and Cu6Sn5 precipitate microstructures were investigated. It was found that Ag3Sn precipitates were highly segregated from Cu6Sn 5 precipitates on a length scale of approximately twenty microns. Furthermore, large (factor of two) variations of the Sn dendrite arm size were observed within given samples. Such variations in values of dendrite arm size within a single sample were much larger than observed variations of this parameter between individual samples. Few significant differences were observed in the average size of precipitates in different samples. While the earliest and latest lifetimes of single Sn grained samples were correlated with Sn grain orientation, effects of precipitate microstructure on lifetimes were not clearly delineated.

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.

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

Observations of Fabric Development in Polycrystalline Ice at Basal Pressures: Methods and Initial Results

NASA Astrophysics Data System (ADS)

Breton, D. J.; Baker, I.; Cole, D. M.

2012-12-01

Understanding and predicting the flow of polycrystalline ice is crucial to ice sheet modeling and paleoclimate reconstruction from ice cores. Ice flow rates depend strongly on the fabric (i.e. the distribution of grain sizes and crystallographic orientations) which evolves over time and enhances the flow rate in the direction of applied stress. The mechanisms for fabric evolution in ice have been extensively studied at atmospheric pressures, but little work has been done to observe these processes at the high pressures experienced deep within ice sheets where long-term changes in ice rheology are expected to have significance. We conducted compressive creep tests on a 917 kg m-3 polycrystalline ice specimen at 20 MPa hydrostatic pressure, thus simulating ~2,000 m depth. Initial specimen grain orientations were random, typical grain diameters were 1.2 mm, and the applied creep stress was 0.3 MPa. Subsequent microstructural analyses on the deformed specimen and a similarly prepared, undeformed specimen allowed characterization of crystal fabric evolution under pressure. Our microstructural analysis technique simultaneously collected grain shape and size data from Scanning Electron Microscope (SEM) micrographs and obtained crystallographic orientation data via Electron BackScatter Diffraction (EBSD). Combining these measurements allows rapid analysis of the ice fabric over large numbers of grains, yielding statistically useful numbers of grain size and full c- and a-axis grain orientation data. The combined creep and microstructural data demonstrate pressure-dependent effects on the mechanical and microstructural evolution of polycrystalline ice. We discuss possible mechanisms for the observed phenomena, and future directions for hydrostatic creep testing.

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.

Strain softening during tension in cold drawn Cu–Ag alloys

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

Chang, L.L., E-mail: lilichang@sdu.edu.cn; Wen, S.; Li, S.L.

2015-10-15

Experiments were conducted on Cu–0.1wt.%Ag alloys to evaluate the influence of producing procedures and annealing conditions on microstructure evolution and mechanical properties of Cu–Ag alloys. Optical microscopy (OM), electron back-scattered diffraction (EBSD), X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used for microstructural evaluation and mechanical properties were characterized by tensile tests. The results indicated that hot-extruded Cu–Ag alloys had a typical dynamic recrystallized microstructure with equiaxed grains. Cold drawing at room temperature leaded to partial recrystallized microstructure with a mixture of coarse and fine grains. The dominate {001}<100 > cubic texture formed during hot extrusion was changed tomore » be {112}<111 > copper texture by cold drawing. Strain softening occurred during room temperature tension of cold drawn Cu–Ag alloys with an average grain size of 13–19.7 μm. - Highlights: • Strain softening occurred during tension of Cu–Ag alloys with coarse grain size. • Work hardening was observed in hot-extruded and annealed Cu–0.1wt.%Ag alloys. • Strain softening was ascribed to dynamic recovery and dynamic recrystallization.« less

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.

Multi-passes warm rolling of AZ31 magnesium alloy, effect on evaluation of texture, microstructure, grain size and hardness

NASA Astrophysics Data System (ADS)

Kamran, J.; Hasan, B. A.; Tariq, N. H.; Izhar, S.; Sarwar, M.

2014-06-01

In this study the effect of multi-passes warm rolling of AZ31 magnesium alloy on texture, microstructure, grain size variation and hardness of as cast sample (A) and two rolled samples (B & C) taken from different locations of the as-cast ingot was investigated. The purpose was to enhance the formability of AZ31 alloy in order to help manufacturability. It was observed that multi-passes warm rolling (250°C to 350°C) of samples B & C with initial thickness 7.76mm and 7.73 mm was successfully achieved up to 85% reduction without any edge or surface cracks in ten steps with a total of 26 passes. The step numbers 1 to 4 consist of 5, 2, 11 and 3 passes respectively, the remaining steps 5 to 10 were single pass rolls. In each discrete step a fixed roll gap is used in a way that true strain per step increases very slowly from 0.0067 in the first step to 0.7118 in the 26th step. Both samples B & C showed very similar behavior after 26th pass and were successfully rolled up to 85% thickness reduction. However, during 10th step (27th pass) with a true strain value of 0.772 the sample B experienced very severe surface as well as edge cracks. Sample C was therefore not rolled for the 10th step and retained after 26 passes. Both samples were studied in terms of their basal texture, microstructure, grain size and hardness. Sample C showed an equiaxed grain structure after 85% total reduction. The equiaxed grain structure of sample C may be due to the effective involvement of dynamic recrystallization (DRX) which led to formation of these grains with relatively low misorientations with respect to the parent as cast grains. The sample B on the other hand showed a microstructure in which all the grains were elongated along the rolling direction (RD) after 90 % total reduction and DRX could not effectively play its role due to heavy strain and lack of plastic deformation systems. The microstructure of as cast sample showed a near-random texture (mrd 4.3), with average grain size of 44 & micro-hardness of 52 Hv. The grain size of sample B and C was 14μm and 27μm respectively and mrd intensity of basal texture was 5.34 and 5.46 respectively. The hardness of sample B and C came out to be 91 and 66 Hv respectively due to reduction in grain size and followed the well known Hall-Petch relationship.

Grain Refinement of Freeform Fabricated Ti-6Al-4V Alloy Using Beam/Arc Modulation

NASA Technical Reports Server (NTRS)

Mitzner, Scott; Liu, Stephen; Domack, Marcia S.; Hafley, Robert A.

2012-01-01

Grain refinement can significantly improve the mechanical properties of freeform-fabricated Ti-6Al-4V alloy, promoting increased strength and enhanced isotropy compared with coarser grained material. Large beta-grains can lead to a segregated microstructure, in regard to both alpha-phase morphology and alpha-lath orientation. Beam modulation, which has been used in conventional fusion welding to promote grain refinement, is explored in this study for use in additive manufacturing processes including electron beam freeform fabrication (EBF(sup 3)) and gas-tungsten arc (GTA) deposition to alter solidification behavior and produce a refined microstructure. The dynamic molten pool size induced by beam modulation causes rapid heat flow variance and results in a more competitive grain growth environment, reducing grain size. Consequently, improved isotropy and strength can be achieved with relatively small adjustments to deposition parameters.

Location specific solidification microstructure control in electron beam melting of Ti-6Al-4V

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

Narra, Sneha P.; Cunningham, Ross; Beuth, Jack

Relationships between prior beta grain size in solidified Ti-6Al-4V and melting process parameters in the Electron Beam Melting (EBM) process are investigated. Samples are built by varying a machine-dependent proprietary speed function to cover the process space. Optical microscopy is used to measure prior beta grain widths and assess the number of prior beta grains present in a melt pool in the raster region of the build. Despite the complicated evolution of beta grain sizes, the beta grain width scales with melt pool width. The resulting understanding of the relationship between primary machine variables and prior beta grain widths ismore » a key step toward enabling the location specific control of as-built microstructure in the EBM process. Control of grain width in separate specimens and within a single specimen is demonstrated.« less

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.

Cleavage fracture in pearlitic eutectoid steel

NASA Astrophysics Data System (ADS)

Alexander, D. J.; Bernstein, I. M.

1989-11-01

The effect of microstructure on flow and fracture properties of fully pearlitic steel has been studied by independently varying the prior austenite grain size and the pearlite interlamellar spacing through appropriate heat treatments. The yield strength is independent of the prior austenite grain size but increases as the interlamellar spacing or the temperature decreases. The microstructural dependence can be explained by using a model which assumes that yielding is controlled by dislocation motion in the ferrite lamellae. The critical tensile stress for cleavage fracture is found to be independent of prior austenite grain size, increasing as the interlamellar spacing decreases. The cleavage fracture stress is independent of temperature for fine pearlite but increases as the temperature decreases for coarse pearlite. The associated fracture in blunt notch specimens initiates at inclusions beneath notch surface near the location of maximum tensile stress. From the size of such inclusions, the effective surface energy for cleavage fracture can be directly calculated and is found to be independent of temperature and prior austenite grain size but to increase as the interlamellar spacing decreases, from about 5 to 13 J/m2 for the range of microstructures and temperatures used in this study. Additional measurements of the effective surface energy and further theoretical analyses of the cleavage process are needed.

Microstructure-Tensile Properties Correlation for the Ti-6Al-4V Titanium Alloy

NASA Astrophysics Data System (ADS)

Shi, Xiaohui; Zeng, Weidong; Sun, Yu; Han, Yuanfei; Zhao, Yongqing; Guo, Ping

2015-04-01

Finding the quantitative microstructure-tensile properties correlations is the key to achieve performance optimization for various materials. However, it is extremely difficult due to their non-linear and highly interactive interrelations. In the present investigation, the lamellar microstructure features-tensile properties correlations of the Ti-6Al-4V alloy are studied using an error back-propagation artificial neural network (ANN-BP) model. Forty-eight thermomechanical treatments were conducted to prepare the Ti-6Al-4V alloy with different lamellar microstructure features. In the proposed model, the input variables are microstructure features including the α platelet thickness, colony size, and β grain size, which were extracted using Image Pro Plus software. The output variables are the tensile properties, including ultimate tensile strength, yield strength, elongation, and reduction of area. Fourteen hidden-layer neurons which can make ANN-BP model present the most excellent performance were applied. The training results show that all the relative errors between the predicted and experimental values are within 6%, which means that the trained ANN-BP model is capable of providing precise prediction of the tensile properties for Ti-6Al-4V alloy. Based on the corresponding relations between the tensile properties predicted by ANN-BP model and the lamellar microstructure features, it can be found that the yield strength decreases with increasing α platelet thickness continuously. However, the α platelet thickness exerts influence on the elongation in a more complicated way. In addition, for a given α platelet thickness, the yield strength and the elongation both increase with decreasing β grain size and colony size. In general, the β grain size and colony size play a more important role in affecting the tensile properties of Ti-6Al-4V alloy than the α platelet thickness.

Microstructure and nanohardness distribution in a polycrystalline Zn deformed by high strain rate impact

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

Dirras, G., E-mail: dirras@univ-paris13.fr; Ouarem, A.; Couque, H.

2011-05-15

Polycrystalline Zn with an average grain size of about 300 {mu}m was deformed by direct impact Hopkinson pressure bar at a velocity of 29 m/s. An inhomogeneous grain structure was found consisting of a center region having large average grain size of 20 {mu}m surrounded by a fine-grained rim with an average grain size of 6 {mu}m. Transmission electron microscopy investigations showed a significant dislocation density in the large-grained area while in the fine-grained rim the dislocation density was negligible. Most probably, the higher strain yielded recrystallization in the outer ring while in the center only recovery occurred. The hardeningmore » effect of dislocations overwhelms the smaller grain size strengthening in the center part resulting in higher nanohardness in this region than in the outer ring. - Graphical Abstract: (a): EBSD micrograph showing the initial microstructure of polycrystalline Zn that was subsequently submitted to high strain rate impact. (b): an inhomogeneous grain size refinement was obtained which consists of a central coarse-grained area, surrounded by a fine-grained recrystallized rim. The black arrow points to the disc center. Research Highlights: {yields} A polycrystalline Zn specimen was submitted to high strain rate impact loading. {yields} Inhomogeneous grain refinement occurred due to strain gradient in impacted sample. {yields} A fine-grained recrystallized rim surrounded the coarse-grained center of specimen. {yields} The coarse-grained center exhibited higher hardness than the fine-grained rim. {yields} The higher hardness of the center was caused by the higher dislocation density.« less

Grain size distribution and microstructures of experimentally sheared granitoid gouge at coseismic slip rates - Criteria to distinguish seismic and aseismic faults?

NASA Astrophysics Data System (ADS)

Stünitz, Holger; Keulen, Nynke; Hirose, Takehiro; Heilbronner, Renée

2010-01-01

Microstructures and grain size distribution from high velocity friction experiments are compared with those of slow deformation experiments of Keulen et al. (2007, 2008) for the same material (Verzasca granitoid). The mechanical behavior of granitoid gouge in fast velocity friction experiments at slip rates of 0.65 and 1.28 m/s and normal stresses of 0.4-0.9 MPa is characterized by slip weakening in a typical exponential friction coefficient vs displacement relationship. The grain size distributions yield similar D-values (slope of frequency versus grain size curve = 2.2-2.3) as those of slow deformation experiments (D = 2.0-2.3) for grain sizes larger than 1 μm. These values are independent of the total displacement above a shear strain of about γ = 20. The D-values are also independent of the displacement rates in the range of ˜1 μm/s to ˜1.3 m/s and do not vary in the normal stress range between 0.5 MPa and 500 MPa. With increasing displacement, grain shapes evolve towards more rounded and less serrated grains. While the grain size distribution remains constant, the progressive grain shape evolution suggests that grain comminution takes place by attrition at clast boundaries. Attrition produces a range of very small grain sizes by crushing with a D <-value = 1. The results of the study demonstrate that most cataclastic and gouge fault zones may have resulted from seismic deformation but the distinction of seismic and aseismic deformation cannot be made on the basis of grain size distribution.

Microstructure as a function of the grain size distribution for packings of frictionless disks: Effects of the size span and the shape of the distribution.

PubMed

Estrada, Nicolas; Oquendo, W F

2017-10-01

This article presents a numerical study of the effects of grain size distribution (GSD) on the microstructure of two-dimensional packings of frictionless disks. The GSD is described by a power law with two parameters controlling the size span and the shape of the distribution. First, several samples are built for each combination of these parameters. Then, by means of contact dynamics simulations, the samples are densified in oedometric conditions and sheared in a simple shear configuration. The microstructure is analyzed in terms of packing fraction, local ordering, connectivity, and force transmission properties. It is shown that the microstructure is notoriously affected by both the size span and the shape of the GSD. These findings confirm recent observations regarding the size span of the GSD and extend previous works by describing the effects of the GSD shape. Specifically, we find that if the GSD shape is varied by increasing the proportion of small grains by a certain amount, it is possible to increase the packing fraction, increase coordination, and decrease the proportion of floating particles. Thus, by carefully controlling the GSD shape, it is possible to obtain systems that are denser and better connected, probably increasing the system's robustness and optimizing important strength properties such as stiffness, cohesion, and fragmentation susceptibility.

Effects of laser power density and initial grain size in laser shock punching of pure copper foil

NASA Astrophysics Data System (ADS)

Zheng, Chao; Zhang, Xiu; Zhang, Yiliang; Ji, Zhong; Luan, Yiguo; Song, Libin

2018-06-01

The effects of laser power density and initial grain size on forming quality of holes in laser shock punching process were investigated in the present study. Three different initial grain sizes as well as three levels of laser power densities were provided, and then laser shock punching experiments of T2 copper foil were conducted. Based upon the experimental results, the characteristics of shape accuracy, fracture surface morphology and microstructures of punched holes were examined. It is revealed that the initial grain size has a noticeable effect on forming quality of holes punched by laser shock. The shape accuracy of punched holes degrades with the increase of grain size. As the laser power density is enhanced, the shape accuracy can be improved except for the case in which the ratio of foil thickness to initial grain size is approximately equal to 1. Compared with the fracture surface morphology in the quasistatic loading conditions, the fracture surface after laser shock can be divided into three zones including rollover, shearing and burr. The distribution of the above three zones strongly relates with the initial grain size. When the laser power density is enhanced, the shearing depth is not increased, but even diminishes in some cases. There is no obvious change of microstructures with the enhancement of laser power density. However, while the initial grain size is close to the foil thickness, single-crystal shear deformation may occur, suggesting that the ratio of foil thickness to initial grain size has an important impact on deformation behavior of metal foil in laser shock punching process.

Evolution of microstructural disorder in annealed bismuth telluride nanowires

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

Erickson, Kristopher J.; Limmer, Steven J.; Yelton, W. Graham

Controlling the distribution of structural defects in nanostructures is important since such defects can strongly affect critical properties, including thermal and electronic transport. However, characterizing the defect arrangements in individual nanostructures is difficult because of the small length scales involved. Here, we investigate the evolution of microstructural disorder with annealing in electrochemically deposited Bi2Te3 nanowires, which are of interest for thermoelectrics. We combine Convergent Beam Electron Diffraction (CBED) and Scanning Transmission Electron Microscopy (STEM) to provide the necessary spatial and orientational resolution. We find that despite their large initial grain sizes and strong Formula crystallographic texturing, the as-deposited nanowires stillmore » exhibit significant intragranular orientational disorder. Annealing drives both grain growth and a significant reduction in the intragranular disorder. The results are discussed in the context of the existing understanding of the initial microstructure of electrodeposited materials and the understanding of annealing microstructures in both electrochemically deposited and bulk-deformed materials. Finally, this analysis highlights the importance of assessing both the grain size and intragranular disorder in understanding the microstructural evolution of individual nanostructures.« less

Evolution of microstructural disorder in annealed bismuth telluride nanowires

DOE PAGES

Erickson, Kristopher J.; Limmer, Steven J.; Yelton, W. Graham; ...

2017-03-01

Controlling the distribution of structural defects in nanostructures is important since such defects can strongly affect critical properties, including thermal and electronic transport. However, characterizing the defect arrangements in individual nanostructures is difficult because of the small length scales involved. Here, we investigate the evolution of microstructural disorder with annealing in electrochemically deposited Bi2Te3 nanowires, which are of interest for thermoelectrics. We combine Convergent Beam Electron Diffraction (CBED) and Scanning Transmission Electron Microscopy (STEM) to provide the necessary spatial and orientational resolution. We find that despite their large initial grain sizes and strong Formula crystallographic texturing, the as-deposited nanowires stillmore » exhibit significant intragranular orientational disorder. Annealing drives both grain growth and a significant reduction in the intragranular disorder. The results are discussed in the context of the existing understanding of the initial microstructure of electrodeposited materials and the understanding of annealing microstructures in both electrochemically deposited and bulk-deformed materials. Finally, this analysis highlights the importance of assessing both the grain size and intragranular disorder in understanding the microstructural evolution of individual nanostructures.« less

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.

Effect of severe plastic deformation on microstructure and mechanical properties of magnesium and aluminium alloys in wide range of strain rates

NASA Astrophysics Data System (ADS)

Skripnyak, Vladimir; Skripnyak, Evgeniya; Skripnyak, Vladimir; Vaganova, Irina; Skripnyak, Nataliya

2013-06-01

Results of researches testify that a grain size have a strong influence on the mechanical behavior of metals and alloys. Ultrafine grained HCP and FCC metal alloys present higher values of the spall strength than a corresponding coarse grained counterparts. In the present study we investigate the effect of grain size distribution on the flow stress and strength under dynamic compression and tension of aluminium and magnesium alloys. Microstructure and grain size distribution in alloys were varied by carrying out severe plastic deformation during the multiple-pass equal channel angular pressing, cyclic constrained groove pressing, and surface mechanical attrition treatment. Tests were performed using a VHS-Instron servo-hydraulic machine. Ultra high speed camera Phantom V710 was used for photo registration of deformation and fracture of specimens in range of strain rates from 0,01 to 1000 1/s. In dynamic regime UFG alloys exhibit a stronger decrease in ductility compared to the coarse grained material. The plastic flow of UFG alloys with a bimodal grain size distribution was highly localized. Shear bands and shear crack nucleation and growth were recorded using high speed photography.

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.

Strengthening Mechanisms in Thermomechanically Processed NbTi-Microalloyed Steel

NASA Astrophysics Data System (ADS)

Kostryzhev, Andrii G.; Marenych, Olexandra O.; Killmore, Chris R.; Pereloma, Elena V.

2015-08-01

The effect of deformation temperature on microstructure and mechanical properties was investigated for thermomechanically processed NbTi-microalloyed steel with ferrite-pearlite microstructure. With a decrease in the finish deformation temperature at 1348 K to 1098 K (1075 °C to 825 °C) temperature range, the ambient temperature yield stress did not vary significantly, work hardening rate decreased, ultimate tensile strength decreased, and elongation to failure increased. These variations in mechanical properties were correlated to the variations in microstructural parameters (such as ferrite grain size, solid solution concentrations, precipitate number density and dislocation density). Calculations based on the measured microstructural parameters suggested the grain refinement, solid solution strengthening, precipitation strengthening, and work hardening contributed up to 32 pct, up to 48 pct, up to 25 pct, and less than 3 pct to the yield stress, respectively. With a decrease in the finish deformation temperature, both the grain size strengthening and solid solution strengthening increased, the precipitation strengthening decreased, and the work hardening contribution did not vary significantly.

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.

Effect of Molten Pool Size on Microstructure and Tensile Properties of Wire Arc Additive Manufacturing of Ti-6Al-4V Alloy.

PubMed

Wu, Qianru; Lu, Jiping; Liu, Changmeng; Fan, Hongli; Shi, Xuezhi; Fu, Jie; Ma, Shuyuan

2017-07-04

Wire arc additive manufacturing (WAAM) technique is a cost-competitive and efficient technology to produce large structure components in industry domains. Mechanical properties are mainly dominated by the microstructure of the components, which is deeply affected by the molten pool size. In this work, to investigate the effect of the molten pool size on microstructure and mechanical properties of the components, a series of Ti-6Al-4V alloy blocks with different width of molten pool (WMP) ranging from 7 mm to 22 mm were deposited by adjusting the wire feed speed (WFS) from 100 cm/min to 500 cm/min. It is interesting to find that the macrostructure changes from columnar grains to equiaxial grains, and then returns to large columnar grains with the increase of WMP, which is mainly caused by the different cooling rates and thermal gradients. Nonetheless, the tensile properties of the components have a tendency to decline with the increase of WMP.

Effect of Molten Pool Size on Microstructure and Tensile Properties of Wire Arc Additive Manufacturing of Ti-6Al-4V Alloy

PubMed Central

Wu, Qianru; Lu, Jiping; Liu, Changmeng; Fan, Hongli; Shi, Xuezhi; Fu, Jie; Ma, Shuyuan

2017-01-01

Wire arc additive manufacturing (WAAM) technique is a cost-competitive and efficient technology to produce large structure components in industry domains. Mechanical properties are mainly dominated by the microstructure of the components, which is deeply affected by the molten pool size. In this work, to investigate the effect of the molten pool size on microstructure and mechanical properties of the components, a series of Ti-6Al-4V alloy blocks with different width of molten pool (WMP) ranging from 7 mm to 22 mm were deposited by adjusting the wire feed speed (WFS) from 100 cm/min to 500 cm/min. It is interesting to find that the macrostructure changes from columnar grains to equiaxial grains, and then returns to large columnar grains with the increase of WMP, which is mainly caused by the different cooling rates and thermal gradients. Nonetheless, the tensile properties of the components have a tendency to decline with the increase of WMP. PMID:28773107

Microstructural Evaluation of Forging Parameters for Superalloy Disks

NASA Technical Reports Server (NTRS)

Falsey, John R.

2004-01-01

Forgings of nickel base superalloy were formed under several different strain rates and forging temperatures. Samples were taken from each forging condition to find the ASTM grain size, and the as large as grain (ALA). The specimens were mounted in bakelite, polished, etched and then optical microscopy was used to determine grain size. The specimens ASTM grain sizes from each forging condition were plotted against strain rate, forging temperature, and presoak time. Grain sizes increased with increasing forging temperature. Grain sizes also increased with decreasing strain rates and increasing forging presoak time. The ALA had been determined from each forging condition using the ASTM standard method. Each ALA was compared with the ASTM grain size of each forging condition to determine if the grain sizes were uniform or not. The forging condition of a strain rate of .03/sec and supersolvus heat treatment produced non uniform grains indicated by critical grain growth. Other anomalies are noted as well.

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

Metallographic Characterization of Wrought Depleted Uranium

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

Forsyth, Robert Thomas; Hill, Mary Ann

Metallographic characterization was performed on wrought depleted uranium (DU) samples taken from the longitudinal and transverse orientations from specific locations on two specimens. Characterization of the samples included general microstructure, inclusion analysis, grain size analysis, and microhardness testing. Comparisons of the characterization results were made to determine any differences based on specimen, sample orientation, or sample location. In addition, the characterization results for the wrought DU samples were also compared with data obtained from the metallographic characterization of cast DU samples previously characterized. No differences were observed in microstructure, inclusion size, morphology, and distribution, or grain size in regard tomore » specimen, location, or orientation for the wrought depleted uranium samples. However, a small difference was observed in average hardness with regard to orientation at the same locations within the same specimen. The longitudinal samples were slightly harder than the transverse samples from the same location of the same specimen. This was true for both wrought DU specimens. Comparing the wrought DU sample data with the previously characterized cast DU sample data, distinct differences in microstructure, inclusion size, morphology and distribution, grain size, and microhardness were observed. As expected, the microstructure of the wrought DU samples consisted of small recrystallized grains which were uniform, randomly oriented, and equiaxed with minimal twinning observed in only a few grains. In contrast, the cast DU microstructure consisted of large irregularly shaped grains with extensive twinning observed in most grains. Inclusions in the wrought DU samples were elongated, broken and cracked and light and dark phases were observed in some inclusions. The mean inclusion area percentage for the wrought DU samples ranged from 0.08% to 0.34% and the average density from all wrought DU samples was 1.62E+04/cm 2. Inclusions in the cast DU samples were equiaxed and intact with light and dark phases observed in some inclusions. The mean inclusion area percentage for the cast DU samples ranged from 0.93% to 1.00% and the average density from all wrought DU samples was 2.83E+04/cm 2. The average mean grain area from all wrought DU samples was 141 μm 2 while the average mean grain area from all cast DU samples was 1.7 mm2. The average Knoop microhardness from all wrought DU samples was 215 HK and the average Knoop microhardness from all cast DU samples was 264 HK.« less

Determination of grain size distribution function using two-dimensional Fourier transforms of tone pulse encoded images

NASA Technical Reports Server (NTRS)

Generazio, E. R.

1986-01-01

Microstructural images may be tone pulse encoded and subsequently Fourier transformed to determine the two-dimensional density of frequency components. A theory is developed relating the density of frequency components to the density of length components. The density of length components corresponds directly to the actual grain size distribution function from which the mean grain shape, size, and orientation can be obtained.

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.

Processing, Microstructure, and Material Property Relationships Following Friction Stir Welding of Oxide Dispersion Strengthened Steels

DTIC Science & Technology

2013-09-01

2.75), (b) 400 RPM/100 MMPM (HI= 4 ), (c) 300 RPM/50 MMPM (HI= 6 ), and (d) 500 RPM/25 MMPM (HI=10) showing increase in grain size as HI is increased...Heat Index Weld Quality Weld Penetration 200 50 4 Lack of Consolidation Incomplete 300 50 6 Defect-free Full 300 100 3 Lack of Consolidation...Specifically, the grain size for HI= 6 (300 RPM/50 MMPM) is less than the grain size for HI= 4 (400 RPM/100 MMPM); however, grain size did

Modeling of stress distributions on the microstructural level in Alloy 600

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

Kozaczek, K.J.; Petrovic, B.G.; Ruud, C.O.

1995-04-01

Stress distribution in a random polycrystalline material (Alloy 600) was studied using a topologically correct microstructural model. Distributions of von Mises and hydrostatic stresses at the grain vertices, which could be important in intergranular stress corrosion cracking, were analyzed as functions of microstructure, grain orientations and loading conditions. Grain size, shape, and orientation had a more pronounced effect on stress distribution than loading conditions. At grain vertices the stress concentration factor was higher for hydrostatic stress (1.7) than for von Mises stress (1.5). The stress/strain distribution in the volume (grain interiors) is a normal distribution and does not depend onmore » the location of the studied material volume i.e., surface vs/bulk. The analysis of stress distribution in the volume showed the von Mises stress concentration of 1.75 and stress concentration of 2.2 for the hydrostatic pressure. The observed stress concentration is high enough to cause localized plastic microdeformation, even when the polycrystalline aggregate is in the macroscopic elastic regime. Modeling of stresses and strains in polycrystalline materials can identify the microstructures (grain size distributions, texture) intrinsically susceptible to stress/strain concentrations and justify the correctness of applied stress state during the stress corrosion cracking tests. Also, it supplies the information necessary to formulate the local failure criteria and interpret of nondestructive stress measurements.« less

Microstructural evolution and grain growth kinetics of GZ31 magnesium alloy

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

Roostaei, M., E-mail: miladroustaei68@ut.ac.ir

2016-08-15

Grain growth behavior of Mg–3Gd–1Zn (GZ31) magnesium alloy was studied in a wide range of annealing time and temperature to clarify the kinetics of grain growth, microstructural evolution and related metallurgical phenomena. This material exhibited typical normal grain growth mode under annealing conditions with annealing temperature of lower than 300 °C and soaking time of lower than 240 min. However, the abnormality in grain growth was also evident at annealing temperature of 400 °C and 500 °C. The dependence of abnormal grain growth (AGG) at mentioned annealing temperatures upon microstructural features such as dispersed precipitates, which were rich in Znmore » and Gd, was investigated by optical micrographs, X-ray diffraction patterns, scanning electron microscopy images, and energy dispersive X-ray analysis spectra. The bimodality in grain-size distribution histograms also signified the occurrence of AGG. Based on the experimental data on grain growth obtained by annealing treatments, the grain growth exponent and the activation energy were also figured out.« less

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

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.

Experimental study of microstructure changes due to low cycle fatigue of a steel nanocrystallised by Surface Mechanical Attrition Treatment (SMAT)

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

Sun, Z.

Electron Backscatter Diffraction technique is used to characterize the microstructure of 316L steel generated by Surface Mechanical Attrition Treatment (SMAT) before and after low cycle fatigue tests. A grain size gradient is generated from the top surface to the interior of the samples after SMAT so that three main regions can be distinguished below the treated surface: (i) the ultra-fine grain area within 5 μm under the top surface with preferably oriented grains, (ii) the intermediate area where the original grains are partially transformed, and (iii) the edge periphery area where the original grains are just mechanically deformed with themore » presence of plastic slips. Fatigue tests show that cyclic loading does not change the grain orientation spread and does not activate any plastic slip in the ultra-fine grain top surface area induced by SMAT. On the opposite, in the plastically SMAT affected region including the intermediate area and the edge periphery area, new slip systems are activated by low cycle fatigue while the grain orientation spread is increased. These results represent a first very interesting step towards the characterization and understanding of mechanical mechanisms involved during the fatigue of a grain size gradient material. - Highlights: •LCF tests are carried out on specimens processed by SMAT. •EBSD is used to investigate microstructural changes induced by LCF. •A grain size gradient is generated by SMAT from surface to the bulk of the fatigue samples. •New slip systems are activated by LCF and GOS is increased in plastically deformed region. •However, these phenomena are not observed in the top surface ultra-fine grain area.« less

Localized melt-scan strategy for site specific control of grain size and primary dendrite arm spacing in electron beam additive manufacturing

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

Raghavan, Narendran; Simunovic, Srdjan; Dehoff, Ryan

In addition to design geometry, surface roughness, and solid-state phase transformation, solidification microstructure plays a crucial role in controlling the performance of additively manufactured components. Crystallographic texture, primary dendrite arm spacing (PDAS), and grain size are directly correlated to local solidification conditions. We have developed a new melt-scan strategy for inducing site specific, on-demand control of solidification microstructure. We were able to induce variations in grain size (30 μm–150 μm) and PDAS (4 μm - 10 μm) in Inconel 718 parts produced by the electron beam additive manufacturing system (Arcam®). A conventional raster melt-scan resulted in a grain size ofmore » about 600 μm. The observed variations in grain size with different melt-scan strategies are rationalized using a numerical thermal and solidification model which accounts for the transient curvature of the melt pool and associated thermal gradients and liquid-solid interface velocities. The refinement in grain size at high cooling rates (>104 K/s) is also attributed to the potential heterogeneous nucleation of grains ahead of the epitaxially growing solidification front. The variation in PDAS is rationalized using a coupled numerical-theoretical model as a function of local solidification conditions (thermal gradient and liquid-solid interface velocity) of the melt pool.« less

Microstructure evolution during helium irradiation and post-irradiation annealing in a nanostructured reduced activation steel

NASA Astrophysics Data System (ADS)

Liu, W. B.; Ji, Y. Z.; Tan, P. K.; Zhang, C.; He, C. H.; Yang, Z. G.

2016-10-01

Severe plastic deformation, intense single-beam He-ion irradiation and post-irradiation annealing were performed on a nanostructured reduced activation ferritic/martensitic (RAFM) steel to investigate the effect of grain boundaries (GBs) on its microstructure evolution during these processes. A surface layer with a depth-dependent nanocrystalline (NC) microstructure was prepared in the RAFM steel using surface mechanical attrition treatment (SMAT). Microstructure evolution after helium (He) irradiation (24.8 dpa) at room temperature and after post-irradiation annealing was investigated using Transmission Electron Microscopy (TEM). Experimental observation shows that GBs play an important role during both the irradiation and the post-irradiation annealing process. He bubbles are preferentially trapped at GBs/interfaces during irradiation and cavities with large sizes are also preferentially trapped at GBs/interfaces during post-irradiation annealing, but void denuded zones (VDZs) near GBs could not be unambiguously observed. Compared with cavities at GBs and within larger grains, cavities with smaller size and higher density are found in smaller grains. The average size of cavities increases rapidly with the increase of time during post-irradiation annealing at 823 K. Cavities with a large size are observed just after annealing for 5 min, although many of the cavities with small sizes also exist after annealing for 240 min. The potential mechanism of cavity growth behavior during post-irradiation annealing is also discussed.

High pressure FAST of nanocrystalline barium titanate

DOE PAGES

Fraga, Martin B.; Delplanque, Jean -Pierre; Yang, Nancy; ...

2016-06-01

Here, this work studies the microstructural evolution of nanocrystalline (<1 µm) barium titanate (BaTiO 3), and presents high pressure in field-assisted sintering (FAST) as a robust methodology to obtain >100 nm BaTiO 3 compacts. Using FAST, two commercial ~50 nm powders were consolidated into compacts of varying densities and grain sizes. Microstructural inhomogeneities were investigated for each case, and an interpretation is developed using a modified Monte Carlo Potts (MCP) simulation. Two recurrent microstructural inhomogeneities are highlighted, heterogeneous grain growth and low-density regions, both ubiqutously present in all samples to varying degrees. In the worst cases, HGG presents an areamore » coverage of 52%. Because HGG is sporadic but homogenous throughout a sample, the catalyst (e.g., the local segregation of species) must be, correspondingly, distributed in a homogenous manner. MCP demonstrates that in such a case, a large distance between nucleating abnormal grains is required—otherwise abnormal grains prematurely impinge on each other, and their size is not distinguishable from that of normal grains. Compacts sintered with a pressure of 300 MPa and temperatures of 900 °C, were 99.5% dense and had a grain size of 90±24 nm. These are unprecedented results for commercial BaTiO 3 powders or any starting powder of 50 nm particle size—other authors have used 16 nm lab-produced powder to obtain similar results.« less

Study of grain structure evolution during annealing of a twin-roll-cast Mg alloy

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

Tripathi, A.; Department of Metallurgical Engineering and Materials Science, IIT Bombay; Department of Materials Engineering, Monash University

2016-04-15

The evolution of microstructure under static annealing was studied for mid-thickness section of a twin-roll-cast (TRC) magnesium alloy. Annealing was performed at 300 °C and 500 °C for different times. Microstructural evolution was quantitatively analyzed, from optical micrographs, using grain path envelope analysis. Additional information from electron backscatter diffraction (EBSD) was used for addressing the possible mechanism(s). It was found that the TRC structure had a bimodal grain size, which was preserved even after annealing at 300 °C. However, the annealing at 500 °C led to a unimodal grain size. This difference in the grain size distribution created a contrastingmore » behavior in the normalized standard deviations. This was primarily attributed to a competition between recovery and recrystallization, and their respective dominance at 300° and 500 °C. A deformation induced recrystallization recovery (DIRR) model was proposed. The proposed model could successfully address the experimental microstructural evolution. - Highlights: • Annealing of twin roll cast (TRC) magnesium alloy was done at temperatures of 300 °C and 500 °C. • TRC had bimodal structure. Bimodality preserved for annealing at 300 °C. Annealing at 500 °C led to unimodal structure. • Grain evolution was described based on the competition between recovery and recrystallization. • Deformation induced recrystallization recovery (DIRR) mechanistic model was developed.« less

Oxidizing annealing effects on VO2 films with different microstructures

NASA Astrophysics Data System (ADS)

Dou, Yan-Kun; Li, Jing-Bo; Cao, Mao-Sheng; Su, De-Zhi; Rehman, Fida; Zhang, Jia-Song; Jin, Hai-Bo

2015-08-01

Vanadium dioxide (VO2) films have been prepared by direct-current magnetron sputter deposition on m-, a-, and r-plane sapphire substrates. The obtained VO2 films display different microstructures depending on the orientation of sapphire substrates, i.e. mixed microstructure of striped grains and equiaxed grains on m-sapphire, big equiaxed grains on a-sapphire and fine-grained microstructure on r-sapphire. The VO2 films were treated by the processes of oxidation in air. The electric resistance and infrared transmittance of the oxidized films were characterized to examine performance characteristics of VO2 films with different microstructures in oxidation environment. The oxidized VO2 films on m-sapphire exhibit better electrical performance than the other two films. After air oxidization for 600 s at 450 °C, the VO2 films on m-sapphire show a resistance change of 4 orders of magnitude over the semiconductor-to-metal transition. The oxidized VO2 films on a-sapphire have the highest optical modulation efficiency in infrared region compared to other samples. The different performance characteristics of VO2 films are understood in terms of microstructures, i.e. grain size, grain shape, and oxygen vacancies. The findings reveal the correlation of microstructures and performances of VO2 films, and provide useful knowledge for the design of VO2 materials to different applications.

Microstructure and Mechanical Properties of Ultrafine-Grained Al-6061 Prepared Using Intermittent Ultrasonic-Assisted Equal-Channel Angular Pressing

NASA Astrophysics Data System (ADS)

Lu, Jianxun; Wu, Xiaoyu; Wu, Zhaozhi; Liu, Zhiyuan; Guo, Dengji; Lou, Yan; Ruan, Shuangchen

2017-10-01

Equal-channel angular pressing (ECAP) is an efficient technique to achieve grain refinement in a wide range of materials. However, the extrusion process requires an excessive extrusion force, the microstructure of ECAPed specimens scatters heterogeneously because of considerable fragmentation of the structure and strain heterogeneity, and the resultant ultrafine grains exhibit poor thermal stability. The intermittent ultrasonic-assisted ECAP (IU-ECAP) approach was proposed to address these issues. In this work, ECAP and IU-ECAP were applied to produce ultrafine-grained Al-6061 alloys, and the differences in their mechanical properties, microstructural characteristics, and thermal stability were investigated. Mechanical testing demonstrated that the necessary extrusion force for IU-ECAP was significantly reduced; even more, the microhardness and ultimate tensile strength were strengthened. In addition, the IU-ECAPed Al alloy exhibited a smaller grain size with a more homogeneous microstructure. X-ray diffraction analysis indicated that the intensities of the textures were weakened using IU-ECAP, and a more homogeneous microstructure and larger dislocation densities were obtained. Investigation of the thermal stability revealed that the ultrafine-grained materials produced using IU-ECAP recrystallized at higher temperature or after longer time; the materials thus exhibited improved thermal stability.

Comparisons of Fabric Strength and Development in Polycrystalline Ice at Atmospheric and Basal Hydrostatic Pressures

NASA Astrophysics Data System (ADS)

Breton, Daniel; Baker, Ian; Cole, David

2013-04-01

Understanding and predicting the flow of polycrystalline ice is crucial to ice sheet modeling and paleoclimate reconstruction from ice cores. Ice flow rates depend strongly on the fabric (i.e. the distribution of grain sizes and crystallographic orientations) which evolves over time and enhances the flow rate in the direction of applied stress. The mechanisms for fabric evolution in ice have been extensively studied at atmospheric pressures, but little work has been done to observe these processes at the high pressures experienced deep within ice sheets where long-term changes in ice rheology are expected to have significance. We conducted compressive creep tests to ~10% strain on 917 kg m-3, initially randomly-oriented polycrystalline ice specimens at 0.1 (atmospheric) and 20 MPa (simulating ~2,000 m depth) hydrostatic pressures, performing microstructural analyses on the resulting deformed specimens to characterize the evolution and strength of crystal fabric. Our microstructural analysis technique simultaneously collects grain shape and size data from Scanning Electron Microscope (SEM) micrographs and obtains crystallographic orientation data via Electron BackScatter Diffraction (EBSD). Combining these measurements allows rapid analysis of the ice fabric over large numbers of grains, yielding statistically useful numbers of grain size and orientation data. We present creep and microstructural data to demonstrate pressure-dependent effects on the mechanical and microstructural evolution of polycrystalline ice and discuss possible mechanisms for the observed differences.

Using Antifreeze Proteins to understand ice microstructure evolution

NASA Astrophysics Data System (ADS)

Bayer-Giraldi, Maddalena; Azuma, Nobuhiko; Takata, Morimasa; Weikusat, Christian; Kondo, Hidemasa; Kipfstuhl, Sepp

2017-04-01

Polar ice sheets are considered a unique climate archive. The chemical analysis of its impurities and the development of its microstructure with depth give insight in past climate conditions as well as in the development of the ice sheet with time and deformation. Microstructural patterns like small grain size observed in specific depths are thought to be linked to the retarding effect of impurities on ice grain growth. Clear evidence of size or chemical composition of the impurities causing this effect is missing, but in this context a major role of nanoparticles has been suggested. In order to shed light on different mechanisms by which nanoparticles can control microstructure development we used antifreeze proteins (AFPs) as proxies for particles in ice. These proteins are small nanoparticles, approx. 5 nm in size, with the special characteristics of firmly binding to ice through several hydrogen bonds. We used AFPs from the sea-ice microalgae Fragilariopsis cylindrus (fcAFPs) in bubble-free, small-grained polycrystalline ice obtained by the phase-transition size refinement method. We explain how fcAFP bind to ice by presenting the 3-D-protein structure model inferred by X-ray structure analysis, and show the importance of the chemical interaction between particles and ice in controlling normal grain growth, comparing fcAFPs to other protein nanoparticles. We used modifications of fcAFPs for particle localization through fluorescence spectroscopy. Furthermore, the effect of fcAFPs on the driving factors for ice deformation during creep, i.e. on internal dislocations due to incorporation within the lattice and on the mobility of grain boundaries due to pinning, makes these proteins particularly interesting in studying the process of ice deformation.

Microstructural evolution during reheating of A356 machining chips at semisolid state

NASA Astrophysics Data System (ADS)

Wang, Fang; Zhang, Wen-qiang; Xiao, Wen-long; Yamagata, Hiroshi; Ma, Chao-li

2017-08-01

The microstructural evolution of A356 machining chips in the semisolid state was studied at different temperatures and holding times. The results showed that the elongated α-Al grains first recrystallized in the semisolid state and then became globular with a high shape factor (SF). Both the temperature and the holding time clearly affected the grain size and SF. When the heating temperature or holding time was increased, the grain size and SF gradually increased and finally became stable. Moreover, the Vickers hardness of primary α-Al grains gradually decreased with increasing heating temperature. The optimal slurry for semisolid processing, with a good combination of grain size and SF, was obtained when the chips were held at 600°C for 15 min. The semisolid slurry of A356 chips exhibited a lower coarsening rate of α-Al grains than those produced by most of the conventional semisolid processes. The coarsening coefficient was determined to be 436 μm3·s-1 on the basis of the linear Lifshitz-Slyozov-Wagner (LSW) relationship.

Effect of Hierarchical Microstructures of Lath Martensite on the Transitional Behavior of Fatigue Crack Growth Rate

NASA Astrophysics Data System (ADS)

Yang, Ming; Zhong, Yi; Liang, Yi-long

2018-04-01

In this study, the fatigue-crack growth (FCG) behavior of 20CrMTiH steel with different substructure sizes was investigated. The results showed that coarsen microstructures exhibit excellent growth resistance. Moreover, two transitional behaviors were observed in the FCG curves of all specimens. The first transition point occurs in the near-threshold regime, whereas the second transition point occurs in the Paris regime. A comparison of substructure size to cyclic plastic size showed that the block size is almost equal to cyclic plastic size at ΔKT1, indicating that block size is an effective grain size to control the first transitional behavior of fatigue-crack propagation, whereas the second transitional behavior is related to the packet width or grain size. According to the fracture morphology, the fracture mechanism above and below the transition point responsible for the above phenomenon were distinguished. In addition, two prediction models based on microstructure size were established for lath martensite to evaluate the threshold and stress intensity factor range at the transition point.

Microstructure and Charpy impact properties of 12 14Cr oxide dispersion-strengthened ferritic steels

NASA Astrophysics Data System (ADS)

Oksiuta, Z.; Baluc, N.

2008-02-01

This paper describes the microstructure and Charpy impact properties of 12-14 Cr ODS ferritic steels fabricated by mechanical alloying of pure Fe, Cr, W, Ti and Y 2O 3 powders in a Retsch ball mill in argon atmosphere, followed by hot isostatic pressing at 1100 °C under 200 MPa for 4 h and heat treatment at 850 °C for 1 h. Weak Charpy impact properties were obtained in the case of both types of as-hipped materials. In the case of 14Cr materials, the weak Charpy properties appeared related to a bimodal grain size distribution and a heterogeneous dislocation density between the coarse and fine grains. No changes in microstructure were evidenced after heat treatment at 850 °C. Significant improvement in the transition temperature and upper shelf energy of 12Cr materials was obtained by heat treatment at 850 °C for 1 h, which was attributed to the formation of smaller grains, homogenous in size and containing fewer dislocations, with respect to the as-hipped microstructure. This modified microstructure results in a good compromise between strength and Charpy impact properties.

Evolution of microstructure and surface topography of gold thin films under thermal annealing

NASA Astrophysics Data System (ADS)

Dash, P.; Rath, H.; Dash, B. N.; Mallick, P.; Basu, T.; Som, T.; Singh, U. P.; Mishra, N. C.

2012-07-01

In the present study, we probe into evolution of microstructure and surface morphology of gold thin films of 10 to 50 nm thickness deposited on Si (100) substrate by thermal evaporation method. These films were annealed at 250°C under vacuum. The as-deposited and annealed films were characterized by glancing angle X-Ray diffraction (GAXRD) and atomic force microscopy (AFM), techniques. XRD indicated improvement of crystallinity up to 2 hours of annealing and degradation of the same thereafter. In agreement with XRD result, the grain size distribution histogram obtained from AFM indicated grain growth with annealing time up to 2 hours and saturation or decrease of grain size thereafter. The observed result is explained by the occurrence of two competing phenomena like roughening induced grain growth and smoothening induced inhibition of grain growth with increasing annealing time.

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.

SLM processing-microstructure-mechanical property correlation in an aluminum alloy produced by additive manufacturing

NASA Astrophysics Data System (ADS)

Alejos, Martin Fernando

Additive manufacturing has become a highly researched topic in recent years all over the world. The current research evaluates the merits of additive manufacturing based on the mechanical, microstructural, and fracture properties of additive manufactured AlSi10Mg test specimens. The additive manufactured build plates consisted of tensile and fatigue test specimens. They were printed in the 0°, 30°, 60°, and 90° orientations relative to the build platform. Tensile and dynamic fatigue tests were conducted followed by microstructural characterization and fracture analysis. A wrought 6061 T6 aluminum alloy was also tested for comparison. Tensile tests revealed similar ultimate tensile strengths for all aluminum tensile specimens (350-380 MPa). Fatigue strength was greatest for wrought 6061 T6 aluminum (175 MPa). The fatigue behavior was a strong function of build orientation for the additive manufactured specimens. The 0°, 30°, and 60° orientations had fatigue strengths close to 104 MPa while the 90° orientation had a fatigue strength of 125 MPa. All test specimens failed primarily in a ductile manner. The effect of laser power, hatch spacing, and scan speed were also studied using microstructural analysis. Increasing laser power decreased grain size and void size. Increasing scan speed led to the formation of columnar grains. Increasing hatch spacing decreased grain size and the amount of voids present in the microstructure.

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.

Computational study of deformation mechanisms and grain size evolution in granulites - Implications for the rheology of the lower crust

NASA Astrophysics Data System (ADS)

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

2017-05-01

Most of granulite terrains worldwide are characterized by large mean grain sizes of 1 mm or more. An important exception are the high-pressure felsic granulites in the Bohemian Massif, the European Variscan belt. There, recrystallization of original coarse-grained ternary feldspar led to formation of a fine-grained (∼100 μm) mixed matrix dominated by plagioclase and K-feldspar. This change occurred at temperatures of ∼850 °C and was probably caused by chemically induced decomposition related to slight cooling and enhanced by deformation during continental collision. The resulting microstructure shows indications of diffusion creep assisted by melt-enhanced grain-boundary sliding. Further on, minor coarsening occurred associated with deformation by dislocation creep and aggregation of mineral phases. Using a thermodynamics-based model of grain size evolution we show that stability of the fine-grained microstructure crucially depends on Zener pinning in the two-phase mineral matrix. Pinning efficiently hinders grain growth, and the small grain size that resulted from the ternary feldspar decomposition can be stable even at high temperatures. The late switch from the grain-size-sensitive creep to dislocation creep is rather difficult to explain by temperature and strain rate (or stress) changes only. However, a simple incorporation of melt solidification can successfully simulate this behavior. Alternatively, the switch and the associated grain size growth can be related to mineral phase aggregation at lower pressure-temperature conditions resulting into a decrease of pinning efficiency. This study suggests that the fine grain size of the Bohemian granulites, in contrast to the common coarse-grained type, stems from abrupt recrystallization during the high-pressure high-temperature conditions, and pinning in the fine-grained matrix. Such a process may in some cases significantly and suddenly reduce the strength of the lower continental crust and allow for its efficient redistribution.

Effect of microstructure on the thermoelectric performance of La{sub 1−x}Sr{sub x}CoO{sub 3}

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

Viskadourakis, Z.; Department of Mechanical and Manufacturing Engineering, University of Cypruss, 75 Kallipoleos Avenue, P.O. Box 20537, 1678 Nicosia; Athanasopoulos, G.I.

We present a case where the microstructure has a profound effect on the thermoelectric properties of oxide compounds. Specifically, we have investigated the effect of different sintering treatments on La{sub 1−x}Sr{sub x}CoO{sub 3} samples synthesized using the Pechini method. We found that the samples, which are dense and consist of inhomogeneously-mixed grains of different size, exhibit both higher Seebeck coefficient and thermoelectric figure of merit than the samples, which are porous and consist of grains with almost identical size. The enhancement of Seebeck coefficient in the dense samples is attributed to the so-called “energy-filtering” mechanism that is related to themore » energy barrier of the grain boundary. On the other hand, the thermal conductivity for the porous compounds is significantly reduced in comparison to the dense compounds. It is suggested that a fine-manipulation of grain size ratio combined with a fine-tuning of porosity could considerably enhance the thermoelectric performance of oxides. - Graphical abstract: The enhancement of the dimensionless thermoelectric figure ZT of merit is presented for two equally Sr-doped LaCoO3 compounds, possessing different microstructure, indicating the effect of the latter to the thermoelectric performance of the La{sub 1−x}Sr{sub x}CoO{sub 3} solid solution. - Highlights: • Electrical and thermal transport properties are affected by the microstructure in La{sub 1−x}Sr{sub x}CoO{sub 3} polycrystalline materials. • Coarse/fine grain size distribution enhances the Seebeck coefficient. • Porosity reduces the thermal conductivity in La{sub 1−x}Sr{sub x}CoO{sub 3} polycrystalline samples. • The combination of large/small grain ratio distribution with the high porosity may result to the enhancement of the thermoelectric performance of the material.« less

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.

Microstructural investigations on carbonate fault core rocks in active extensional fault zones from the central Apennines (Italy)

NASA Astrophysics Data System (ADS)

Cortinovis, Silvia; Balsamo, Fabrizio; Storti, Fabrizio

2017-04-01

The study of the microstructural and petrophysical evolution of cataclasites and gouges has a fundamental impact on both hydraulic and frictional properties of fault zones. In the last decades, growing attention has been payed to the characterization of carbonate fault core rocks due to the nucleation and propagation of coseismic ruptures in carbonate successions (e.g., Umbria-Marche 1997, L'Aquila 2009, Amatrice 2016 earthquakes in Central Apennines, Italy). Among several physical parameters, grain size and shape in fault core rocks are expected to control the way of sliding along the slip surfaces in active fault zones, thus influencing the propagation of coseismic ruptures during earthquakes. Nevertheless, the role of grain size and shape distribution evolution in controlling the weakening or strengthening behavior in seismogenic fault zones is still not fully understood also because a comprehensive database from natural fault cores is still missing. In this contribution, we present a preliminary study of seismogenic extensional fault zones in Central Apennines by combining detailed filed mapping with grain size and microstructural analysis of fault core rocks. Field mapping was aimed to describe the structural architecture of fault systems and the along-strike fault rock distribution and fracturing variations. In the laboratory we used a Malvern Mastersizer 3000 granulometer to obtain a precise grain size characterization of loose fault rocks combined with sieving for coarser size classes. In addition, we employed image analysis on thin sections to quantify the grain shape and size in cemented fault core rocks. The studied fault zones consist of an up to 5-10 m-thick fault core where most of slip is accommodated, surrounded by a tens-of-meters wide fractured damage zone. Fault core rocks consist of (1) loose to partially cemented breccias characterized by different grain size (from several cm up to mm) and variable grain shape (from very angular to sub-rounded), and (2) very fine-grained gouges (< 1 mm) localized along major and minor mirror-like slip surfaces. Damage zones mostly consist of fractured rocks and, locally, pulverized rocks. Collectively, field observations and laboratory analyses indicate that within the fault cores of the studied fault zones, grain size progressively decreases approaching the master slip surfaces. Furthermore, grain shape changes from very angular to sub-rounded clasts moving toward the master slip surfaces. These features suggest that the progressive evolution of grain size and shape distributions within fault cores may have determined the development of strain localization by the softening and cushioning effects of smaller particles in loose fault rocks.

Microstructural and petrophysical characterization of a "structurally oversimplified" fault zone in poorly lithified sands: evidence for a coseismic rupture?

NASA Astrophysics Data System (ADS)

Balsamo, Fabrizio; Storti, Fabrizio

2010-05-01

We studied an extensional fault zone developed in poorly lithified, quartz-rich high porosity sandy sediments of the seismically active Crotone basin (southern Italy). The fault zone cuts across interlayered fine- to coarse-grained sands and consists of a cm-thick, discrete fault core embedded in virtually undeformed wall sediments. Consequently, it can be described as "structurally oversimplified" due to the lack of footwall and hanging wall damage zones. We acquired microstructural, grain size, grain shape, porosity, mineralogical and permeability data to investigate the influence of initial sedimentological characteristics of sands on the final faulted granular products and related hydrologic properties. Faulting evolves by a general grain size and porosity reduction with a combination of intragranular fracturing, spalling, and flaking of grain edges, irrespective of grain mineralogy. The dominance of cataclasis, also confirmed by fractal dimensions >2.6, is generally not expected at a deformation depth <1 km. Coarse-grained sand shows a much higher comminution intensity, grain shape variations and permeability drop than fine-grained sands. This is because coarser aggregates have (i) fewer grain-to-grain contacts for a given area, which results in higher stress concentration at contact points, and (ii) a higher probability of pre-existing intragranular microstructural defects that result in a lower grain strength. The peculiar structural architecture, the dominance of cataclasis over non-destructive particulate flow, and the compositional variations of clay minerals in the fault core, strongly suggest that the studied fault zone developed by a coseismic rupture.

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.

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.

Effect of grain morphology on gas bubble swelling in UMo fuels – A 3D microstructure dependent Booth model

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

Hu, Shenyang; Burkes, Douglas; Lavender, Curt A.

2016-11-01

A three dimensional microstructure dependent swelling model is developed for studying the fission gas swelling kinetics in irradiated nuclear fuels. The model is extended from the Booth model [1] in order to investigate the effect of heterogeneous microstructures on gas bubble swelling kinetics. As an application of the model, the effect of grain morphology, fission gas diffusivity, and spatial dependent fission rate on swelling kinetics are simulated in UMo fuels. It is found that the decrease of grain size, the increase of grain aspect ratio for the grain having the same volume, and the increase of fission gas diffusivity (fissionmore » rate) cause the increase of swelling kinetics. Other heterogeneities such as second phases and spatial dependent thermodynamic properties including diffusivity of fission gas, sink and source strength of defects could be naturally integrated into the model to enhance the model capability.« less

Quantifying the effect of 3D spatial resolution on the accuracy of microstructural distributions

NASA Astrophysics Data System (ADS)

Loughnane, Gregory; Groeber, Michael; Uchic, Michael; Riley, Matthew; Shah, Megna; Srinivasan, Raghavan; Grandhi, Ramana

The choice of spatial resolution for experimentally-collected 3D microstructural data is often governed by general rules of thumb. For example, serial section experiments often strive to collect at least ten sections through the average feature-of-interest. However, the desire to collect high resolution data in 3D is greatly tempered by the exponential growth in collection times and data storage requirements. This paper explores the use of systematic down-sampling of synthetically-generated grain microstructures to examine the effect of resolution on the calculated distributions of microstructural descriptors such as grain size, number of nearest neighbors, aspect ratio, and Ω3.

Effect of Hypoeutectic Boron Additions on the Grain Size and Mechanical Properties of Ti-6Al-4V Manufactured with Powder Bed Electron Beam Additive Manufacturing

NASA Astrophysics Data System (ADS)

Mahbooba, Zaynab; West, Harvey; Harrysson, Ola; Wojcieszynski, Andrzej; Dehoff, Ryan; Nandwana, Peeyush; Horn, Timothy

2017-03-01

In additive manufacturing, microstructural control is feasible via processing parameter alteration. However, the window for parameter variation for certain materials, such as Ti-6Al-4V, is limited, and alternative methods must be employed to customize microstructures. Grain refinement and homogenization in cast titanium alloys has been demonstrated through the addition of hypoeutectic concentrations of boron. This work explores the influence of 0.00 wt.%, 0.25 wt.%, 0.50 wt.%, and 1.0 wt.% boron additions on the microstructure and bulk mechanical properties of Ti-6Al-4V samples fabricated in an Arcam A2 electron beam melting (EBM) system with commercial processing parameters for Ti-6Al-4V. Analyses of EBM fabricated Ti-6Al-4V + B indicate that the addition of 0.25-1.0 wt.% boron progressively refines the grain structure, and it improves hardness and elastic modulus. Despite a reduction in size, the β grain structure remained columnar as a result of directional heat transfer during EBM fabrication.

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

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.

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

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

The influence of sintering conditions on microstructure and mechanical properties of titanium dioxide scaffolds for the treatment of bone tissue defects.

PubMed

Rumian, Łucja; Reczyńska, Katarzyna; Wrona, Małgorzata; Tiainen, Hanna; Haugen, Håvard J; Pamuła, Elżbieta

2015-01-01

In this study the attempts to improve mechanical properties of highly-porous titanium dioxide scaffolds produced by polymer sponge replication method were investigated. Particularly the effect of two-step sintering at different temperatures on microstructure and mechanical properties (compression test) of the scaffolds were analysed. To this end microcomputed tomography and scanning electron microscopy were used as analytical methods. Our experiments showed that the most appropriate conditions of manufacturing were when the scaffolds were heat-treated at 1500 °C for 1 h followed by sintering at 1200 °C for 20 h. Such scaffolds exhibited the highest compressive strength which was correlated with the highest linear density and the lowest size of grains. Moreover, grain size distribution was narrower with predominating fraction of fine grains 10-20 μm in size. Smaller grains and higher linear density sug- gested that in this case densification process prevailed over undesirable process of grain coarsening, which finally resulted in im- proved mechanical properties of the scaffolds.

Investigation on the Size Effect in Large-Scale Beta-Processed Ti-17 Disks Based on Quantitative Metallography

NASA Astrophysics Data System (ADS)

Zhang, Saifei; Zeng, Weidong; Gao, Xiongxiong; Zhao, Xingdong; Li, Siqing

2017-10-01

The present study investigates the mechanical properties of large-scale beta-processed Ti-17 forgings because of the increasing interest in beta thermal-mechanical processing method for fabricating compressor disks or blisks in aero-engines due to its advantage in damage tolerance performance. Three Ti-17 disks with different weights of 57, 250 and 400 kg were prepared by beta processing techniques firstly for comparative study. The results reveal a significant `size effect' in beta-processed Ti-17 disks, i.e., dependences of high cycle fatigue, tensile properties and fracture toughness of beta-processed Ti-17 disks on disk size (or weight). With increasing disk weight from 57 to 400 kg, the fatigue limit (fatigue strength at 107 cycles, R = -1) was reduced from 583 to 495 MPa, tensile yield strength dropped from 1073 to 1030 MPa, while fracture toughness ( K IC) rose from 70.9 to 95.5 MPaṡm1/2. Quantitative metallography analysis shows that the `size effect' of mechanical properties can be attributed to evident differences between microstructures of the three disk forgings. With increasing disk size, nearly all microstructural components in the basket-weave microstructure, including prior β grain, α layers at β grain boundaries (GB- α) and α lamellas at the interior of the grains, get coarsened to different degrees. Further, the microstructural difference between the beta-processed disks is proved to be the consequence of longer pre-forging soaking time and lower post-forging cooling rate for large disks than small ones. Finally, suggestions are made from the perspective of microstructural control on how to improve mechanical properties of large-scale beta-processed Ti-17 forgings.

Influence of Grain Size on Mechanical Responses in Beta Ti-12Mo Alloy Demonstrating Concurrent Twinning-Induced Plasticity/Transformation-induced Plasticity Effects

NASA Astrophysics Data System (ADS)

Zhang, D. C.; Xue, Q.; Lei, J. F.; Ma, Y. J.; Yang, R.; Wang, C.

2018-06-01

Metastable β Ti-12Mo wt pct alloys with controllable grain sizes are successfully produced, and the effect of grain size on mechanical responses has been thoroughly investigated. It is found that target alloys possess concurrent twinning-induced plasticity (TWIP) and transformation-induced plasticity (TRIP) features. Mechanisms governing mechanical properties through well-manipulated tensile experiments, detailed microstructure analysis, as well as strong correlations between triggering stress and twinning/phase transformation are offered.

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.

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.

Correlating the internal length in strain gradient plasticity theory with the microstructure of material

NASA Astrophysics Data System (ADS)

Zhao, Jianfeng; Zhang, Xu; Konstantinidis, Avraam A.; Kang, Guozheng

2015-06-01

The internal length is the governing parameter in strain gradient theories which among other things have been used successfully to interpret size effects at the microscale. Physically, the internal length is supposed to be related with the microstructure of the material and evolves during the deformation. Based on Taylor hardening law, we propose a power-law relationship to describe the evolution of the variable internal length with strain. Then, the classical Fleck-Hutchinson strain gradient theory is extended with a strain-dependent internal length, and the generalized Fleck-Hutchinson theory is confirmed here, by comparing our model predictions to recent experimental data on tension and torsion of thin wires with varying diameter and grain size. Our work suggests that the internal length is a configuration-dependent parameter, closely related to dislocation characteristics and grain size, as well as sample geometry when this affects either the underlying microstructure or the ductility of the material.

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.

Fabrication of fine-grain tantalum diffusion barrier tube for Nb3Sn conductors

NASA Astrophysics Data System (ADS)

Hartwig, K. T.; Balachandran, S.; Mezyenski, R.; Seymour, N.; Robinson, J.; Barber, R. E.

2014-01-01

Diffusion barriers used in Nb3Sn wire are often fabricated by wrapping Ta sheet into a tube with an overlap seam. A common result of such practice is non-uniform deformation in the Ta sheet as it thins by wire drawing because of non-uniform grain size and texture in the original Ta sheet. Seamless Ta tube with a fine-grain and uniform microstructure would be much better for the diffusion barrier application, but such material is expensive and difficult to manufacture. This report presents results on a new fabrication strategy for Ta tube that shows promise for manufacture of less costly tube with an improved microstructure. The fabrication method begins with seam-welded tube but gives a fine-grain uniform microstructure with little difference between the longitudinal seam weld region and the parent metal after post-weld processing. Severe plastic deformation processing (SPD) applied by area reduction extrusion and tube equal channel angular extrusion (tECAE) are used to refine and homogenize the microstructure. Microstructure and mechanical property results are presented for Ta tubes fabricated by this new processing strategy.

Effect of crystallographic orientations of grains on the global mechanical properties of steel sheets by depth sensing indentation

NASA Astrophysics Data System (ADS)

Burik, P.; Pesek, L.; Kejzlar, P.; Andrsova, Z.; Zubko, P.

2017-01-01

The main idea of this work is using a physical model to prepare a virtual material with required properties. The model is based on the relationship between the microstructure and mechanical properties. The macroscopic (global) mechanical properties of steel are highly dependent upon microstructure, crystallographic orientation of grains, distribution of each phase present, etc... We need to know the local mechanical properties of each phase separately in multiphase materials. The grain size is a scale, where local mechanical properties are responsible for the behavior. Nanomechanical testing using depth sensing indentation (DSI) provides a straightforward solution for quantitatively characterizing each of phases in microstructure because it is very powerful technique for characterization of materials in small volumes. The aim of this experimental investigation is: (i) to prove how the mixing rule works for local mechanical properties (indentation hardness HIT) in microstructure scale using the DSI technique on steel sheets with different microstructure; (ii) to compare measured global properties with properties achieved by mixing rule; (iii) to analyze the effect of crystallographic orientations of grains on the mixing rule.

Predicting mesoscale microstructural evolution in electron beam welding

DOE PAGES

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

2016-03-16

Using the kinetic Monte Carlo simulator, Stochastic Parallel PARticle Kinetic Simulator, from Sandia National Laboratories, a user routine has been developed to simulate mesoscale predictions of a grain structure near a moving heat source. Here, we demonstrate the use of this user routine to produce voxelized, synthetic, three-dimensional microstructures for electron-beam welding by comparing them with experimentally produced microstructures. When simulation input parameters are matched to experimental process parameters, qualitative and quantitative agreement for both grain size and grain morphology are achieved. The method is capable of simulating both single- and multipass welds. As a result, the simulations provide anmore » opportunity for not only accelerated design but also the integration of simulation and experiments in design such that simulations can receive parameter bounds from experiments and, in turn, provide predictions of a resultant microstructure.« less

Elaboration of austenitic stainless steel samples with bimodal grain size distributions and investigation of their mechanical behavior

NASA Astrophysics Data System (ADS)

Flipon, B.; de la Cruz, L. Garcia; Hug, E.; Keller, C.; Barbe, F.

2017-10-01

Samples of 316L austenitic stainless steel with bimodal grain size distributions are elaborated using two distinct routes. The first one is based on powder metallurgy using spark plasma sintering of two powders with different particle sizes. The second route applies the reverse-annealing method: it consists in inducing martensitic phase transformation by plastic strain and further annealing in order to obtain two austenitic grain populations with different sizes. Microstructural analy ses reveal that both methods are suitable to generate significative grain size contrast and to control this contrast according to the elaboration conditions. Mechanical properties under tension are then characterized for different grain size distributions. Crystal plasticity finite element modelling is further applied in a configuration of bimodal distribution to analyse the role played by coarse grains within a matrix of fine grains, considering not only their volume fraction but also their spatial arrangement.

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.

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

BHQ revisited (1) - Looking at grain size

NASA Astrophysics Data System (ADS)

Heilbronner, Renée; Kilian, Rüdiger; Tullis, Jan

2016-04-01

Black Hills Quartzite (BHQ) has been used extensively in experimental rock deformation for numerous studies. Coaxial and general shear experiments have been carried out, for example, to define the dislocation creep regimes of quartz (Hirth & Tullis, 1992), to determine the effect of annealing (Heilbronner & Tullis, 2002) or to study the development of texture and microstructure with strain (Heilbronner & Tullis, 2006). BHQ was also used to determine the widely used quartz piezometer by Stipp & Tullis (2003). Among the microstructure analyses that were performed in those original papers, grain size was usually determined using CIP misorientation images. However, the CIP method (= computer-integrated polarization microscopy, details in Heilbronner and Barrett, 2014) is only capable of detecting the c-axis orientation of optically uniaxial materials and hence is only capable of detecting grain boundaries between grains that differ in c-axis orientation. One of the puzzling results we found (Heilbronner & Tullis, 2006) was that the recrystallized grain size seemed to depend on the crystallographic preferred orientation of the domain. In other words the grain size did not only depend on the flow stress but also on the orientation of the c-axis w/r to the shear direction. At the time, no EBSD analysis (electron back scatter diffraction) was carried out and hence the full crystallographic orientation was not known. In principle it is therefore possible that we missed some grain boundaries (between grains with parallel c-axes) and miscalculated our grain sizes. In the context of recent shear experiments on quartz gouge at the brittle-viscous transition (see Richter et al., this conference), where EBSD is used to measure the recrystallized grain size, we wanted to re-measure the CIP grain sizes of our 2006 samples (deformed in regime 1, 2 and 3 of dislocation) in exactly the same way. In two companion posters we use EBSD orientation imaging to repeat, refine and expand the microstructure and texture analysis of Heilbronner & Tullis (2006). Here, in poster (1), we focus on the recrystallized grain size with the aim of (a) comparing CIP- and EBSD derived grain size measurements, (b) of comparing the recrystallized grain size of coaxially deformed and sheared BHQ and (c) in order to confirm that the quartz piezometer indeed depends on texture, and (d) to test if it also depends on the type of deformation (irrotational versus rotational deformation). References cited: Heilbronner, R., and S.D. Barrett (2014) Image Analysis in Earth Sciences, Springer. Heilbronner, R., and J. Tullis (2002), The effect of static annealing on micro- structure and crystallographic preferred orientations of quartzites experimentally deformed in axial compression and shear, Geol. Soc. Spec. Publ., 200, 191 - 218. Heilbronner, R., and J. Tullis (2006), Evolution of c axis pole figures and grain size during dynamic recrystallization: Results from experimentally sheared quartzite. JGR, 111, B10202, doi:10.1029/2005JB004194, 2006 Hirth, G., and J. Tullis (1992), Dislocation creep regimes in quartz aggregates, JSG, 14, 145-159. Stipp, M., and J. Tullis (2003), The recrystallized grain size piezometer for quartz, Geophys. Res. Lett., 30(21), 2088, doi:10.1029/2003GL018444.

The Effect of Ultrafine-Grained Microstructure on Creep Behaviour of 9% Cr Steel

PubMed Central

Kral, Petr; Dvorak, Jiri; Sklenicka, Vaclav; Masuda, Takahiro; Horita, Zenji; Kucharova, Kveta; Kvapilova, Marie; Svobodova, Marie

2018-01-01

The effect of ultrafine-grained size on creep behaviour was investigated in P92 steel. Ultrafine-grained steel was prepared by one revolution of high-pressure torsion at room temperature. Creep tensile tests were performed at 873 K under the initially-applied stress range between 50 and 160 MPa. The microstructure was investigated using transmission electron microscopy and scanning electron microscopy equipped with an electron-back scatter detector. It was found that ultrafine-grained steel exhibits significantly faster minimum creep rates, and there was a decrease in the value of the stress exponent in comparison with coarse-grained P92 steel. Creep results also showed an abrupt decrease in the creep rate over time during the primary stage. The abrupt deceleration of the creep rate during the primary stage was shifted, with decreasing applied stress with longer creep times. The change in the decline of the creep rate during the primary stage was probably related to the enhanced precipitation of the Laves phase in the ultrafine-grained microstructure. PMID:29757206

The role of grain size and shape in strengthening of dispersion hardened nickel alloys.

NASA Technical Reports Server (NTRS)

Wilcox, B. A.; Clauer, A. H.

1972-01-01

Thermomechanical processing was used to develop various microstructures in Ni, Ni-2ThO2, Ni-20Cr, Ni-20Cr-2ThO2, Ni-20Cr-10W and Ni-20Cr-10W-2ThO2, and the influence of microstructure on room temperature and elevated temperature strength was investigated. The yield strength at 25 C increased with substructure refinement according to the Hall-Petch relation. It was found that substructure refinement was a much more potent means of strengthening at room temperature than was dispersion hardening. At elevated temperature (1093 C), the most important microstructural feature affecting strength of dispersion hardened nickel alloys was the grain aspect ratio, i.e. grain length, L, divided by grain width,l. The yield strength and creep strength increased linearly with increasing L/l.

Investigation of the Microstructure of Laser-Arc Hybrid Welded Boron Steel

NASA Astrophysics Data System (ADS)

Son, Seungwoo; Lee, Young Ho; Choi, Dong-Won; Cho, Kuk-Rae; Shin, Seung Man; Lee, Youngseog; Kang, Seong-Hoon; Lee, Zonghoon

2018-05-01

The microstructure of boron steel for automotive driving shaft manufacturing after laser-arc hybrid welding was investigated. Laser-arc hybrid welding technology was applied to 3-mm-thick plates of boron steel, ST35MnB. The temperature distribution of the welding pool was analyzed using the finite element method, and the microstructure of the welded boron steel was characterized using optical microscopy and scanning and transmission electron microscopies. The microstructure of the weld joint was classified into the fusion zone, the heat-affected zone (HAZ), and the base material. At the fusion zone, the bainite grains exist in the martensite matrix and show directionality because of heat input from the welding. The HAZ is composed of smaller grains, and the hardness of the HAZ is greater than that of the fusion zone. We discuss that the measured grain size and the hardness of the HAZ originate from undissolved precipitates that retard the grain growth of austenite.

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

The microstructural evolution, crystallography, and thermal processing of ultrahigh carbon Fe-1.85 pct C melt-spun ribbon

NASA Technical Reports Server (NTRS)

Spanos, G.; Ayers, J. D.; Vold, C. L.; Locci, I. E.

1993-01-01

A study is presented to determine if fine microstructures could be achieved using rapid solidification to produce a fine-grained fully austenitic starting structure and then using thermal processing cycles to produce an even finer ferrite-cementite structure. The evolution, mechanisms of grain refinement, and crystallography of the resultant microstructures were examined by TEM. A thermal processing cycle consisted of quenching the ribbon in liquid nitrogen, tempering at 600 C for 10 sec, 'upquenching' to 750 C for 10 sec, and subsequently quenching again in liquid nitrogen. The heat-treatment resulted in martensite grains with sizes of about 1 micron or less in both length and thickness and cementite particles of 0.4 micron or less. It is concluded that these microstructures could be used for producing fine-grained ultrahigh carbon steels of very high strength without the brittleness associated with the formation of coarse carbide particles of the loss of strength due to graphite formation.

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

Corrosion Behavior of Pure Copper Surrounded by Hank's Physiological Electrolyte at 310 K (37 °C) as a Potential Biomaterial for Contraception: An Analogy Drawn Between Micro- and Nano-grained Copper

NASA Astrophysics Data System (ADS)

Fattah-alhosseini, Arash; Imantalab, Omid; Vafaeian, Saeed; Ansari, Ghazaleh

2017-08-01

This work aims to evaluate the corrosion behavior of pure copper from the microstructural viewpoint for a biomedical application, namely intrauterine devices. For this purpose, Tafel polarization and electrochemical impedance spectroscopy (EIS) techniques were used to evaluate the corrosion behavior of annealed pure copper (with the average grain size of 45 ± 1 µm) and nano-grained microstructure in physiological electrolyte of Hank at 310 K (37 °C). Pure copper in nanoscale grain size, typically an average of 90 ± 5 nm, was successfully made by eight-cycle accumulative roll bonding process at room temperature. On the basis of Tafel polarization results, it was revealed that nano-grained sample had lower corrosion current density and more noble corrosion potential for prolonged exposure in Hank's physiological solution at 310 K (37 °C). In addition, the EIS results showed that the nano-grained sample had more corrosion resistance compared to the coarse-grained one for long-time immersion.

The Effect of Friction Stir Processing on Microstructure and Tensile Behavior of Thixomolded AZ91 Magnesium Alloy

NASA Astrophysics Data System (ADS)

Mansoor, B.; Decker, R. F.; Kulkarni, S.; LeBeau, S. E.; Khraisheh, M. K.

Friction Stir Processing (FSP) to partial sheet thickness can be utilized to engineer unique microstructures in metallic alloys. These composite microstructures consist of three distinct layers associated with stirred, transition and core micro structural regions. The stirred region is of particular interest where severe plastic deformation imparted by the rotating and translating FSP tool under frictional heat leads to grain refinement down to 1 urn grain size. In this work, partial depth penetration into thixomolded AZ91 Mg plate from the top and bottom surfaces by friction stir processing is explored. Furthermore, low temperature aging treatments are applied to the processed material. The present results with AZ91 Mg show that FSP processed material exhibits higher strength (> 300 MPa), and improvement in ductility (> 7 % tensile elongation). It is found that in addition to Hall-Petch strengthening produced by 1 um grain size in the stirred region, the enhanced strength levels and ductility are strongly influenced by dispersoids of the intermetallic precipitates found in this alloy.

Ultrasonic Phased Array Sound Field Mapping Through Large-Bore Coarse Grained Cast Austenitic Stainless Steel (CASS) Piping Materials

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

Cinson, Anthony D.; Crawford, Susan L.; Prowant, Matthew S.

2012-04-16

A sound field beam mapping exercise was conducted to further understand the effects of coarse grained microstructures found in CASS materials on phased array ultrasonic wave propagation. Laboratory measurements were made on three CASS specimens with different microstructures; the specimens were polished and etched to reveal measurable grain sizes, shapes and orientations. Three longitudinal, phased array probes were fixed on a specimen's outside diameter with the sound field directed toward one end (face) of the pipe segment over a fixed range of angles. A point receiver was raster scanned over the surface of the specimen face generating a sound fieldmore » image. A slice of CASS material was then removed from the specimen end and the beam mapping exercise repeated. The sound fields acquired were analyzed for spot size, coherency, and beam redirection. Analyses were conducted between the resulting sound fields and the microstructural characteristics of each specimen.« less

Ultrafine-grained commercially pure titanium and microstructure response to hydroxyapatite coating methods

NASA Astrophysics Data System (ADS)

Calvert, Kayla L.

Commercially pure titanium (cp-Ti) is an ideal biomaterial as it does not evoke an inflammatory foreign body response in the body. However, the low strength of cp-Ti prevents the use in most orthopaedic load bearing applications. Therefore, many metal orthopaedic implants are commonly made of higher strength metal alloys that are less biocompatible. Nanostructured materials exhibit superior mechanical properties compared to their conventional grain sized counterparts. Severe plastic deformation (SPD) of metals has been shown to produce nanostructured materials. SPD by machining is a single-step deformation route that refines the grain microstructure, to develop an ultrafine grained (UFG) microstructure. UFG cp-Ti strips were developed with induced shear strains of up to 4.0 using a machining-based process. Both Vickers microhardness evaluation and microstructural analysis were used to characterize the as-received (annealed) and machined states. For induced shear strains between 1.9 and 4.0 in grade 2 cp-Ti the hardness was increased from 188 +/- 7 kg/mm2 in the as-received state to between 244 +/- 6 and 264 +/- 12 kg/mm 2 in the as-machined state, corresponding to an increase in hardness between 31 and 41%. The microstructural analysis revealed a grain size reduction from 34 +/- 11 mum in the as-received state to ˜ 100 nm for machined grade 2-Ti. A complete annealing study suggested that recovery/recrystallization occurs between 300 and 400°C, with a significant hardness drop between 400 and 600°C, while grain growth is continuous, starting at the lowest annealing temperature of 300°C. Hydroxyapatite (HA) is commonly applied to orthopaedic devices to promote bone growth. Machined Ti strips were coated with HA using conventional plasma spray as well as two alternative low-temperature application routes (sol-gel with calcination and anodization with hydrothermal treatment) to evaluate the thermal influence on the UFG-Ti substrate. Plasma spray produced a thick (20 to 70 mum) HA crystalline coating, sol-gel followed by calcination did not produce crystalline HA, while anodization with the proper hydrothermal treatment yielded a homogenous crystalline HA coating 5 to 15 mum thick based on the anodization condition. Mechanical and microstructural evaluation of the UFG-Ti substrates revealed that both the plasma spray and anodization followed by hydrothermal treatment (220 -- 225°C) did not affect the substrate grain size or hardness, while the thermal processing and calcination treatment at 313 -- 446°C for the sol-gel method caused recovery and grain growth, as well as a significant decrease in the hardness of the Ti-substrates.

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

Additive Manufacturing of Metastable Beta Titanium Alloys

NASA Astrophysics Data System (ADS)

Yannetta, Christopher J.

Additive manufacturing processes of many alloys are known to develop texture during the deposition process due to the rapid reheating and the directionality of the dissipation of heat. Titanium alloys and with respect to this study beta titanium alloys are especially susceptible to these effects. This work examines Ti-20wt%V and Ti-12wt%Mo deposited under normal additive manufacturing process parameters to examine the texture of these beta-stabilized alloys. Both microstructures contained columnar prior beta grains 1-2 mm in length beginning at the substrate with no visible equiaxed grains. This microstructure remained constant in the vanadium system throughout the build. The microstructure of the alloy containing molybdenum changed from a columnar to an equiaxed structure as the build height increased. Eighteen additional samples of the Ti-Mo system were created under different processing parameters to identify what role laser power and travel speed have on the microstructure. There appears to be a correlation in alpha lath size and power density. The two binary alloys were again deposited under the same conditions with the addition of 0.5wt% boron to investigate the effects an insoluble interstitial alloying element would have on the microstructure. The size of the prior beta grains in these two alloys were reduced with the addition of boron by approximately 50 (V) and 100 (Mo) times.

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...

Effect of phase transformations on microstructures in deep mantle materials

NASA Astrophysics Data System (ADS)

Merkel, Sébastien; Langrand, Christopher; Rosa, Angelika; Hilairet, Nadège

2017-04-01

Phase transformations induce microstructural changes in deep Earth materials, including changes in grain size and orientation distribution. The effect of phase transformations on mineral microstructures is usually studied using electron microscopy on quench products from high P/T experiments. The method allows for a precise evaluation of the microscopic mechanisms involved. It is limited, however, to samples that can be quenched to ambient conditions and allows for investigations at a single P/T point for each experiment. In recent years, we extended the use of multigrain crystallography to samples inside diamond anvil cells under mantle P/T conditions. The method allows for monitoring the orientations of hundreds of grains and grain size variations during various physical processes, such as plastic deformation and successions of phase transformations (Rosa et al 2015, Langrand et al 2017). Here, we will show results concerning hydrous Mg2SiO4 during the series of α-β-γ phase transformations up to 40 GPa and 850 °C. Such results are important to understand the descending behaviour of subducted slabs, observations of seismic anisotropy, and polarity changes for seismic waves reflected of deep Earth interfaces. The data is used to asses the effect of the transformation on grain orientation and grain sizes. In particular, we do not observe orientation relationships between the parent α-phase and the daughter β-phase phase, suggesting an incoherent growth. We also observe significant grain size reductions and only little grain growth within the newly formed phases (Rosa et al 2016). These new results are important for understanding the mechanical behavior of subducting slabs, seismic anisotropy in the Earth's mantle, and phase transformation mechanisms in olivine. Now that it is validated, the method can also be applied to other phases that can not be studied using electron microscopy, such as perovskite and post-perovskite. Langrand, Hilairet, Nisr, Roskosz, Ribárik, Vaughan, Merkel, Reliability of Multigrain Indexing for Orthorhombic Polycrystals above 1 Mbar: Application to MgSiO3-Post-Perovskite, J Appl Cryst 50, in press (2017) Rosa, Hilairet, Ghosh, Garbarino, Jacobs, Perrillat, Vaughan, Merkel, In situ monitoring of phase transformation microstructures at Earth's mantle pressure and temperature using multi-grain XRD, J Appl Cryst 48, 1346-1354 (2015) Rosa, Hilairet, Ghosh, Perrillat, Garbarino, Merkel, Evolution of grain sizes and orientations during phase transitions in hydrous Mg2SiO4, J Geophys Res 121, 7161-7176 (2016)

Microstructural Evolution of Al2O3-ZrO2 (Y2O3) Composites and its Correlation with Toughness

NASA Astrophysics Data System (ADS)

Kim, Hee Seung; Seo, Mi Young; Kim, Ik Jin

2008-02-01

The microstructure of zirconia (ZrO2) toughened alumina (Al2O3) ceramics was carefully controlled so as to obtain dense and fine-grained ceramics, thereby improving the properties and reliability of the ceramics for capillary applications in semiconductor bonding technology. Al2O3-ZrO2(Y2O3) composite was produced via Ceramic Injection Molding (CIM) technology, followed by Sinter-HIP process. Room temperature strength, hardness, Young's modulus, thermal expansion coefficient and toughness were determined, as well as surface strengthening induced by the fine grained homogenous microstructure and the thermal treatment. The changes in alumina/zirconia grain size, sintering condition and HIP treatment were found to be correlated.

Influence of grain size and texture prior to warm rolling on microstructure, texture and magnetic properties of Fe-6.5 wt% Si steel

NASA Astrophysics Data System (ADS)

Xu, H. J.; Xu, Y. B.; Jiao, H. T.; Cheng, S. F.; Misra, R. D. K.; Li, J. P.

2018-05-01

Fe-6.5 wt% Si steel hot bands with different initial grain size and texture were obtained through different annealing treatment. These bands were then warm rolled and annealed. An analysis on the evolution of microstructure and texture, particularly the formation of recrystallization texture was studied. The results indicated that initial grain size and texture had a significant effect on texture evolution and magnetic properties. Large initial grains led to coarse deformed grains with dense and long shear bands after warm rolling. Such long shear bands resulted in growth advantage for {1 1 3} 〈3 6 1〉 oriented grains during recrystallization. On the other hand, sharp {11 h} 〈1, 2, 1/h〉 (α∗-fiber) texture in the coarse-grained sample led to dominant {1 1 2} 〈1 1 0〉 texture after warm rolling. Such {1 1 2} 〈1 1 0〉 deformed grains provided massive nucleation sites for {1 1 3} 〈3 6 1〉 oriented grains during subsequent recrystallization. These {1 1 3} 〈3 6 1〉 grains were confirmed to exhibit an advantage on grain growth compared to γ-fiber grains. As a result, significant {1 1 3} 〈3 6 1〉 texture was developed and unfavorable γ-fiber texture was inhibited in the final annealed sheet. Both these aspects led to superior magnetic properties in the sample with largest initial grain size. The magnetic induction B8 was 1.36 T and the high frequency core loss P10/400 was 17.07 W/kg.

Scale effects in crystal plasticity

NASA Astrophysics Data System (ADS)

Padubidri Janardhanachar, Guruprasad

The goal of this research work is to further the understanding of crystal plasticity, particularly at reduced structural and material length scales. Fundamental understanding of plasticity is central to various challenges facing design and manufacturing of materials for structural and electronic device applications. The development of microstructurally tailored advanced metallic materials with enhanced mechanical properties that can withstand extremes in stress, strain, and temperature, will aid in increasing the efficiency of power generating systems by allowing them to work at higher temperatures and pressures. High specific strength materials can lead to low fuel consumption in transport vehicles. Experiments have shown that enhanced mechanical properties can be obtained in materials by constraining their size, microstructure (e.g. grain size), or both for various applications. For the successful design of these materials, it is necessary to have a thorough understanding of the influence of different length scales and evolving microstructure on the overall behavior. In this study, distinction is made between the effect of structural and material length scale on the mechanical behavior of materials. A length scale associated with an underlying physical mechanism influencing the mechanical behavior can overlap with either structural length scales or material length scales. If it overlaps with structural length scales, then the material is said to be dimensionally constrained. On the other hand, if it overlaps with material length scales, for example grain size, then the material is said to be microstructurally constrained. The objectives of this research work are: (1) to investigate scale and size effects due to dimensional constraints; (2) to investigate size effects due to microstructural constraints; and (3) to develop a size dependent hardening model through coarse graining of dislocation dynamics. A discrete dislocation dynamics (DDD) framework where the scale of analysis is intermediate between a fully discretized (e.g. atomistic) and fully continuum is used for this study. This mesoscale tool allows to address all the stated objectives of this study within a single framework. Within this framework, the effect of structural and the material length scales are naturally accounted for in the simulations and need not be specified in an ad hoc manner, as in some continuum models. It holds the promise of connecting the evolution of the defect microstructure to the effective response of the crystal. Further, it provides useful information to develop physically motivated continuum models to model size effects in materials. The contributions of this study are: (a) provides a new interpretation of mechanical size effect due to only dimensional constraint using DDD; (b) a development of an experimentally validated DDD simulation methodology to model Cu micropillars; (c) a coarse graining technique using DDD to develop a phenomenological model to capture size effect on strain hardening; and (d) a development of a DDD framework for polycrystals to investigate grain size effect on yield strength and strain hardening.

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).

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.

Comparative study of eddy current and Barkhausen noise nondestructive testing methods in microstructural examination of ferrite-martensite dual-phase steel

NASA Astrophysics Data System (ADS)

Ghanei, S.; Kashefi, M.; Mazinani, M.

2014-04-01

The magnetic properties of ferrite-martensite dual-phase steels were evaluated using eddy current and Barkhausen noise nondestructive testing methods and correlated with their microstructural changes. Several routes were used to produce different microstructures of dual-phase steels. The first route was different heat treatments in γ region to vary the ferrite grain size (from 9.47 to 11.12 in ASTM number), and the second one was variation in intercritical annealing temperatures (from 750 to 890 °C) in order to produce different percentages of martensite in dual-phase microstructure. The results concerning magnetic Barkhausen noise are discussed in terms of height, position and shape of Barkhausen noise profiles, taking into account two main aspects: ferrite grain size, and different percentages of martensite. Then, eddy current testing was used to study the mentioned microstructural changes by detection of impedance variations. The obtained results show that microstructural changes have a noticeable effect on the magnetic properties of dual-phase steels. The results reveal that both magnetic methods have a high potential to be used as a reliable nondestructive tool to detect and monitor microstructural changes occurring during manufacturing of dual-phase steels.

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.

The Microstructural Evolution of Quartzite During Gradually Increasing Stress.

NASA Astrophysics Data System (ADS)

Soleymani, Hamid; Kidder, Steven B.; Hirth, Greg

2016-12-01

In settings where rocks are exhumed along shear zones, mylonites are thought to experience a gradual increase in stress and localization as they approach the brittle-ductile transition (Figure 1. left panel). Our aim is to investigate the microstructural characteristics of experimental samples that have experienced such a stress path and make comparisons to natural samples. A common characteristic of recrystallized grains in shear zones is what appears, at least qualitatively, to be a bimodal distribution of grain size (Figure 1. right panel). We hypothesize that such distributions might form as a natural consequence of a gradual stress increase in rocks approaching the brittle-ductile transition. We carried out several general-shear, Griggs rig experiments on Arkansas novaculite ( 10 micron grain size) and Black Hills quartzite synthesized powder (10-20 micron) annealed at 915°C and confining pressure of 1.5 GPa. To simulate exhumation, stress was increased by gradually decreasing the temperature at various constant rates. Experimental design and mechanical data are presented along with a discussion on grain growth and evolution. Initial results show that the technique is able to successfully simulate the exhumation stre­­­­ss path. The experiments also show that novaculite is roughly twice as strong (at similar water concentrations) as Black Hills quartzite powder ( 10-20 microns). We anticipate that detailed, quantitative study of the microstructure and grain statistics of experiments of this type can lead to improved interpretation of the microstructural development of natural samples.

Grain-size-induced weakening of H2O ices I and II and associated anisotropic recrystallization

USGS Publications Warehouse

Stern, L.A.; Durham, W.B.; Kirby, S.H.

1997-01-01

Grain-size-dependent flow mechanisms tend to be favored over dislocation creep at low differential stresses and can potentially influence the rheology of low-stress, low-strain rate environments such as those of planetary interiors. We experimentally investigated the effect of reduced grain size on the solid-state flow of water ice I, a principal component of the asthenospheres of many icy moons of the outer solar system, using techniques new to studies of this deformation regime. We fabricated fully dense ice samples of approximate grain size 2 ?? 1 ??m by transforming "standard" ice I samples of 250 ?? 50 ??m grain size to the higher-pressure phase ice II, deforming them in the ice II field, and then rapidly releasing the pressure deep into the ice I stability field. At T ??? 200 K, slow growth and rapid nucleation of ice I combine to produce a fine grain size. Constant-strain rate deformation tests conducted on these samples show that deformation rates are less stress sensitive than for standard ice and that the fine-grained material is markedly weaker than standard ice, particularly during the transient approach to steady state deformation. Scanning electron microscope examination of the deformed fine-grained ice samples revealed an unusual microstructure dominated by platelike grains that grew normal to the compression direction, with c axes preferentially oriented parallel to compression. In samples tested at T ??? 220 K the elongation of the grains is so pronounced that the samples appear finely banded, with aspect ratios of grains approaching 50:1. The anisotropic growth of these crystallographically oriented neoblasts likely contributes to progressive work hardening observed during the transient stage of deformation. We have also documented remarkably similar microstructural development and weak mechanical behavior in fine-grained ice samples partially transformed and deformed in the ice II field.

In-situ High Temperature Phase Transformations in Ceramics

DTIC Science & Technology

2009-07-28

microscopy - SEM and transmission electron microscopy - TEM), have identified important microstructural considerations, such as the critical ...particularly with judicial design of the critical particle size and microstructure.12, 47, 48 Likewise, preliminary work indicates the possibility of high...toughening of fiber reinforced, fibrous monolithic or laminated ceramic matrix composites.49, 50 enstatite was above a 7 μm critical grain size

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

Effect of Post-Weld Heat Treatment on Microstructure and Mechanical Properties of X52 Linepipe HFIW Joints

NASA Astrophysics Data System (ADS)

Kavousi Sisi, A.; Mirsalehi, S. E.

2015-04-01

In the present paper, influences of normalization heat treatment on microstructural and mechanical properties of high-frequency induction welded (HFIW) joints of X52 steel have been investigated. HFIW joints were post-weld heat treated at different times and temperatures. The microstructure and mechanical properties of the heat treated joints were then comprehensively investigated. Based on the results, a proper normalization of the primary fine grain steel caused the grain size to increase; but because of converting brittle microstructure into ductile microstructure, it caused the toughness to increase also. In addition, the ductility of the joints was enhanced. Nevertheless, tensile strength, yield strength, and hardness were reduced. The results showed that 950 °C was the optimum normalization temperature from the standpoint of fracture toughness for the X52 steel joints. At 1050 °C, the carbides and/or nitrides in the steel dissolved, and excessive grain growth occurred. Hence, the maximum allowable temperature for normalization was found to be 1000 °C.

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

Computational study of dislocation based mechanisms in FCC materials

NASA Astrophysics Data System (ADS)

Yellakara, Ranga Nikhil

Understanding the relationships between microstructures and properties of materials is a key to developing new materials with more suitable qualities or employing the appropriate materials in special uses. In the present world of material research, the main focus is on microstructural control to cost-effectively enhance properties and meet performance specifications. This present work is directed towards improving the fundamental understanding of the microscale deformation mechanisms and mechanical behavior of metallic alloys, particularly focusing on face centered cubic (FCC) structured metals through a unique computational methodology called three-dimensional dislocation dynamics (3D-DD). In these simulations, the equations of motion for dislocations are mathematically solved to determine the evolution and interaction of dislocations. Microstructure details and stress-strain curves are a direct observation in the simulation and can be used to validate experimental results. The effect of initial dislocation microstructure on the yield strength has been studied. It has been shown that dislocation density based crystal plasticity formulations only work when dislocation densities/numbers are sufficiently large so that a statistically accurate description of the microstructure can be obtainable. The evolution of the flow stress for grain sizes ranging from 0.5 to 10 mum under uniaxial tension was simulated using an improvised model by integrating dislocation pile-up mechanism at grain boundaries has been performed. This study showed that for a same initial dislocation density, the Hall--Petch relationship holds well at small grain sizes (0.5--2 mum), beyond which the yield strength remains constant as the grain size increases. Various dislocation-particle interaction mechanisms have been introduced and investigations were made on their effect on the uniaxial tensile properties. These studies suggested that increase in particle volume fraction and decrease in particle size has contributed to the strength of these alloys. This work has been successful of capturing complex dislocation mechanisms that involves interactions with particles during the deformation of particle hardened FCC alloys. Finally, the DD model has been extended into studying the cyclic behavior of FCC metallic alloys. This study showed that the strength as well as the cyclic hardening increases due to grain refinement and increase in particle volume fraction. It also showed that the cyclic deformation of ultra-fine grained (UFG) material have undergone cyclic softening at all plastic strain amplitudes. The results provided very useful quantitative information for developing future fatigue models.

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.

Microstructure, Mechanical, and Fatigue Strength of Ti-54M Processed by Rotary Swaging

NASA Astrophysics Data System (ADS)

Al-Khazraji, Hasan; El-Danaf, Ehab; Wollmann, Manfred; Wagner, Lothar

2015-05-01

TIMETAL 54M is a newly developed (α + β) titanium alloy with nominal composition Ti-5Al-4V-0.6Mo-0.4Fe. The alloy can provide a cost benefit over Ti-6Al-4V due to improved machinability and formability. In the present work, evolution of mechanical properties in terms of tensile and hardness values is investigated as a function of deformation degrees imposed via rotary swaging (RS). Microstructure, mechanical properties, and fatigue performance of Ti-54M are investigated after severe plastic deformation by RS conducted at 850 °C and after being subjected to two different post-swaging annealing conditions. Optical microscopy and scanning electron microscopy using electron back scatter diffraction were utilized to document the evolution of the microstructure. Tensile tests were conducted to characterize mechanical properties. RS, to a true strain of 3.0, is found to lead to a marked ultrafine-grained structure of about 1 μm grain size with low content of high angle grain boundaries (HAGBs). Post-swaging heat treatment at 800 °C followed by air cooling did not change the grain size but exhibited high content of HAGBs. Post-swaging heat treatment at 940 °C followed by furnace cooling resulted in a grain size of about 5 μm and enhanced work-hardening capability and ductility, which resulted in less fatigue notch sensitivity, but at the same time lower fatigue strength at 107 cycles.

Gas tungsten arc welding and friction stir welding of ultrafine grained AISI 304L stainless steel: Microstructural and mechanical behavior characterization

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

Sabooni, S., E-mail: s.sabooni@ma.iut.ac.ir; Karimzadeh, F.; Enayati, M.H.

In the present study, an ultrafine grained (UFG) AISI 304L stainless steel with the average grain size of 650 nm was successfully welded by both gas tungsten arc welding (GTAW) and friction stir welding (FSW). GTAW was applied without any filler metal. FSW was also performed at a constant rotational speed of 630 rpm and different welding speeds from 20 to 80 mm/min. Microstructural characterization was carried out by High Resolution Scanning Electron Microscopy (HRSEM) with Electron Backscattered Diffraction (EBSD) and Transmission Electron Microscopy (TEM). Nanoindentation, microhardness measurements and tensile tests were also performed to study the mechanical properties ofmore » the base metal and weldments. The results showed that the solidification mode in the GTAW welded sample is FA (ferrite–austenite) type with the microstructure consisting of an austenite matrix embedded with lath type and skeletal type ferrite. The nugget zone microstructure in the FSW welded samples consisted of equiaxed dynamically recrystallized austenite grains with some amount of elongated delta ferrite. Sigma phase precipitates were formed in the region ahead the rotating tool during the heating cycle of FSW, which were finally fragmented into nanometric particles and distributed in the weld nugget. Also there is a high possibility that the existing delta ferrite in the microstructure rapidly transforms into sigma phase particles during the short thermal cycle of FSW. These suggest that high strain and deformation during FSW can promote sigma phase formation. The final austenite grain size in the nugget zone was found to decrease with increasing Zener–Hollomon parameter, which was obtained quantitatively by measuring the peak temperature, calculating the strain rate during FSW and exact examination of hot deformation activation energy by considering the actual grain size before the occurrence of dynamic recrystallization. Mechanical properties observations showed that the welding efficiency of the FSW welded sample is around 70%, which is more than 20% higher than the GTAW welded sample. - Highlights: • Microstructure and mechanical properties of UFG 304L stainless steel were studied during GTAW and FSW. • Sigma phase formation mechanism was studied during FSW of 304L stainless steel. • THERMOCALC analysis was performed to obtain possible formation temperatures for sigma phase. • Nano-mechanical twins were found in the TMAZ region.« less

Modelling study on the three-dimensional neutron depolarisation response of the evolving ferrite particle size distribution during the austenite-ferrite phase transformation in steels

NASA Astrophysics Data System (ADS)

Fang, H.; van der Zwaag, S.; van Dijk, N. H.

2018-07-01

The magnetic configuration of a ferromagnetic system with mono-disperse and poly-disperse distribution of magnetic particles with inter-particle interactions has been computed. The analysis is general in nature and applies to all systems containing magnetically interacting particles in a non-magnetic matrix, but has been applied to steel microstructures, consisting of a paramagnetic austenite phase and a ferromagnetic ferrite phase, as formed during the austenite-to-ferrite phase transformation in low-alloyed steels. The characteristics of the computational microstructures are linked to the correlation function and determinant of depolarisation matrix, which can be experimentally obtained in three-dimensional neutron depolarisation (3DND). By tuning the parameters in the model used to generate the microstructure, we studied the effect of the (magnetic) particle size distribution on the 3DND parameters. It is found that the magnetic particle size derived from 3DND data matches the microstructural grain size over a wide range of volume fractions and grain size distributions. A relationship between the correlation function and the relative width of the particle size distribution was proposed to accurately account for the width of the size distribution. This evaluation shows that 3DND experiments can provide unique in situ information on the austenite-to-ferrite phase transformation in steels.

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.

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.

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

Deformation of olivine during phase transformation to wadsleyite

NASA Astrophysics Data System (ADS)

Mohiuddin, A.; Girard, J.; Karato, S. I.

2017-12-01

The strength of subducting slabs in the transition zone is critical in controlling the style of mantle convection. However, rheological properties of a subducted slab are elusive: low temperatures of a slab would make slabs strong, but in many regions there is evidence of intense deformation of slabs in the transition zone. One potential cause of intense deformation of subducting slabs is grain size reduction and accompanied microstructural changes during phase transformation of olivine to its higher-pressure polymorphs. There have been no experimental studies to quantify the influence of grain-size evolution. In addition to grain size reduction, distribution of small grains during phase transformation governs the degree of weakening during phase transformation (for e.g. load bearing framework vs. inter-connected layered framework). We conducted laboratory studies on the size and spatial distribution of new grains of wadsleyite after the transformation from olivine. Our results under static conditions show that an interconnected microstructure develops during the initial stage of phase transformation and that the grain size of the interconnected phase (wadsleyite) depends on the temperature at which the phase transformation occurs (smaller grains at lower temperatures). Development of an interconnected microstructure may lead to strain localization in the weaker phase, i.e. the fine-grained interconnected network accommodates most of the strain and therefore weakening of the entire composite. We will test this model through a series of two synchrotron in-situ deformation experiments: (i) Olivine aggregate will be deformed during slow pressure increase from deep upper mantle pressure ( 10 GPa) to transition zone pressure ( 15 GPa) at a given temperature simulating the deformation of a slab penetrating into the transition zone (ii) olivine is partially transformed to wadsleyite in a multi anvil apparatus at Yale and will be deformed within the stability field where olivine and wadsleyite coexist. We will use the Rotational Drickamer Apparatus (RDA) at a synchrotron facility (Argonne National Lab, 6-BM-B beamline, white beam and x-ray radiography) and characterize the stresses acting on olivine and wadsleyite during such simulations. We plan to present our preliminary results.

The effect of preparation conditions on the structure and mechanical properties of reaction-sintered silicon nitride

NASA Technical Reports Server (NTRS)

Heinrich, J.

1980-01-01

The microstructure of reaction sintered silicon nitride (RSSN) was changed over a wide range by varying the grain density, grain size of the silicon starting powder, nitriding conditions, and by introducing artificial pores. The influence of single microstructural parameters on mechanical properties like room temperature strength, creep behavior, and resistance to thermal shock was investigated. The essential factors influencing these properties were found to be total porosity, pore size distribution, and the fractions of alpha and beta Si3N4. In view of high temperature engineering applications of RSSN, potentials for optimizing the material's properties by controlled processing are discussed.

Effects of Degassing on the Microstructure, Chemistry, and Estimated Mechanical Properties of a Cryomilled Al-Mg Alloy

NASA Astrophysics Data System (ADS)

Hofmeister, Clara; Zhou, Le; Kellogg, Frank; Giri, Anit; Cho, Kyu; Sohn, Yongho

2018-04-01

Nanostructured aluminum alloys produced through cryomilling have generated interest due to their potential to create consolidated parts with high strength and low density. Degassing prior to consolidation minimizes adsorbed and absorbed volatiles, but is accompanied by microstructural changes such as grain growth, dislocation annihilation, and formation of dispersoids. These changes can influence the mechanical behavior of consolidated components. Cryomilled AA5083 was degassed at temperatures from 473 K to 773 K (200 °C to 500 °C) with a vacuum at or below 2.7 × 10-3 Pa. Grain size in the as-cryomilled powder (ranging from 21 to 34 nm) increased with higher degassing temperature and reached a maximum size of up to 70 to 80 nm. The dislocation density of 1.11 × 1015 m-2 in as-cryomilled powder decreased to 1.56 × 1014 m-2 for powder degassed at 773 K (500 °C). The Al6(MnFeCr) dispersoid formed when powders were degassed at or above 573 K (300 °C). Oxygen and nitrogen concentrations were unaffected by degassing; however, hydrogen concentration decreased with increasing degassing temperature to a minimum of 45 ± 3.16 ppm. Evolutions in composition and microstructure in cryomilled AA5083 were correlated to the strengthening mechanisms of grain size reduction (i.e., Hall-Petch), dislocation forest, and Orowan. However, strengthening by grain size reduction was the dominant strengthening mechanism.

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.

Modeling the Effects of Coolant Application in Friction Stir Processing on Material Microstructure Using 3D CFD Analysis

NASA Astrophysics Data System (ADS)

Aljoaba, Sharif; Dillon, Oscar; Khraisheh, Marwan; Jawahir, I. S.

2012-07-01

The ability to generate nano-sized grains is one of the advantages of friction stir processing (FSP). However, the high temperatures generated during the stirring process within the processing zone stimulate the grains to grow after recrystallization. Therefore, maintaining the small grains becomes a critical issue when using FSP. In the present reports, coolants are applied to the fixture and/or processed material in order to reduce the temperature and hence, grain growth. Most of the reported data in the literature concerning cooling techniques are experimental. We have seen no reports that attempt to predict these quantities when using coolants while the material is undergoing FSP. Therefore, there is need to develop a model that predicts the resulting grain size when using coolants, which is an important step toward designing the material microstructure. In this study, two three-dimensional computational fluid dynamics (CFD) models are reported which simulate FSP with and without coolant application while using the STAR CCM+ CFD commercial software. In the model with the coolant application, the fixture (backing plate) is modeled while is not in the other model. User-defined subroutines were incorporated in the software and implemented to investigate the effects of changing process parameters on temperature, strain rate and material velocity fields in, and around, the processed nugget. In addition, a correlation between these parameters and the Zener-Holloman parameter used in material science was developed to predict the grain size distribution. Different stirring conditions were incorporated in this study to investigate their effects on material flow and microstructural modification. A comparison of the results obtained by using each of the models on the processed microstructure is also presented for the case of Mg AZ31B-O alloy. The predicted results are also compared with the available experimental data and generally show good agreement.

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.

The origin of coercivity decrease in fine grained Nd-Fe-B sintered magnets

NASA Astrophysics Data System (ADS)

Li, W. F.; Ohkubo, T.; Hono, K.; Sagawa, M.

2009-04-01

Microstructures of fine grained Nd-Fe-B sintered magnets that were produced by the pressless process were investigated to understand the origin of the sudden coercivity decrease below a certain grain size. The intrinsic coercivity is inversely proportional to ln D2 with the highest coercivity of 17 kOe at D˜4.5 μm, below which the coercivity drops as the grain size decreases. We found that the degradation of the coercivity of the magnet with a grain size of 3 μm was mainly caused by the inhomogeneous distribution of fcc-Nd oxide whose volume fraction increased with respect to the dhcp Nd-rich phase.

Effect of hypoeutectic boron additions on the grain size and mechanical properties of Ti-6Al-4V manufactured with powder bed electron beam additive manufacturing

DOE PAGES

Mahbooba, Zaynab; West, Harvey; Harrysson, Ola; ...

2016-12-02

In additive manufacturing, microstructural control is feasible via processing parameter alteration. However, the window for parameter variation for certain materials, such as Ti-6Al-4V, is limited, and alternative methods must be employed to customize microstructures. Grain refinement and homogenization in cast titanium alloys has been demonstrated through the addition of hypoeutectic concentrations of boron. This work explores the influence of 0.00 wt.%, 0.25 wt.%, 0.50 wt.%, and 1.0 wt.% boron additions on the microstructure and bulk mechanical properties of Ti-6Al-4V samples fabricated in an Arcam A2 electron beam melting (EBM) system with commercial processing parameters for Ti-6Al-4V. Analyses of EBM fabricatedmore » Ti-6Al-4V + B indicate that the addition of 0.25–1.0 wt.% boron progressively refines the grain structure, and it improves hardness and elastic modulus. Furthermore, despite a reduction in size, the β grain structure remained columnar as a result of directional heat transfer during EBM fabrication.« 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%.

Effect of hypoeutectic boron additions on the grain size and mechanical properties of Ti-6Al-4V manufactured with powder bed electron beam additive manufacturing

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

Mahbooba, Zaynab; West, Harvey; Harrysson, Ola

In additive manufacturing, microstructural control is feasible via processing parameter alteration. However, the window for parameter variation for certain materials, such as Ti-6Al-4V, is limited, and alternative methods must be employed to customize microstructures. Grain refinement and homogenization in cast titanium alloys has been demonstrated through the addition of hypoeutectic concentrations of boron. This work explores the influence of 0.00 wt.%, 0.25 wt.%, 0.50 wt.%, and 1.0 wt.% boron additions on the microstructure and bulk mechanical properties of Ti-6Al-4V samples fabricated in an Arcam A2 electron beam melting (EBM) system with commercial processing parameters for Ti-6Al-4V. Analyses of EBM fabricatedmore » Ti-6Al-4V + B indicate that the addition of 0.25–1.0 wt.% boron progressively refines the grain structure, and it improves hardness and elastic modulus. Furthermore, despite a reduction in size, the β grain structure remained columnar as a result of directional heat transfer during EBM fabrication.« less

MUTLI-OBJECTIVE OPTIMIZATION OF MICROSTRUCTURE IN WROUGHT MAGNESIUM ALLOYS

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

Radhakrishnan, Balasubramaniam; Gorti, Sarma B; Simunovic, Srdjan

2013-01-01

The microstructural features that govern the mechanical properties of wrought magnesium alloys include grain size, crystallographic texture, and twinning. Several processes based on shear deformation have been developed that promote grain refinement, weakening of the basal texture, as well as the shift of the peak intensity away from the center of the basal pole figure - features that promote room temperature ductility in Mg alloys. At ORNL, we are currently exploring the concept of introducing nano-twins within sub-micron grains as a possible mechanism for simultaneously improving strength and ductility by exploiting a potential dislocation glide along the twin-matrix interface amore » mechanism that was originally proposed for face-centered cubic materials. Specifically, we have developed an integrated modeling and optimization framework in order to identify the combinations of grain size, texture and twin spacing that can maximize strength-ductility combinations. A micromechanical model that relates microstructure to material strength is coupled with a failure model that relates ductility to a critical shear strain and a critical hydrostatic stress. The micro-mechanical model is combined with an optimization tool based on genetic algorithm. A multi-objective optimization technique is used to explore the strength-ductility space in a systematic fashion and identify optimum combinations of the microstructural parameters that will simultaneously maximize the strength-ductility in the alloy.« less

Impurity precipitation in atomized particles evidenced by nano x-ray diffraction computed tomography

NASA Astrophysics Data System (ADS)

Bonnin, Anne; Wright, Jonathan P.; Tucoulou, Rémi; Palancher, Hervé

2014-08-01

Performances and physical properties of high technology materials are influenced or even determined by their initial microstructure and by the behavior of impurity phases. Characterizing these impurities and their relations with the surrounding matrix is therefore of primary importance but it unfortunately often requires a destructive approach, with the risk of misinterpreting the observations. The improvement we have done in high resolution X-ray diffraction computed tomography combined with the use of an X-ray nanoprobe allows non-destructive crystallographic description of materials with microscopic heterogeneous microstructure (with a grain size between 10 nm and 10 μm). In this study, the grain localization in a 2D slice of a 20 μm solidified atomized γU-Mo particle is shown and a minority U(C,O) phase (1 wt. %) with sub-micrometer sized grains was characterized inside. Evidence is presented showing that the onset of U(C,O) grain crystallization can be described by a precipitation mechanism since one single U-Mo grain has direct orientation relationship with more than one surrounding U(C,O) grains.

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.

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

Effect of Ag and Pb Addition on Microstructural and Mechanical Properties of SAC 105 Solders

NASA Astrophysics Data System (ADS)

Molnar, Aliz; Janovszky, Dora; Kardos, Ibolya; Molnar, Istvan; Gacsi, Zoltan

2015-10-01

Melting and crystallization processes of lead-free and lead-contaminated alloys in near-equilibrium state were investigated. In addition, the effect of silver content up to 4 wt.% on the microstructure of Sn-Ag-Cu alloys was studied. The volume fraction of β-Sn decreased by half owing to 4 wt.% Ag content. Furthermore, contamination by lead strongly influences the properties of the solidified microstructure. The Pb grains appear as a result of two processes when the Pb content is equal to 0.5 wt.% or higher: Pb phase solidifies in the quaternary eutectic at 176°C, and Pb grains precipitate from the primary β-Sn solid solution grain during a solid state reaction. The freezing range enlarges to 51°C due to 2 wt.% Pb content owing to quaternary eutectic. Above 1 wt.% Pb content, the mechanical properties also improve due to grains of quaternary eutectic Pb and precipitated Pb grains with a size <1 μm.

Grain boundary engineering: fatigue fracture

NASA Astrophysics Data System (ADS)

Das, Arpan

2017-04-01

Grain boundary engineering has revealed significant enhancement of material properties by modifying the populations and connectivity of different types of grain boundaries within the polycrystals. The character and connectivity of grain boundaries in polycrystalline microstructures control the corrosion and mechanical behaviour of materials. A comprehensive review of the previous researches has been carried out to understand this philosophy. Present research thoroughly explores the effect of total strain amplitude on phase transformation, fatigue fracture features, grain size, annealing twinning, different grain connectivity and grain boundary network after strain controlled low cycle fatigue deformation of austenitic stainless steel under ambient temperature. Electron backscatter diffraction technique has been used extensively to investigate the grain boundary characteristics and morphologies. The nominal variation of strain amplitude through cyclic plastic deformation is quantitatively demonstrated completely in connection with the grain boundary microstructure and fractographic features to reveal the mechanism of fatigue fracture of polycrystalline austenite. The extent of boundary modifications has been found to be a function of the number of applied loading cycles and strain amplitudes. It is also investigated that cyclic plasticity induced martensitic transformation strongly influences grain boundary characteristics and modifications of the material's microstructure/microtexture as a function of strain amplitudes. The experimental results presented here suggest a path to grain boundary engineering during fatigue fracture of austenite polycrystals.

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

Tiegs, T.N.

The Cooperative Research and Development Agreement (CRADA) was to develop composites of TiC-Ni{sub 3}Al with refined grain microstructures for application in diesel engine fuel injection devices. Grain refinement is important for improved wear resistance and high strength for the applications of interest. Attrition milling effectively reduces the initial particle size and leads to a reduction of the final grain size. However, an increase in the oxygen content occurs concomitantly with the grinding operation and decreased densification of the compacts occurs during sintering.

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

Microstructure development in Kolmogorov, Johnson-Mehl, and Avrami nucleation and growth kinetics

NASA Astrophysics Data System (ADS)

Pineda, Eloi; Crespo, Daniel

1999-08-01

A statistical model with the ability to evaluate the microstructure developed in nucleation and growth kinetics is built in the framework of the Kolmogorov, Johnson-Mehl, and Avrami theory. A populational approach is used to compute the observed grain-size distribution. The impingement process which delays grain growth is analyzed, and the effective growth rate of each population is estimated considering the previous grain history. The proposed model is integrated for a wide range of nucleation and growth protocols, including constant nucleation, pre-existing nuclei, and intermittent nucleation with interface or diffusion-controlled grain growth. The results are compared with Monte Carlo simulations, giving quantitative agreement even in cases where previous models fail.

Role of microstructure on twin nucleation and growth in HCP titanium: A statistical study

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

Arul Kumar, M.; Wroński, M.; McCabe, Rodney James

In this study, a detailed statistical analysis is performed using Electron Back Scatter Diffraction (EBSD) to establish the effect of microstructure on twin nucleation and growth in deformed commercial purity hexagonal close packed (HCP) titanium. Rolled titanium samples are compressed along rolling, transverse and normal directions to establish statistical correlations for {10–12}, {11–21}, and {11–22} twins. A recently developed automated EBSD-twinning analysis software is employed for the statistical analysis. Finally, the analysis provides the following key findings: (I) grain size and strain dependence is different for twin nucleation and growth; (II) twinning statistics can be generalized for the HCP metalsmore » magnesium, zirconium and titanium; and (III) complex microstructure, where grain shape and size distribution is heterogeneous, requires multi-point statistical correlations.« less

Role of microstructure on twin nucleation and growth in HCP titanium: A statistical study

DOE PAGES

Arul Kumar, M.; Wroński, M.; McCabe, Rodney James; ...

2018-02-01

In this study, a detailed statistical analysis is performed using Electron Back Scatter Diffraction (EBSD) to establish the effect of microstructure on twin nucleation and growth in deformed commercial purity hexagonal close packed (HCP) titanium. Rolled titanium samples are compressed along rolling, transverse and normal directions to establish statistical correlations for {10–12}, {11–21}, and {11–22} twins. A recently developed automated EBSD-twinning analysis software is employed for the statistical analysis. Finally, the analysis provides the following key findings: (I) grain size and strain dependence is different for twin nucleation and growth; (II) twinning statistics can be generalized for the HCP metalsmore » magnesium, zirconium and titanium; and (III) complex microstructure, where grain shape and size distribution is heterogeneous, requires multi-point statistical correlations.« less

A Community Database of Quartz Microstructures: Can we make measurements that constrain rheology?

NASA Astrophysics Data System (ADS)

Toy, Virginia; Peternell, Mark; Morales, Luiz; Kilian, Ruediger

2014-05-01

Rheology can be explored by performing deformation experiments, and by examining resultant microstructures and textures as links to naturally deformed rocks. Certain deformation processes are assumed to result in certain microstructures or textures, of which some might be uniquely indicative, while most cannot be unequivocally used to interpret the deformation mechanism and hence rheology. Despite our lack of a sufficient understanding of microstructure and texture forming processes, huge advances in texture measurements and quantification of microstructural parameters have been made. Unfortunately, there are neither standard procedures nor a common consensus on interpretation of many parameters (e.g. texture, grain size, shape preferred orientation). Textures (crystallographic preferred orientations) have been extensively correlated to the interpretation of deformation mechanisms. For example the strength of textures can be measured either from the orientation distribution function (e.g. the J-index (Bunge, 1983) or texture entropy (Hielscher et al., 2007) or via the intensity of polefigures. However, there are various ways to identify a representative volume, to measure, to process the data and to calculate an odf and texture descriptors, which restricts their use as a comparative and diagnostic measurement. Microstructural parameters such as grain size, grain shape descriptors and fabric descriptors are similarly used to deduce and quantify deformation mechanisms. However there is very little consensus on how to measure and calculate some of these very important parameters, e.g. grain size which makes comparison of a vast amount of precious data in the literature very difficult. We propose establishing a community database of a standard set of such measurements, made using typical samples of different types of quartz rocks through standard methods of microstructural and texture quantification. We invite suggestions and discussion from the community about the worth of proposed parameters, methodology and usefulness and willingness to contribute to a database with free access of the community. We further invite institutions to participate on a benchmark analysis of a set of 'standard' thin sections. Bunge, H.J. 1983, Texture Analysis in Materials Science: mathematical methods. Butterworth-Heinemann, 593pp. Hielscher, R., Schaeben, H., Chateigner, D., 2007, On the entropy to texture index relationship in quantitative texture analysis: Journal of Applied Crystallography 40, 371-375.

The effect of thermal processing on microstructure and mechanical properties in a nickel-iron alloy

NASA Astrophysics Data System (ADS)

Yang, Ling

The correlation between processing conditions, resulted microstructure and mechanical properties is of interest in the field of metallurgy for centuries. In this work, we investigated the effect of thermal processing parameters on microstructure, and key mechanical properties to turbine rotor design: tensile yield strength and crack growth resistance, for a nickel-iron based superalloy Inconel 706. The first step of the designing of experiments is to find parameter ranges for thermal processing. Physical metallurgy on superalloys was combined with finite element analysis to estimate variations in thermal histories for a large Alloy 706 forging, and the results were adopted for designing of experiments. Through the systematic study, correlation was found between the processing parameters and the microstructure. Five different types of grain boundaries were identified by optical metallography, fractography, and transmission electron microscopy, and they were found to be associated with eta precipitation at the grain boundaries. Proportions of types of boundaries, eta size, spacing and angle respect to the grain boundary were found to be dependent on processing parameters. Differences in grain interior precipitates were also identified, and correlated with processing conditions. Further, a strong correlation between microstructure and mechanical properties was identified. The grain boundary precipitates affect the time dependent crack propagation resistance, and different types of boundaries have different levels of resistance. Grain interior precipitates were correlated with tensile yield strength. It was also found that there is a strong environmental effect on time dependent crack propagation resistance, and the sensitivity to environmental damage is microstructure dependent. The microstructure with eta decorated on grain boundaries by controlled processing parameters is more resistant to environmental damage through oxygen embrittlement than material without eta phase on grain boundaries. Effort was made to explore the mechanisms of improving the time dependent crack propagation resistance through thermal processing, several mechanisms were identified in both environment dependent and environment independent category, and they were ranked based on their contributions in affecting crack propagation.

Parameters controlling microstructures and resistance switching of electrodeposited cuprous oxide thin films

NASA Astrophysics Data System (ADS)

Yazdanparast, Sanaz

2016-12-01

Cuprous oxide (Cu2O) thin films were electrodeposited cathodically from a highly alkaline bath using tartrate as complexing agent. Different microstructures for Cu2O thin films were achieved by varying the applied potential from -0.285 to -0.395 V versus a reference electrode of Ag/AgCl at 50 °C in potentiostatic mode, and separately by changing the bath temperature from 25 to 50 °C in galvanostatic mode. Characterization experiments showed that both grain size and orientation of Cu2O can be controlled by changing the applied potential. Applying a high negative potential of -0.395 V resulted in smaller grain size of Cu2O thin films with a preferred orientation in [111] direction. An increase in the bath temperature in galvanostatic electrodeposition increased the grain size of Cu2O thin films. All the films in Au/Cu2O/Au-Pd cell showed unipolar resistance switching behavior after an initial FORMING process. Increasing the grain size of Cu2O thin films and decreasing the top electrode area increased the FORMING voltage and decreased the current level of high resistance state (HRS). The current in low resistance state (LRS) was independent of the top electrode area and the grain size of deposited films, suggesting a filamentary conduction mechanism in unipolar resistance switching of Cu2O.

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.

Manufacture of gradient micro-structures of magnesium alloys using two stage extrusion dies

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

Hwang, Yeong-Maw; Huang, Tze-Hui; Alexandrov, Sergei

2013-12-16

This paper aims to manufacture magnesium alloy metals with gradient micro-structures using hot extrusion process. The extrusion die was designed to have a straight channel part combined with a conical part. Materials pushed through this specially-designed die generate a non-uniform velocity distribution at cross sections inside the die and result in different strain and strain rate distributions. Accordingly, a gradient microstructure product can be obtained. Using the finite element analysis, the forming temperature, effective strain, and effective strain rate distributions at the die exit were firstly discussed for various inclination angles in the conical die. Then, hot extrusion experiments withmore » a two stage die were conducted to obtain magnesium alloy products with gradient micro-structures. The effects of the inclination angle on the grain size distribution at cross sections of the products were also discussed. Using a die of an inclination angle of 15°, gradient micro-structures of the grain size decreasing gradually from 17 μm at the center to 4 μm at the edge of product were achieved.« less

Effect of grain growth of [beta]-silicon nitride on strength, Weibull modulus, and fracture toughness

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

Hirosaki, Naota; Akimune, Yoshio; Mitomo, Mamoru

1993-07-01

[beta]-Si[sub 3]N[sub 4] powder containing 1 mol% of equimolar Y[sub 2]O[sub 3]-Nd[sub 2]O[sub 3] was gas-pressure sintered at 2,000C for 2 h (SN2), 4 h (SN4), and 8 h (SN8) in 30-MPa nitrogen gas. These materials had a microstructure of in-situ composites'' as a result of exaggerated grain growth of some [beta]-Si[sub 3]N[sub 4] grains during firing. Growth of elongated grains was controlled by the sintering time, so that the desired microstructures were obtained. SN2 had a Weibull modulus as high as 53 because of the uniform size and spatial distribution of its large grains. SN4 had a fracture toughnessmore » of 10.3 MPa[center dot]m[sup 1/2] because of toughening provided by the bridging of elongated grains, whereas SN8 showed a lower fracture toughness, possibly caused by extensive microcracking resulting from excessively large grains. Gas-pressure sintering of [beta]-Si[sub 3]N[sub 4] powder was shown to be effective in fostering selective grain growth for obtaining the desired composite microstructure.« less

Calculation for tensile strength and fracture toughness of granite with three kinds of grain sizes using three-point-bending test

PubMed Central

Yu, Miao; Wei, Chenhui; Niu, Leilei; Li, Shaohua; Yu, Yongjun

2018-01-01

Tensile strength and fracture toughness, important parameters of the rock for engineering applications are difficult to measure. Thus this paper selected three kinds of granite samples (grain sizes = 1.01mm, 2.12mm and 3mm), used the combined experiments of physical and numerical simulation (RFPA-DIP version) to conduct three-point-bending (3-p-b) tests with different notches and introduced the acoustic emission monitor system to analyze the fracture mechanism around the notch tips. To study the effects of grain size on the tensile strength and toughness of rock samples, a modified fracture model was established linking fictitious crack to the grain size so that the microstructure of the specimens and fictitious crack growth can be considered together. The fractal method was introduced to represent microstructure of three kinds of granites and used to determine the length of fictitious crack. It is a simple and novel method to calculate the tensile strength and fracture toughness directly. Finally, the theoretical model was verified by the comparison to the numerical experiments by calculating the nominal strength σn and maximum loads Pmax. PMID:29596422

Calculation for tensile strength and fracture toughness of granite with three kinds of grain sizes using three-point-bending test.

PubMed

Yu, Miao; Wei, Chenhui; Niu, Leilei; Li, Shaohua; Yu, Yongjun

2018-01-01

Tensile strength and fracture toughness, important parameters of the rock for engineering applications are difficult to measure. Thus this paper selected three kinds of granite samples (grain sizes = 1.01mm, 2.12mm and 3mm), used the combined experiments of physical and numerical simulation (RFPA-DIP version) to conduct three-point-bending (3-p-b) tests with different notches and introduced the acoustic emission monitor system to analyze the fracture mechanism around the notch tips. To study the effects of grain size on the tensile strength and toughness of rock samples, a modified fracture model was established linking fictitious crack to the grain size so that the microstructure of the specimens and fictitious crack growth can be considered together. The fractal method was introduced to represent microstructure of three kinds of granites and used to determine the length of fictitious crack. It is a simple and novel method to calculate the tensile strength and fracture toughness directly. Finally, the theoretical model was verified by the comparison to the numerical experiments by calculating the nominal strength σn and maximum loads Pmax.

Micromagnetic finite element simulation of nanocrystalline α-Fe/Nd2Fe14B/Fe3B magnets

NASA Astrophysics Data System (ADS)

Saiden, N. M.; Schrefl, T.; Davies, H. A.; Hrkac, G.

2014-09-01

Nanocomposite Nd2Fe14B permanent magnets with Fe3B and α-Fe as the soft phase have been simulated using micromagnetic modelling. This paper reviews extensively the results from the simulation point of view. The magnetization configuration along the hysteresis loop is discussed in details. It was clear that the grain size and phase distribution play important roles in determining the magnetic properties. By changing the size of the grain and the volume fraction of the hard and soft phase, the magnetic properties change and the relationship between microstructure and properties is investigated. The remanence, Jr increases with decreasing of grain size, but oppositely for coercivity, Hc. The highest Jr, 1.46 T was obtained with a grain size 10 nm, and volume fraction of α-Fe, 40%. Whereas, the highest Hc with combination Nd2Fe14B 80% and 20% Fe3B, 947 kA/m. On the other hand, if Nd2Fe14B alone, the Hc able to reach up to 1000 kA/m. From this study, micromagnetic modelling contributes to a better understanding how microstructure and phase distribution influences the magnetic properties.

Highly oriented NdFeCoB nanocrystalline magnets from partially disproportionated compacts by reactive deformation under low pressure

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

Zheng, Qing; Li, Jun; Liu, Ying, E-mail: liuying5536@163.com

2014-05-07

In the present investigation, we take advantage of the ultrafine grain size of NdFeCoB partially hydrogen-disproportionated phases, and prepare anisotropic nanocrystalline magnets with full density and homogenous microstructure and texture by reactive deformation under low pressure. Our results suggest that the pressure could properly promote an occurrence of desorption-recombination reaction due to a shorter-range rearrangement of the atoms, and the newly recombined Nd{sub 2}Fe{sub 14}B grains with fine grain size could undergo deformation immediately after the phase transformation, and then an obvious anisotropy and uniform alignment would be obtained. The maximum magnetic properties, (BH){sub max} = 25.8 MGOe, Br = 11.8 kG, H{sub cj} = 5.5more » kOe, were obtained after being treated for 5 min at 820 °C in vacuum. The present study highlights the feasibility to prepare anisotropic nanocrystalline magnets with homogeneous microstructure and a strong (00l) texture of uniform grain size under low pressure.« less

Influence of Microstructure Representation on Flow Stress and Grain Size Prediction in Through-Process Modeling of AA5182 Sheet Production

NASA Astrophysics Data System (ADS)

Lohmar, Johannes; Bambach, Markus; Karhausen, Kai F.

2013-01-01

Integrated computational materials engineering is an up to date method for developing new materials and optimizing complete process chains. In the simulation of a process chain, material models play a central role as they capture the response of the material to external process conditions. While much effort is put into their development and improvement, less attention is paid to their implementation, which is problematic because the representation of microstructure in the model has a decisive influence on modeling accuracy and calculation speed. The aim of this article is to analyze the influence of different microstructure representation concepts on the prediction of flow stress and microstructure evolution when using the same set of material equations. Scalar, tree-based and cluster-based concepts are compared for a multi-stage rolling process of an AA5182 alloy. It was found that implementation influences the predicted flow stress and grain size, in particular in the regime of coupled hardening and softening.

Yield Asymmetry Design of Magnesium Alloys by Integrated Computational Materials Engineering

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

Li, Dongsheng; Joshi, Vineet V.; Lavender, Curt A.

2013-11-01

Deformation asymmetry of magnesium alloys is an important factor on machine design in automobile industry. Represented by the ratio of compressive yield stress (CYS) against tensile yield stress (TYS), deformation asymmetry is strongly related to microstructure, characterized by texture and grain size. Modified intermediate phi-model, a polycrystalline viscoplasticity model, is used to predict the deformation behavior of magnesium alloys with different grain sizes. Validated with experimental results, integrated computational materials engineering is applied to find out the route in achieving desired asymmetry by thermomechanical processing. In some texture, for example, rolled texture, CYS/TYS is smaller than 1 under different loadingmore » directions. In some texture, for example, extruded texture, asymmetry is large along normal direction. Starting from rolled texture, the asymmetry will increased to close to 1 along rolling direction after compressed to a strain of 0.2. Our model shows that grain refinement increases CYS/TYS. Besides texture control, grain refinement can also optimize the yield asymmetry. After the grain size decreased to a critical value, CYS/TYS reaches to 1 since CYS increases much faster than TYS. By tailoring the microstructure using texture control and grain refinement, it is achievable to optimize yield asymmetry in wrought magnesium alloys.« less

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.

Comparisons of Different Models on Dynamic Recrystallization of Plate during Asymmetrical Shear Rolling

PubMed Central

Zhang, Tao; Li, Lei; Lu, Shi-Hong; Gong, Hai; Wu, Yun-Xin

2018-01-01

Asymmetrical shear rolling with velocity asymmetry and geometry asymmetry is beneficial to enlarge deformation and refine grain size at the center of the thick plate compared to conventional symmetrical rolling. Dynamic recrystallization (DRX) plays a vital role in grain refinement during hot deformation. Finite element models (FEM) coupled with microstructure evolution models and cellular automata models (CA) are established to study the microstructure evolution of plate during asymmetrical shear rolling. The results show that a larger DRX fraction and a smaller average grain size can be obtained at the lower layer of the plate. The DRX fraction at the lower part increases with the ascending speed ratio, while that at upper part decreases. With the increase of the offset distance, the DRX fraction slightly decreases for the whole thickness of the plate. The differences in the DRX fraction and average grain size between the upper and lower surfaces increase with the ascending speed ratio; however, it varies little with the change of the speed ratio. Experiments are conducted and the CA models have a higher accuracy than FEM models as the grain morphology, DRX nuclei, and grain growth are taken into consideration in CA models, which are more similar to the actual DRX process during hot deformation. PMID:29342080

Comparisons of Different Models on Dynamic Recrystallization of Plate during Asymmetrical Shear Rolling.

PubMed

Zhang, Tao; Li, Lei; Lu, Shi-Hong; Gong, Hai; Wu, Yun-Xin

2018-01-17

Asymmetrical shear rolling with velocity asymmetry and geometry asymmetry is beneficial to enlarge deformation and refine grain size at the center of the thick plate compared to conventional symmetrical rolling. Dynamic recrystallization (DRX) plays a vital role in grain refinement during hot deformation. Finite element models (FEM) coupled with microstructure evolution models and cellular automata models (CA) are established to study the microstructure evolution of plate during asymmetrical shear rolling. The results show that a larger DRX fraction and a smaller average grain size can be obtained at the lower layer of the plate. The DRX fraction at the lower part increases with the ascending speed ratio, while that at upper part decreases. With the increase of the offset distance, the DRX fraction slightly decreases for the whole thickness of the plate. The differences in the DRX fraction and average grain size between the upper and lower surfaces increase with the ascending speed ratio; however, it varies little with the change of the speed ratio. Experiments are conducted and the CA models have a higher accuracy than FEM models as the grain morphology, DRX nuclei, and grain growth are taken into consideration in CA models, which are more similar to the actual DRX process during hot deformation.

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

The effects of surface finish and grain size on the strength of sintered silicon carbide

NASA Technical Reports Server (NTRS)

You, Y. H.; Kim, Y. W.; Lee, J. G.; Kim, C. H.

1985-01-01

The effects of surface treatment and microstructure, especially abnormal grain growth, on the strength of sintered SiC were studied. The surfaces of sintered SiC were treated with 400, 800 and 1200 grit diamond wheels. Grain growth was induced by increasing the sintering times at 2050 C. The beta to alpha transformation occurred during the sintering of beta-phase starting materials and was often accompanied by abnormal grain growth. The overall strength distributions were established using Weibull statistics. The strength of the sintered SiC is limited by extrinsic surface flaws in normal-sintered specimens. The finer the surface finish and grain size, the higher the strength. But the strength of abnormal sintering specimens is limited by the abnormally grown large tabular grains. The Weibull modulus increases with decreasing grain size and decreasing grit size for grinding.

Ring rolling process simulation for microstructure optimization

NASA Astrophysics Data System (ADS)

Franchi, Rodolfo; Del Prete, Antonio; Donatiello, Iolanda; Calabrese, Maurizio

2017-10-01

Metal undergoes complicated microstructural evolution during Hot Ring Rolling (HRR), which determines the quality, mechanical properties and life of the ring formed. One of the principal microstructure properties which mostly influences the structural performances of forged components, is the value of the average grain size. In the present paper a ring rolling process has been studied and optimized in order to obtain anular components to be used in aerospace applications. In particular, the influence of process input parameters (feed rate of the mandrel and angular velocity of driver roll) on microstructural and on geometrical features of the final ring has been evaluated. For this purpose, a three-dimensional finite element model for HRR has been developed in SFTC DEFORM V11, taking into account also microstructural development of the material used (the nickel superalloy Waspalloy). The Finite Element (FE) model has been used to formulate a proper optimization problem. The optimization procedure has been developed in order to find the combination of process parameters which allows to minimize the average grain size. The Response Surface Methodology (RSM) has been used to find the relationship between input and output parameters, by using the exact values of output parameters in the control points of a design space explored through FEM simulation. Once this relationship is known, the values of the output parameters can be calculated for each combination of the input parameters. Then, an optimization procedure based on Genetic Algorithms has been applied. At the end, the minimum value of average grain size with respect to the input parameters has been found.

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.

Effect of Grain Refinement and Cooling Rate on the Microstructure and Mechanical Properties of Secondary Al-Si-Cu Alloys

NASA Astrophysics Data System (ADS)

Timelli, Giulio; Camicia, Giordano; Ferraro, Stefano

2014-02-01

The effect of AlTi5B1 grain refinement and different solidification rates on metallurgical and mechanical properties of a secondary AlSi7Cu3Mg alloy is reported. While the Ti content ranges from 0.04 up to 0.225 wt.%, the cooling rate varies between 0.1 and 5.5 °C/s. Metallographic and thermal analysis techniques have been used to quantitatively examine the macro- and microstructural changes occurring with grain refiner addition at various cooling rates. The results indicate that a small AlTi5B1 addition produces the greatest refinement, while no significant reduction of grain size is obtained with a great amount of grain refiner. On increasing the cooling rate, a lower amount of AlTi5B1 master alloy is necessary to produce a uniform grain size throughout the casting. The combined addition of AlTi5B1 and Sr does not produce any reciprocal interaction or effect on primary α-Al and eutectic solidification. The grain refinement improves the plastic behavior of the alloy and increases the reliability of castings, as evidenced by the Weibull statistics.

A novel ultrafine-grained Fe−22Mn−0.6C TWIP steel with superior strength and ductility

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

Tian, Y.Z., E-mail: yztian@imr.ac.cn

A fully recrystallized ultrafine-grained (UFG) Fe−22wt.%Mn−0.6wt.%C twinning-induced plasticity (TWIP) steel with mean grain size of 576 nm was fabricated by cold rolling and annealing process. Tensile test showed that this UFG steel possessed high yield strength of 785 MPa, and unprecedented uniform elongation of 48%. The Hall-Petch relationship was verified from the coarse-grained (CG) regime to the ultrafine-grained (UFG) regime. The microstructures at specified tensile strains were characterized by electron backscattered diffraction (EBSD) and transmission electron microscopy (TEM). The microstructures and strain hardening behavior of the UFG TWIP steel were compared with the CG counterpart. The strong strain hardening capabilitymore » of the UFG steel is supposed to be responsible for the high strength and good ductility. - Highlights: • A fully recrystallized Fe−22Mn−0.6C TWIP steel with mean grain size of 576 nm was fabricated. • The ultrafine-grained (UFG) steel exhibits strong strain-hardening capability, excellent strength and ductility. • The Hall-Petch relationship is fitted well from the CG regime to the UFG regime.« less

Beta-Tin Grain Formation in Aluminum-Modified Lead-Free Solder Alloys

NASA Astrophysics Data System (ADS)

Reeve, Kathlene N.; Handwerker, Carol A.

2018-01-01

The limited number of independent β-Sn grain orientations that typically form during solidification of Sn-based solders and the resulting large β-Sn grain size have major effects on overall solder performance and reliability. This study analyzes whether additions of Al to Sn-Cu and Sn-Cu-Ag alloys can be used to change the grain size, morphology, and twinning structures of atomized (as-solidified) and re-melted (reflowed) β-Sn dendrites as determined using scanning electron microscopy and electron backscatter diffraction for as-solidified and reflow cycled (20-250°C, 1-5 cycles) Sn-Cu-Al and Sn-Ag-Cu-Al drip atomized spheres (260 μm diameter). The resulting microstructures were compared to as-solidified and reflow cycled Sn-Ag-Cu spheres (450 μm diameter) as well as as-solidified Sn-Ag-Cu, Sn-Cu, and Sn-Ag microstructures from the literature. Previous literature observations reporting reductions in undercooling and β-Sn grain size with Al micro-alloying additions could not be correlated to the presence of the Cu9Al4 phase or Al solute. The as-solidified spheres displayed no change in β-Sn dendrite structure or grain size when compared to non-Al-modified alloys, and the reflow cycled spheres produced high undercoolings (22-64°C), indicating a lack of potent nucleation sites. The current findings highlighted the role of Ag in the formation of the interlaced twinning structure and demonstrated that with deliberate compositional choices, formation of the alloy's β-Sn grain structure (cyclical twinning versus interlaced twinning) could be influenced, in both the as-solidified and reflow cycled states, though still not producing the fine-grain sizes and multiple orientations desired for improved thermomechanical properties.

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

The influence of surface friction on the AA2024 microstructure

NASA Astrophysics Data System (ADS)

Eliseev, A. A.; Kolubaev, E. A.; Fortuna, S. V.

2017-12-01

This work is devoted to the study of the effect of sliding at velocities close to those achieved during friction stir welding or friction drilling on the microstructural evolution of 2024 aluminum alloy. The distribution of both solid solution grains and intermetallic precipitates is analyzed. No layers of recrystallized grains depleted by precipitates, which is a common finding in FSW or friction drilling, are found below the worn surface independently of the sliding velocity. A small precipitate content and size changes alone are observed.

System and methods to determine and monitor changes in microstructural properties

DOEpatents

Turner, Joseph A

2014-11-18

A system and methods with which changes in microstructure properties such as grain size, grain elongation, texture, and porosity of materials can be determined and monitored over time to assess conditions such as stress and defects. An example system includes a number of ultrasonic transducers configured to transmit ultrasonic waves towards a target region on a specimen, a voltage source configured to excite the first and second ultrasonic transducers, and a processor configured to determine one or more properties of the specimen.

A novel route for processing cobalt–chromium–molybdenum orthopaedic alloys

PubMed Central

Patel, Bhairav; Inam, Fawad; Reece, Mike; Edirisinghe, Mohan; Bonfield, William; Huang, Jie; Angadji, Arash

2010-01-01

Spark plasma sintering has been used for the first time to prepare the ASTM F75 cobalt–chromium–molybdenum (Co–Cr–Mo) orthopaedic alloy composition using nanopowders. In the preliminary work presented in this report, the effect of processing variables on the structural features of the alloy (phases present, grain size and microstructure) has been investigated. Specimens of greater than 99.5 per cent theoretical density were obtained. Carbide phases were not detected in the microstructure but oxides were present. However, harder materials with finer grains were produced, compared with the commonly used cast/wrought processing methods, probably because of the presence of oxides in the microstructure. PMID:20200035

Microstructures and Grain Refinement of Additive-Manufactured Ti- xW Alloys

NASA Astrophysics Data System (ADS)

Mendoza, Michael Y.; Samimi, Peyman; Brice, David A.; Martin, Brian W.; Rolchigo, Matt R.; LeSar, Richard; Collins, Peter C.

2017-07-01

It is necessary to better understand the composition-processing-microstructure relationships that exist for materials produced by additive manufacturing. To this end, Laser Engineered Net Shaping (LENS™), a type of additive manufacturing, was used to produce a compositionally graded titanium binary model alloy system (Ti- xW specimen (0 ≤ x ≤ 30 wt pct), so that relationships could be made between composition, processing, and the prior beta grain size. Importantly, the thermophysical properties of the Ti- xW, specifically its supercooling parameter ( P) and growth restriction factor ( Q), are such that grain refinement is expected and was observed. The systematic, combinatorial study of this binary system provides an opportunity to assess the mechanisms by which grain refinement occurs in Ti-based alloys in general, and for additive manufacturing in particular. The operating mechanisms that govern the relationship between composition and grain size are interpreted using a model originally developed for aluminum and magnesium alloys and subsequently applied for titanium alloys. The prior beta grain factor observed and the interpretations of their correlations indicate that tungsten is a good grain refiner and such models are valid to explain the grain-refinement process. By extension, other binary elements or higher order alloy systems with similar thermophysical properties should exhibit similar grain refinement.

Synthesis, processing and properties of TaC-TaB2-C Ceramics

DTIC Science & Technology

2010-01-01

powder used. • A very important conclusion from the present study is that the grain size of nominally pure TaC ceramics is a strong function of carbon...ceramics at temperatures as low as 1500 ◦C. The grain size of nominally pure TaC ceramics was a strong function of carbon stoichiometry. Enhanced grain...evaluate the properties of ceramics in the TaC–TaB2–C system. Published by Elsevier Ltd. Keywords: A . Sintering; B. Microstructure; D. Carbides; D. Carbon

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.

Short communication on Kinetics of grain growth and particle pinning in U-10 wt.% Mo

NASA Astrophysics Data System (ADS)

Frazier, William E.; Hu, Shenyang; Overman, Nicole; Lavender, Curt; Joshi, Vineet V.

2018-01-01

The alloy U-10 wt% Mo was annealed at temperatures ranging from 700 °C to 900 °C for periods lasting up to 24 h. Annealed microstructures were examined using Electron Backscattered Diffraction (EBSD) to obtain average grain sizes and grain size distributions. From the temporal evolution of the average grain size, the activation energy of grain growth was determined to be 172.4 ± 0.961 kJ/mol. Grain growth over the annealing period stagnated after a period of 1-4 h. This stagnation is apparently caused by the pinning effect of second-phase particles in the materials. Back-scattered electron imaging (BSE) was used to confirm that these particles do not appreciably coarsen or dissolve during annealing at the aforementioned temperatures.

Improving hydro-formability of stainless steel tubes by tube channel pressing

NASA Astrophysics Data System (ADS)

Kitano, Y.; Yuasa, M.; Miyamoto, H.; Farshidi, M. H.; Bagherpour, E.

2017-05-01

Tube channel pressing (TCP), which is one of the severe plastic deformation (SPD) technologies to refine grain size into submicron size for tubular materials, have been applied to ferritic stainless steel tubes for one pass, in order to alleviate ridging and enhance the hydro-formability. It was found that grain-scale shear bands were introduced by one-pass TCP, and texture and microstructure was successfully modified by promoting recrystallization of deformation microstructure, which is otherwise hard-to-recrystallize, in the post-TCP annealing. Elongation to failure, strain-hardening exponent (n-value) and Lankford values of both longitudinal and circumferential directions increased in comparison to with the tube fabricated by conventional process.

Investigation on Simultaneous Effects of Shot Peen and Austenitizing Time and Temperature on Grain Size and Microstructure of Austenitic Manganese Steel (Hadfield)

NASA Astrophysics Data System (ADS)

Beheshti, M.; Zabihiazadboni, M.; Ismail, M. C.; Kakooei, S.; Shahrestani, S.

2018-03-01

Optimal conditions to increase life time of casting parts have been investigated by applying various cycles of heat treatment and shot peening on Hadfield steel surface. Metallographic and SEM microstructure examinations were used to determine the effects of shot peen, austenitizing time and temperature simultaneously. The results showed that with increasing austenitizing time and temperature of casting sample, carbides resolved in austenite phase and by further increase of austenitizing temperature and time, the austenite grain size becomes larger. Metallographic images illustrated that shot peening on Hadfield steel surface; Austenite - Martensite transformation has not occurred, but its matrix hardened through twining formation process.

Nitrogen doped RGO-Co3O4 nanograin cookies: highly porous and robust catalyst for removing nitrophenol from waste water

NASA Astrophysics Data System (ADS)

Pervaiz, Erum; Syam Azhar Virk, Muhammad; Bingxue, Zhang; Yin, Conglin; Yang, Minghui

2017-09-01

The fabrication of nanograins with a uniform morphology wrapped with reduced graphene oxide (RGO) in a designed manner is critical for obtaining a large surface, high porosity and efficient catalytic ability at mild conditions. Hybrid structures of metal oxides decorated on two-dimensional (2D) RGO lacked an interface and channels between the individual grains and RGO. The present work focuses on the synthesis of RGO-wrapped Co3O4 nanograin architecture in micron-sized polyhedrons and the ability to reduce aromatic nitro compounds. Doping N in the designed microstructure polyhedrons resulted in very large surface area (1085.6 m2 g-1) and pore density (0.47 m3 g-1) microcages. Binding energies from x-ray photoelectron spectroscopy (XPS) and Raman intensities confirmed the presence of doped N and RGO-wrapped around Co3O4 nanograins. However, the morphology and microstructure was supported by FESEM and HRTEM images revealing the fabrication of high integrity RGO-Co3O4 microstructure hybrids composed of a 10 nm grain size with narrower grain size distribution. Ammonia treatment produced interconnected channels and dumbbell pores that facilitated ion exchange between the catalyst surface and the liquid medium at the grain boundary interfaces, and offered less mass transport resistance providing fast adsorption of reactants and desorption of the product causing surface renewal. Prepared N-RGO-Co3O4 shows the largest percentage reduction (96%) of p-nitrophenol (p-NP) at room temperature as compared to pure Co3O4 and RGO-Co3O4 nanograin microstructures over 10 min. Fabricated architectures can be applied effectively for fast and facile treatment of industrial waste streams with complex organic molecules.

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.

Microstructure and critical strain of dynamic recrystallization of 6082 aluminum alloy in thermal deformation

NASA Astrophysics Data System (ADS)

Ren, W. W.; Xu, C. G.; Chen, X. L.; Qin, S. X.

2018-05-01

Using high temperature compression experiments, true stress true strain curve of 6082 aluminium alloy were obtained at the temperature 460°C-560°C and the strain rate 0.01 s-1-10 s-1. The effects of deformation temperature and strain rate on the microstructure are investigated; (‑∂lnθ/∂ε) ‑ ε curves are plotted based on σ-ε curve. Critical strains of dynamic recrystallization of 6082 aluminium alloy model were obtained. The results showed lower strain rates were beneficial to increase the volume fraction of recrystallization, the average recrystallized grain size was coarse; High strain rates are beneficial to refine average grain size, the volume fraction of dynamic recrystallized grain is less than that by using low strain rates. High temperature reduced the dislocation density and provided less driving force for recrystallization so that coarse grains remained. Dynamic recrystallization critical strain model and thermal experiment results can effectively predict recrystallization critical point of 6082 aluminium alloy during thermal deformation.

Predicting the constitutive behavior of semi-solids via a direct finite element simulation: application to AA5182

NASA Astrophysics Data System (ADS)

Phillion, A. B.; Cockcroft, S. L.; Lee, P. D.

2009-07-01

The methodology of direct finite element (FE) simulation was used to predict the semi-solid constitutive behavior of an industrially important aluminum-magnesium alloy, AA5182. Model microstructures were generated that detail key features of the as-cast semi-solid: equiaxed-globular grains of random size and shape, interconnected liquid films, and pores at the triple-junctions. Based on the results of over fifty different simulations, a model-based constitutive relationship which includes the effects of the key microstructure features—fraction solid, grain size and fraction porosity—was derived using regression analysis. This novel constitutive equation was then validated via comparison with both the FE simulations and experimental stress/strain data. Such an equation can now be used to incorporate the effects of microstructure on the bulk semi-solid flow stress within a macro- scale process model.

Morphology and microstructure evolution of Ti-50 at.% Al cathodes during cathodic arc deposition of Ti-Al-N coatings

NASA Astrophysics Data System (ADS)

Syed, Bilal; Zhu, Jianqiang; Polcik, Peter; Kolozsvari, Szilard; Hâkansson, Greger; Johnson, Lars; Ahlgren, Mats; Jöesaar, Mats; Odén, Magnus

2017-06-01

Today's research on the cathodic arc deposition technique and coatings therefrom primarily focuses on the effects of, e.g., nitrogen partial pressure, growth temperature, and substrate bias. Detailed studies on the morphology and structure of the starting material—the cathode—during film growth and its influence on coating properties at different process conditions are rare. This work aims to study the evolution of the converted layer, its morphology, and microstructure, as a function of the cathode material grain size during deposition of Ti-Al-N coatings. The coatings were reactively grown in pure N2 discharges from powder metallurgically manufactured Ti-50 at.% Al cathodes with grain size distribution averages close to 1800, 100, 50, and 10 μm, respectively, and characterized with respect to microstructure, composition, and mechanical properties. The results indicate that for the cathode of 1800 μm grain size the disparity in the work function among parent phases plays a dominant role in the pronounced erosion of Al, which yields the coatings rich in macro-particles and of high Al content. We further observed that a reduction in the grain size of Ti-50 at.% Al cathodes to 10 μm provides favorable conditions for self-sustaining reactions between Ti and Al phases upon arcing to form γ phase. The combination of self-sustaining reaction and the arc process not only result in the formation of hole-like and sub-hole features on the converted layer but also generate coatings of high Al content and laden with macro-particles.

Influence of processing on the microstructure and mechanical properties of 14YWT

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

Hoelzer, D. T.; Unocic, K. A.; Sokolov, Mikhail A.

2016-04-25

The investigation of the mechanical alloying (MA) conditions for producing the advanced oxide dispersion strengthened (ODS) 14YWT ferritic alloy led to significant improvements in balancing the strength, ductility and fracture toughness properties while still maintaining the salient microstructural features consisting of ultra-fine grains and high concentration of Y-, Ti- and O-enriched nanoclusters. The implemented changes to the processing conditions included reducing the contamination of the powder during ball milling, applying a pre-extrusion annealing treatment on the ball milled powder and exploring different extrusion temperatures at 850 C (SM170 heat), 1000 C (SM185) and 1150 C (SM200). The microstructural studies ofmore » the three 14YWT heats showed similarities in the dispersion of nanoclusters and sub-micron size grains, indicating the microstructure was insensitive to the different extrusion conditions. Compared to past 14YWT heats, the three new heats showed lower strength, but higher ductility levels between 25 and 800 C and significantly higher fracture toughness values between 25 C and 700 C. The lower contamination levels of O, C and N achieved with improved ball milling conditions plus the slightly larger grain size were identified as important factors for improving the balance in mechanical properties of the three heats of 14YWT.« less

Evolution of microstructure of Haynes 230 and Inconel 617 under mechanical testing at high temperatures

NASA Astrophysics Data System (ADS)

Hrutkay, Kyle

Haynes 230 and Inconel 617 are austenitic nickel based superalloys, which are candidate structural materials for next generation high temperature nuclear reactors. High temperature deformation behavior of Haynes 230 and Inconel 617 have been investigated at the microstructural level in order to gain a better understanding of mechanical properties. Tensile tests were performed at strain rates ranging from 10-3-10-5 s -1 at room temperature, 600 °C, 800 °C and 950 °C. Subsequent microstructural analysis, including Scanning Electron Microscopy, Transmission Electron Microscopy, Energy-Dispersive X-ray Spectroscopy, and X-Ray Diffraction were used to relate the microstructural evolution at high temperatures to that of room temperature samples. Grain sizes and precipitate morphologies were used to determine high temperature behavior and fracture mechanics. Serrated flow was observed at intermediate and high temperatures as a result of discontinuous slip and dynamic recrystallization. The amplitude of serration increased with a decrease in the strain rate and increase in the temperature. Dynamic strain ageing was responsible for serrations at intermediate temperatures by means of a locking and unlocking phenomenon between dislocations and solute atoms. Dynamic recrystallization nucleated by grain and twin bulging resulting in a refinement of grain size. Existing models found in the literature were discussed to explain both of these phenomena.

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.

Automated grain mapping using wide angle convergent beam electron diffraction in transmission electron microscope for nanomaterials.

PubMed

Kumar, Vineet

2011-12-01

The grain size statistics, commonly derived from the grain map of a material sample, are important microstructure characteristics that greatly influence its properties. The grain map for nanomaterials is usually obtained manually by visual inspection of the transmission electron microscope (TEM) micrographs because automated methods do not perform satisfactorily. While the visual inspection method provides reliable results, it is a labor intensive process and is often prone to human errors. In this article, an automated grain mapping method is developed using TEM diffraction patterns. The presented method uses wide angle convergent beam diffraction in the TEM. The automated technique was applied on a platinum thin film sample to obtain the grain map and subsequently derive grain size statistics from it. The grain size statistics obtained with the automated method were found in good agreement with the visual inspection method.

Microstructure Optimization of Dual-Phase Steels Using a Representative Volume Element and a Response Surface Method: Parametric Study

NASA Astrophysics Data System (ADS)

Belgasam, Tarek M.; Zbib, Hussein M.

2017-12-01

Dual-phase (DP) steels have received widespread attention for their low density and high strength. This low density is of value to the automotive industry for the weight reduction it offers and the attendant fuel savings and emission reductions. Recent studies on developing DP steels showed that the combination of strength/ductility could be significantly improved when changing the volume fraction and grain size of phases in the microstructure depending on microstructure properties. Consequently, DP steel manufacturers are interested in predicting microstructure properties and in optimizing microstructure design. In this work, a microstructure-based approach using representative volume elements (RVEs) was developed. The approach examined the flow behavior of DP steels using virtual tension tests with an RVE to identify specific mechanical properties. Microstructures with varied martensite and ferrite grain sizes, martensite volume fractions, carbon content, and morphologies were studied in 3D RVE approaches. The effect of these microstructure parameters on a combination of strength/ductility of DP steels was examined numerically using the finite element method by implementing a dislocation density-based elastic-plastic constitutive model, and a Response surface methodology to determine the optimum conditions for a required combination of strength/ductility. The results from the numerical simulations are compared with experimental results found in the literature. The developed methodology proves to be a powerful tool for studying the effect and interaction of key microstructural parameters on strength and ductility and thus can be used to identify optimum microstructural conditions.

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.

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.

Grain size effect on yield strength of titanium alloy implanted with aluminum ions

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

Popova, Natalya, E-mail: natalya-popova-44@mail.ru; Institute of Strength Physics and Materials Science, SB RAS, 2/4, Akademicheskii Ave., 634021, Tomsk; Nikonenko, Elena, E-mail: vilatomsk@mail.ru

2016-01-15

The paper presents a transmission electron microscopy (TEM) study of the microstructure and phase state of commercially pure titanium VT1-0 implanted by aluminum ions. This study has been carried out before and after the ion implantation for different grain size, i.e. 0.3 µm (ultra-fine grain condition), 1.5 µm (fine grain condition), and 17 µm (polycrystalline condition). This paper presents details of calculations and analysis of strength components of the yield stress. It is shown that the ion implantation results in a considerable hardening of the entire thickness of the implanted layer in the both grain types. The grain size has, however, a differentmore » effect on the yield stress. So, both before and after the ion implantation, the increase of the grain size leads to the decrease of the alloy hardening. Thus, hardening in ultra-fine and fine grain alloys increased by four times, while in polycrystalline alloy it increased by over six times.« less

Stable Eutectoid Transformation in Nodular Cast Iron: Modeling and Validation

NASA Astrophysics Data System (ADS)

Carazo, Fernando D.; Dardati, Patricia M.; Celentano, Diego J.; Godoy, Luis A.

2017-01-01

This paper presents a new microstructural model of the stable eutectoid transformation in a spheroidal cast iron. The model takes into account the nucleation and growth of ferrite grains and the growth of graphite spheroids. Different laws are assumed for the growth of both phases during and below the intercritical stable eutectoid. At a microstructural level, the initial conditions for the phase transformations are obtained from the microstructural simulation of solidification of the material, which considers the divorced eutectic and the subsequent growth of graphite spheroids up to the initiation of the stable eutectoid transformation. The temperature field is obtained by solving the energy equation by means of finite elements. The microstructural (phase change) and macrostructural (energy balance) models are coupled by a sequential multiscale procedure. Experimental validation of the model is achieved by comparison with measured values of fractions and radius of 2D view of ferrite grains. Agreement with such experiments indicates that the present model is capable of predicting ferrite phase fraction and grain size with reasonable accuracy.

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.

Production, microstructure and mechanical properties of two different austenitic ODS steels

NASA Astrophysics Data System (ADS)

Gräning, T.; Rieth, M.; Hoffmann, J.; Möslang, A.

2017-04-01

This article is to summarize and examine processing parameters of novel developed austenitic oxide dispersed strengthened (ODS) steels. Comparing hot-rolled and extruded conditions after the same degree of deformation after and before annealing, are just some examples to give insights into the complex processing of austenitic ODS steels. One of the major drawbacks of the material is the more sophisticated production process. Due to a ductile matrix material with an increased stickiness during milling, a two-step milling procedure with the use of ZrO2 milling balls was applied to raise the production yield and to use the abrasion of the ZrO2 as an additional element to facilitate the formation of nano-sized precipitates. To get a better understanding how the different powder particle sizes after milling affect final properties, sieving was applied and revealed a serious effect in terms of precipitate size, distribution and mechanical properties. Grain sizes in relation to the precipitate size, annealing time and processing parameters were determined and compared to the mechanical properties. Hardness and tensile test have pointed out, that the precipitate size and number are more important in respect to the ultimate tensile strength than the grain size and that in this study hot-rolled material exhibited the better properties. The investigation of the microstructure illustrated the stability of precipitates during annealing at 1100 °C for 40 h. These heat treatments also led to a consistent grain size, due to the pinning effect of the grain boundaries, caused by precipitates.

cm-scale variations of crystal orientation fabric in cold Alpine ice core from Colle Gnifetti

NASA Astrophysics Data System (ADS)

Kerch, Johanna; Weikusat, Ilka; Eisen, Olaf; Wagenbach, Dietmar; Erhardt, Tobias

2015-04-01

Analysis of the microstructural parameters of ice has been an important part of ice core analyses so far mainly in polar cores in order to obtain information about physical processes (e.g. deformation, recrystallisation) on the micro- and macro-scale within an ice body. More recently the influence of impurities and climatic conditions during snow accumulation on these processes has come into focus. A deeper understanding of how palaeoclimate proxies interact with physical properties of the ice matrix bears relevance for palaeoclimatic interpretations, improved geophysical measurement techniques and the furthering of ice dynamical modeling. Variations in microstructural parameters e.g. crystal orientation fabric or grain size can be observed on a scale of hundreds and tens of metres but also on a centimetre scale. The underlying processes are not necessarily the same on all scales. Especially for the short-scale variations many questions remain unanswered. We present results from a study that aims to investigate following hypotheses: 1. Variations in grain size and fabric, i.e. strong changes of the orientation of ice crystals with respect to the vertical, occur on a centimetre scale and can be observed in all depths of an ice core. 2. Palaeoclimate proxies like dust and impurities have an impact on the microstructural processes and thus are inducing the observed short-scale variations in grain size and fabric. 3. The interaction of proxies with the ice matrix leads to depth intervals that show correlating behaviour as well as ranges with anticorrelation between microstructural parameters and palaeoclimatic proxies. The respective processes need to be identified. Fabric Analyser measurements were conducted on more than 80 samples (total of 8 m) from different depth ranges of a cold Alpine ice core (72 m length) drilled in 2013 at Colle Gnifetti, Switzerland/Italy. Results were obtained by automatic image processing, providing estimates for grain size distributions and crystal orientation fabric, and comparison with data from continuous flow analysis of chemical impurities. A microstructural characterisation of the analysed core is presented with emphasis on the observed variations in crystal orientation fabric. The relevance of these results for palaeoclimate reconstruction and geophysical applications in ice are discussed.

Cohesive zone model for intergranular slow crack growth in ceramics: influence of the process and the microstructure

NASA Astrophysics Data System (ADS)

Romero de la Osa, M.; Estevez, R.; Olagnon, C.; Chevalier, J.; Tallaron, C.

2011-10-01

Ceramic polycrystals are prone to slow crack growth (SCG) which is stress and environmentally assisted, similarly to observations reported for silica glasses. The kinetics of fracture are known to be dependent on the load level, the temperature and the relative humidity. In addition, evidence is available on the influence of the microstructure on the SCG rate with an increase in the crack velocity with decreasing the grain size. Crack propagation takes place beyond a load threshold, which is grain size dependent. We present a cohesive zone model for the intergranular failure process. The methodology accounts for an intrinsic opening that governs the length of the cohesive zone and allows the investigation of grain size effects. A rate and temperature-dependent cohesive model is proposed (Romero de la Osa M, Estevez R et al 2009 J. Mech. Adv. Mater. Struct. 16 623-31) to mimic the reaction-rupture mechanism. The formulation is inspired by Michalske and Freiman's picture (Michalske and Freiman 1983 J. Am. Ceram. Soc. 66 284-8) together with a recent study by Zhu et al (2005 J. Mech. Phys. Solids 53 1597-623) of the reaction-rupture mechanism. The present investigation extends a previous work (Romero de la Osa et al 2009 Int. J. Fracture 158 157-67) in which the problem is formulated. Here, we explore the influence of the microstructure in terms of grain size, their elastic properties and residual thermal stresses originating from the cooling from the sintering temperature down to ambient conditions. Their influence on SCG for static loadings is reported and the predictions compared with experimental trends. We show that the initial stress state is responsible for the grain size dependence reported experimentally for SCG. Furthermore, the account for the initial stresses enables the prediction of a load threshold below which no crack growth is observed: a crack arrest takes place when the crack path meets a region in compression.

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

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

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

Grain Refinement Efficiency in Commercial-Purity Aluminum Influenced by the Addition of Al-4Ti Master Alloys with Varying TiAl3 Particles

PubMed Central

Zhao, Jianhua; He, Jiansheng; Tang, Qi; Wang, Tao; Chen, Jing

2016-01-01

A series of Al-4Ti master alloys with various TiAl3 particles were prepared via pouring the pure aluminum added with K2TiF6 or sponge titanium into three different molds made of graphite, copper, and sand. The microstructure and morphology of TiAl3 particles were characterized and analyzed by scanning electron microscope (SEM) with energy dispersive spectroscopy (EDS). The microstructure of TiAl3 particles in Al-4Ti master alloys and their grain refinement efficiency in commercial-purity aluminum were investigated in this study. Results show that there were three different morphologies of TiAl3 particles in Al-4Ti master alloys: petal-like structures, blocky structures, and flaky structures. The Al-4Ti master alloy with blocky TiAl3 particles had better and more stable grain refinement efficiency than the master alloys with petal-like and flaky TiAl3 particles. The average grain size of the refined commercial-purity aluminum always hereditarily followed the size of the original TiAl3 particles. In addition, the grain refinement efficiency of Al-4Ti master alloys with the same morphology, size, and distribution of TiAl3 particles prepared through different processes was almost identical. PMID:28773987

Grain Refinement Efficiency in Commercial-Purity Aluminum Influenced by the Addition of Al-4Ti Master Alloys with Varying TiAl₃ Particles.

PubMed

Zhao, Jianhua; He, Jiansheng; Tang, Qi; Wang, Tao; Chen, Jing

2016-10-26

A series of Al-4Ti master alloys with various TiAl₃ particles were prepared via pouring the pure aluminum added with K₂TiF₆ or sponge titanium into three different molds made of graphite, copper, and sand. The microstructure and morphology of TiAl₃ particles were characterized and analyzed by scanning electron microscope (SEM) with energy dispersive spectroscopy (EDS). The microstructure of TiAl₃ particles in Al-4Ti master alloys and their grain refinement efficiency in commercial-purity aluminum were investigated in this study. Results show that there were three different morphologies of TiAl₃ particles in Al-4Ti master alloys: petal-like structures, blocky structures, and flaky structures. The Al-4Ti master alloy with blocky TiAl₃ particles had better and more stable grain refinement efficiency than the master alloys with petal-like and flaky TiAl₃ particles. The average grain size of the refined commercial-purity aluminum always hereditarily followed the size of the original TiAl₃ particles. In addition, the grain refinement efficiency of Al-4Ti master alloys with the same morphology, size, and distribution of TiAl₃ particles prepared through different processes was almost identical.

Refinement of Ferrite Grain Size near the Ultrafine Range by Multipass, Thermomechanical Compression

NASA Astrophysics Data System (ADS)

Patra, S.; Neogy, S.; Kumar, Vinod; Chakrabarti, D.; Haldar, A.

2012-11-01

Plane-strain compression testing was carried out on a Nb-Ti-V microalloyed steel, in a GLEEBLE3500 simulator using a different amount of roughing, intermediate, and finishing deformation over the temperature range of 1373 K to 1073 K (1100 °C to 800 °C). A decrease in soaking temperature from 1473 K to 1273 K (1200 °C to 1000 °C) offered marginal refinement in the ferrite ( α) grain size from 7.8 to 6.6 μm. Heavy deformation using multiple passes between A e3 and A r3 with true strain of 0.8 to 1.2 effectively refined the α grain size (4.1 to 3.2 μm) close to the ultrafine size by dynamic-strain-induced austenite ( γ) → ferrite ( α) transformation (DSIT). The intensities of microstructural banding, pearlite fraction in the microstructure (13 pct), and fraction of the harmful "cube" texture component (5 pct) were reduced with the increase in finishing deformation. Simultaneously, the fractions of high-angle (>15 deg misorientation) boundaries (75 to 80 pct), beneficial gamma-fiber (ND//<111>) texture components, along with {332}<133> and {554}<225> components were increased. Grain refinement and the formation of small Fe3C particles (50- to 600-nm size) increased the hardness of the deformed samples (184 to 192 HV). For the same deformation temperature [1103 K (830 °C)], the difference in α-grain sizes obtained after single-pass (2.7 μm) and multipass compression (3.2 μm) can be explained in view of the static- and dynamic-strain-induced γ → α transformation, strain partitioning between γ and α, dynamic recovery and dynamic recrystallization of the deformed α, and α-grain growth during interpass intervals.

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.

Microstructure and Mechanical Properties of the As-Cast and As-Homogenized Mg-Zn-Sn-Mn-Ca Alloy Fabricated by Semicontinuous Casting

PubMed Central

Lu, Xing; Zhao, Guoqun; Zhou, Jixue; Zhang, Cunsheng; Yu, Junquan

2018-01-01

In this paper, a new type of low-cost Mg-3.36Zn-1.06Sn-0.33Mn-0.27Ca (wt %) alloy ingot with a diameter of 130 mm and a length of 4800 mm was fabricated by semicontinuous casting. The microstructure and mechanical properties at different areas of the ingot were investigated. The microstructure and mechanical properties of the alloy under different one-step and two-step homogenization conditions were studied. For the as-cast alloy, the average grain size and the second phase size decrease from the center to the surface of the ingot, while the area fraction of the second phase increases gradually. At one-half of the radius of the ingot, the alloy presents the optimum comprehensive mechanical properties along the axial direction, which is attributed to the combined effect of relatively small grain size, low second-phase fraction, and uniform microstructure. For the as-homogenized alloy, the optimum two-step homogenization process parameters were determined as 340 °C × 10 h + 520 °C × 16 h. After the optimum homogenization, the proper size and morphology of CaMgSn phase are conducive to improve the microstructure uniformity and the mechanical properties of the alloy. Besides, the yield strength of the alloy is reduced by 20.7% and the elongation is increased by 56.3%, which is more favorable for the subsequent hot deformation processing. PMID:29710818

Microstructure and Mechanical Properties of the As-Cast and As-Homogenized Mg-Zn-Sn-Mn-Ca Alloy Fabricated by Semicontinuous Casting.

PubMed

Lu, Xing; Zhao, Guoqun; Zhou, Jixue; Zhang, Cunsheng; Yu, Junquan

2018-04-29

In this paper, a new type of low-cost Mg-3.36Zn-1.06Sn-0.33Mn-0.27Ca (wt %) alloy ingot with a diameter of 130 mm and a length of 4800 mm was fabricated by semicontinuous casting. The microstructure and mechanical properties at different areas of the ingot were investigated. The microstructure and mechanical properties of the alloy under different one-step and two-step homogenization conditions were studied. For the as-cast alloy, the average grain size and the second phase size decrease from the center to the surface of the ingot, while the area fraction of the second phase increases gradually. At one-half of the radius of the ingot, the alloy presents the optimum comprehensive mechanical properties along the axial direction, which is attributed to the combined effect of relatively small grain size, low second-phase fraction, and uniform microstructure. For the as-homogenized alloy, the optimum two-step homogenization process parameters were determined as 340 °C × 10 h + 520 °C × 16 h. After the optimum homogenization, the proper size and morphology of CaMgSn phase are conducive to improve the microstructure uniformity and the mechanical properties of the alloy. Besides, the yield strength of the alloy is reduced by 20.7% and the elongation is increased by 56.3%, which is more favorable for the subsequent hot deformation processing.

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

Microstructure study of a severely plastically deformed Mg-Zn-Y alloy by application of low angle annular dark field diffraction contrast imaging.

PubMed

Basha, Dudekula Althaf; Rosalie, Julian M; Somekawa, Hidetoshi; Miyawaki, Takashi; Singh, Alok; Tsuchiya, Koichi

2016-01-01

Microstructural investigation of extremely strained samples, such as severely plastically deformed (SPD) materials, by using conventional transmission electron microscopy techniques is very challenging due to strong image contrast resulting from the high defect density. In this study, low angle annular dark field (LAADF) imaging mode of scanning transmission electron microscope (STEM) has been applied to study the microstructure of a Mg-3Zn-0.5Y (at%) alloy processed by high pressure torsion (HPT). LAADF imaging advantages for observation of twinning, grain fragmentation, nucleation of recrystallized grains and precipitation on second phase particles in the alloy processed by HPT are highlighted. By using STEM-LAADF imaging with a range of incident angles, various microstructural features have been imaged, such as nanoscale subgrain structure and recrystallization nucleation even from the thicker region of the highly strained matrix. It is shown that nucleation of recrystallized grains starts at a strain level of revolution [Formula: see text] (earlier than detected by conventional bright field imaging). Occurrence of recrystallization of grains by nucleating heterogeneously on quasicrystalline particles is also confirmed. Minimizing all strain effects by LAADF imaging facilitated grain size measurement of [Formula: see text] nm in fully recrystallized HPT specimen after [Formula: see text].

Bonanza: An extremely large dust grain from a supernova

NASA Astrophysics Data System (ADS)

Gyngard, Frank; Jadhav, Manavi; Nittler, Larry R.; Stroud, Rhonda M.; Zinner, Ernst

2018-01-01

We report the morphology, microstructure, and isotopic composition of the largest SiC stardust grain known to have condensed from a supernova. The 25-μm diameter grain, termed Bonanza, was found in an acid-resistant residue of the Murchison meteorite. Grains of such large size have neither been observed around supernovae nor predicted to form in stellar environments. The large size of Bonanza has allowed the measurement of the isotopic composition of more elements in it than any other previous presolar grain, including: Li, B, C, N, Mg, Al, Si, S, Ca, Ti, Fe, and Ni. Bonanza exhibits large isotopic anomalies in the elements C, N, Mg, Si, Ca, Ti, Fe, and Ni typical of an astrophysical origin in ejecta of a Type II core-collapse supernova and comparable to those previously observed for other presolar SiC grains of type X. Additionally, we extracted multiple focused ion beam lift-out sections from different regions of the grain. Our transmission electron microscopy demonstrates that the crystalline order varies at the micrometer scale, and includes rare, higher order polytype domains (e.g., 15 R). Analyses with STEM-EDS show Bonanza contains a heterogeneous distribution of subgrains with sizes ranging from <10 nm to >100 nm of Ti(N, C); Fe, Ni-rich grains with variable Fe:Ni; and (Al, Mg)N. Bonanza also has the highest ever inferred initial 26Al/27Al ratio, consistent with its supernova origin. This unique grain affords us the largest expanse of data, both microstructurally and isotopically, to compare with detailed calculations of nucleosynthesis and dust condensation in supernovae.

The Femtosecond Laser Ablation on Ultrafine-Grained Copper

NASA Astrophysics Data System (ADS)

Lu, Jianxun; Wu, Xiaoyu; Ruan, Shuangchen; Guo, Dengji; Du, Chenlin; Liang, Xiong; Wu, Zhaozhi

2018-07-01

To investigate the effects of femtosecond laser ablation on the surface morphology and microstructure of ultrafine-grained copper, point, single-line scanning, and area scanning ablation of ultrafine-grained and coarse-grained copper were performed at room temperature. The ablation threshold gradually increased and materials processing became more difficult with decreasing grain size. In addition, the ablation depth and width of the channels formed by single-line scanning ablation gradually increased with increasing grain size for the same laser pulse energy. The microhardness of the ablated specimens was also evaluated as a function of laser pulse energy using area scanning ablation. The microhardness difference before and after ablation increased with decreasing grain size for the same laser pulse energy. In addition, the microhardness after ablation gradually decreased with increasing laser pulse energy for the ultrafine-grained specimens. However, for the coarse-grained copper specimens, no clear changes of the microhardness were observed after ablation with varying laser pulse energies. The grain sizes of the ultrafine-grained specimens were also surveyed as a function of laser pulse energy using electron backscattered diffraction (EBSD). The heat generated by laser ablation caused recrystallization and grain growth of the ultrafine-grained copper; moreover, the grain size gradually increased with increasing pulse energy. In contrast, no obvious changes in grain size were observed for the coarse-grained copper specimens with increasing pulse energy.

The Femtosecond Laser Ablation on Ultrafine-Grained Copper

NASA Astrophysics Data System (ADS)

Lu, Jianxun; Wu, Xiaoyu; Ruan, Shuangchen; Guo, Dengji; Du, Chenlin; Liang, Xiong; Wu, Zhaozhi

2018-05-01

To investigate the effects of femtosecond laser ablation on the surface morphology and microstructure of ultrafine-grained copper, point, single-line scanning, and area scanning ablation of ultrafine-grained and coarse-grained copper were performed at room temperature. The ablation threshold gradually increased and materials processing became more difficult with decreasing grain size. In addition, the ablation depth and width of the channels formed by single-line scanning ablation gradually increased with increasing grain size for the same laser pulse energy. The microhardness of the ablated specimens was also evaluated as a function of laser pulse energy using area scanning ablation. The microhardness difference before and after ablation increased with decreasing grain size for the same laser pulse energy. In addition, the microhardness after ablation gradually decreased with increasing laser pulse energy for the ultrafine-grained specimens. However, for the coarse-grained copper specimens, no clear changes of the microhardness were observed after ablation with varying laser pulse energies. The grain sizes of the ultrafine-grained specimens were also surveyed as a function of laser pulse energy using electron backscattered diffraction (EBSD). The heat generated by laser ablation caused recrystallization and grain growth of the ultrafine-grained copper; moreover, the grain size gradually increased with increasing pulse energy. In contrast, no obvious changes in grain size were observed for the coarse-grained copper specimens with increasing pulse energy.

Relationships between microstructure and microfissuring in alloy 718

NASA Technical Reports Server (NTRS)

Thompson, R. G.

1985-01-01

Microfissures which occur in the weld heat affected zone of alloy 718 can be a limiting factor in the material's weldability. Several studies have attempted to relate microfissuring susceptibility to processing conditions, microstructure, and/or heat-to-heat chemistry differences. The present investigation studies the relationships between microstructure and microfissuring by isolating a particular microstructural feature and measuring microfissuring as a function of that feature. Results to date include the identification of a microstructure-microfissure sequence, microfissuring susceptibility as a function of grain size, and microfissuring susceptibility as a function of solution annealing time.

Influence of heat treatment and hot extrusion on the microstructure and tensile properties of rare earth modified Mg-Zn based alloy

NASA Astrophysics Data System (ADS)

Sheng, L. Y.; Wang, B. J.; Du, B. N.; Lai, C.; Xi, T. F.

2018-01-01

In the present paper, the Mg-Zn-Y-Nd alloy was prepared by casting, heat treatment and hot extrusion. The microstructure and mechanical properties of the alloys were tested by OM, SEM, TEM and tensile test. The results showed that the Mg3Zn2Y3 phase is the main strengthening phase and forms the eutectic structure with α-Mg matrix in the as cast alloy. The strengthening phases semi-continuously connect and separate the α-Mg matrix into cell structure. The average grain size of the as cast alloy is about 60 μm. The heat treatment promotes the solid solution of the strengthening phase and precipitation of small particles inside grain.Compared with the as cast alloy, the heat treatment increases grain size a little and mechanical properties more than 30%. The hot extrusion refines the grain and strengthening phase, which increase the mechanical properties significantly. Moreover, the great deformation by the hot extrusion results in the ultrafine structure and abundant of crystal defects. The intersection of micro-twins lead to the special region with nanometer size.

Experimental investigation of the brittle-viscous transition in mafic rocks - Interplay between fracturing, reaction, and viscous deformation

NASA Astrophysics Data System (ADS)

Marti, Sina; Stünitz, Holger; Heilbronner, Renée; Plümper, Oliver; Drury, Martyn

2017-12-01

Rock deformation experiments are performed on fault gouge fabricated from 'Maryland Diabase' rock powder to investigate the transition from dominant brittle to dominant viscous behaviour. At the imposed strain rates of γ˙ = 3 ·10-5 - 3 ·10-6 s-1, the transition is observed in the temperature range of (600 °C < T < 800 °C) at confining pressures of (0.5 GPa ≤ Pc ≤ 1.5 GPa). The transition thereby takes place by a switch from brittle fracturing and cataclastic flow to viscous dissolution-precipitation creep and grain boundary sliding. Mineral reactions and resulting grain size refinement by nucleation are observed to be critical processes for the switch to viscous deformation, i.e., grain size sensitive creep. In the transitional regime, the mechanical response of the sample is a mixed-mode between brittle and viscous rheology and microstructures associated with both brittle and viscous deformation are observed. As grain size reduction by reaction and nucleation is a time dependent process, the brittle-viscous transition is not only a function of T but to a large extent also of microstructural evolution.

Influence of Heat Input on Microstructure and Toughness Properties in Simulated CGHAZ of X80 Steel Manufactured Using High-Temperature Processing

NASA Astrophysics Data System (ADS)

Zhu, Zhixiong; Han, Jian; Li, Huijun

2015-11-01

To determine and demonstrate the weldability of high-Nb high-temperature processed (HTP) steels and provide extremely valuable information for future line pipe steel design and general steel manufacture, in the current study the toughness in simulated coarse-grained heat-affected zone (CGHAZ) of an X80 grade steel manufactured using HTP was evaluated. The simulated CGHAZs subjected to thermal cycles with various heat inputs (HIs) (0.8 to 5.0 kJ/mm) were produced using a Gleeble 3500 simulator. The microstructures and corresponding mechanical properties were investigated by means of optical microscopy, scanning electron microscopy, electron backscatter diffraction, hardness testing, and Charpy V-notch (CVN) testing. The microstructural examination shows that the simulated CGHAZs consisted of a bainite-dominant microstructure and relatively low amount (<2 pct) of martensite-austenite (M-A) constituent. The prior austenite grain size was controlled to be 45 to 55 µm at HIs of 0.8 to 3.5 kJ/mm, and remarkably increased to 85 µm at an HI of 5 kJ/mm. The results of CVN testing suggest that superior toughness can be achieved in the studied range of HIs (0.8 to 5 kJ/mm). This is thought to be associated with the combined effects of bainitic microstructure and low M-A fraction as well as comparatively fine austenite grain size in the studied CGHAZs.

Impact of friction stir welding on the microstructure of ODS steel

NASA Astrophysics Data System (ADS)

Dawson, H.; Serrano, M.; Cater, S.; Iqbal, N.; Almásy, L.; Tian, Q.; Jimenez-Melero, E.

2017-04-01

We have assessed the impact of the welding parameters on the nano-sized oxide dispersion and the grain size in the matrix of an ODS steel after friction stir welding. Our results, based on combined small angle neutron scattering and electron microscopy, reveal a decrease in the volume fraction of the particles smaller than 80 nm in the welds, mainly due to particle agglomeration. The increase in tool rotation speed or decrease in transverse speed leads to a higher reduction in nano-sized particle fraction, and additionally to the occurrence of particle melting. The dependence of the average grain size in the matrix on the particle volume fraction follows a Zener pinning-type relationship. This result points to the principal role that the particles have in pinning grain boundary movement, and consequently in controlling the grain size during welding.

The Effects of Dy Addition on Microstructure and Mechanical Properties of the As-Cast Mg-5Al-3Ca-2Nd Alloys.

PubMed

Son, Hyeon-Taek; Kim, Yong-Ho; Yoo, Hyo-Sang

2018-03-01

The microstructure of the as-cast Mg-5Al-3Ca-2Nd-xDy alloys consists of α-Mg matrix, (Mg, Al)2Ca eutectic phase, Al-Nd and Al-Dy intermetallic compounds. α-Mg matrix morphology was changed from dendritic to equiaxed with the increase Dy addition. And grain size was remarkably refined. As Dy content was increased, yield strength was improved due to the refined grains and the homogeneous distribution of Al-Dy phase.

Linking natural microstructures with numerical modeling of pinch-and-swell structures

NASA Astrophysics Data System (ADS)

Peters, Max; Berger, Alfons; Herwegh, Marco; Regenauer-Lieb, Klaus

2016-04-01

For a variety of geological problems, the change from homogeneous to localized deformation and the establishment of steady-state conditions are equally important. Here, we show that pinch-and-swell structures are ideal candidates for the study of the switch in deformation style and mechanism during ductile creep. We present an interdisciplinary approach to the onset of pinch-and-swell structures and to the flow conditions during pre- to post-localization stages in ductile rocks. For this reason, naturally boudinaged calcite veins, embedded in a calc-mylonite, and their microfabrics were investigated quantitatively. Remnants of slightly deformed calcite hosts build up the swells, showing twinning and minor dislocation glide as crystal plastic deformation mechanisms which are accompanied by subgrain rotation recrystallization (SGR). Towards the pinches, we find a gradient of severe grain size reduction through progressive SGR, developing a characteristic dislocation creep crystallographic preferred orientation (CPO). Along this gradient, the finest recrystallized calcite grains appear randomly oriented, expressed by a "smearing-out" of the CPO and missing systematics of misorientation angles in the most extended areas. We interpret this microstructure as a switch from dislocation dominated creep to grain boundary sliding processes. Further, we show that the onset of boudinage is independent on both the original orientation and grain size of calcite hosts. We implemented these microstructural observations into a layered elasto-visco-plastic finite element framework, tracing variations in grain size (Peters et al., 2015). We base the microstructural evolution on thermo-mechanical-chemical principles and end-member flow laws (Herwegh et al., 2014). The simulated pinch-and-swell structures indicate that low strain rates in the swells favor dislocation creep, whereas accelerated rates provoke continuous grain size reduction allowing strain accommodation by diffusion creep dominated deformation at relatively high extensional strains in the pinches. The numerical simulations indicate that viscosity weakening due to dissipated heat from grain size reduction marks the onset of localization, resulting in continuous necking of the layer. Interestingly, there exist multiple steady states, i.e. a first homogeneous state out of which localization arises, steady states of the stable end-member structure, expressed by homogeneous conditions in both pinches and swells, and in the surrounding matrix, the latter obeying a linear rheology. Based on our microstructural and numerical results, we suggest that the onset of localization represents a fundamental material bifurcation. This implies that the studied structures can be described as ductile instabilities. Finally, we discuss the profound role of the energy theory of localization described here, which allows deriving the paleo-deformation conditions, as well as fundamental material properties in a self-consistent manner. REFERENCES Herwegh, M., Poulet, T., Karrech, A. and Regenauer-Lieb, K. (2014): Journal of Geophysical Research 119, doi:10.1002/2013JB010701 Peters, M., Veveakis, M., Poulet, T., Karrech, A., Herwegh, M. and Regenauer-Lieb, K. (2015): Journal of Structural Geology 78, doi:10.1016/j.jsg.2015.06.005

Evolution of grain boundary character distributions in alloy 825 tubes during high temperature annealing: Is grain boundary engineering achieved through recrystallization or grain growth?

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

Bai, Qin; Zhao, Qing

Grain boundary engineering (GBE) of nickel-based alloy 825 tubes was carried out with different cold drawing deformations by using a draw-bench on a factory production line and subsequent annealing at various temperatures. The microstructure evolution of alloy 825 during thermal-mechanical processing (TMP) was characterized by means of the electron backscatter diffraction (EBSD) technique to study the TMP effects on the grain boundary network and the evolution of grain boundary character distributions during high temperature annealing. The results showed that the proportion of ∑ 3{sup n} coincidence site lattice (CSL) boundaries of alloy 825 tubes could be increased to > 75%more » by the TMP of 5% cold drawing and subsequent annealing at 1050 °C for 10 min. The microstructures of the partially recrystallized samples and the fully recrystallized samples suggested that the proportion of low ∑ CSL grain boundaries depended on the annealing time. The frequency of low ∑ CSL grain boundaries increases rapidly with increasing annealing time associating with the formation of large-size highly-twinned grains-cluster microstructure during recrystallization. However, upon further increasing annealing time, the frequency of low ∑ CSL grain boundaries decreased markedly during grain growth. So it is concluded that grain boundary engineering is achieved through recrystallization rather than grain growth. - Highlights: •The grain boundary engineering (GBE) is applicable to 825 tubes. •GBE is achieved through recrystallization rather than grain growth. •The low ∑ CSL grain boundaries in 825 tubes can be increased to > 75%.« less

Microstructure and mesh sensitivities of mesoscale surrogate driving force measures for transgranular fatigue cracks in polycrystals

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

Castelluccio, Gustavo M.; McDowell, David L.

The number of cycles required to form and grow microstructurally small fatigue cracks in metals exhibits substantial variability, particularly for low applied strain amplitudes. This variability is commonly attributed to the heterogeneity of cyclic plastic deformation within the microstructure, and presents a challenge to minimum life design of fatigue resistant components. Our paper analyzes sources of variability that contribute to the driving force of transgranular fatigue cracks within nucleant grains. We also employ crystal plasticity finite element simulations that explicitly render the polycrystalline microstructure and Fatigue Indicator Parameters (FIPs) averaged over different volume sizes and shapes relative to the anticipatedmore » fatigue damage process zone. Volume averaging is necessary to both achieve description of a finite fatigue damage process zone and to regularize mesh dependence in simulations. Furthermore, results from constant amplitude remote applied straining are characterized in terms of the extreme value distributions of volume averaged FIPs. Grain averaged FIP values effectively mitigate mesh sensitivity, but they smear out variability within grains. Furthermore, volume averaging over bands that encompass critical transgranular slip planes appear to present the most attractive approach to mitigate mesh sensitivity while preserving variability within grains.« less

Microstructure and mesh sensitivities of mesoscale surrogate driving force measures for transgranular fatigue cracks in polycrystals

DOE PAGES

Castelluccio, Gustavo M.; McDowell, David L.

2015-05-22

The number of cycles required to form and grow microstructurally small fatigue cracks in metals exhibits substantial variability, particularly for low applied strain amplitudes. This variability is commonly attributed to the heterogeneity of cyclic plastic deformation within the microstructure, and presents a challenge to minimum life design of fatigue resistant components. Our paper analyzes sources of variability that contribute to the driving force of transgranular fatigue cracks within nucleant grains. We also employ crystal plasticity finite element simulations that explicitly render the polycrystalline microstructure and Fatigue Indicator Parameters (FIPs) averaged over different volume sizes and shapes relative to the anticipatedmore » fatigue damage process zone. Volume averaging is necessary to both achieve description of a finite fatigue damage process zone and to regularize mesh dependence in simulations. Furthermore, results from constant amplitude remote applied straining are characterized in terms of the extreme value distributions of volume averaged FIPs. Grain averaged FIP values effectively mitigate mesh sensitivity, but they smear out variability within grains. Furthermore, volume averaging over bands that encompass critical transgranular slip planes appear to present the most attractive approach to mitigate mesh sensitivity while preserving variability within grains.« less

Effect of Microstructure on the Mechanical Properties of Extruded Magnesium and a Magnesium Alloy

NASA Astrophysics Data System (ADS)

McGhee, Paul

The main objective of this research was to investigate the relationship between the fatigue behavior and crystallographic texture evolution of magnesium (Mg) alloys with a range of microalloying element content processed under various extrusion conditions. Several Mg alloys were processed under a range of extrusion temperatures, extrusion ratios, and alloying content and tested under monotonic and cyclic fatigue loading conditions: fully-reversed condition tested at strain amplitudes of 0.15% - 1.00% in strain-control mode. After fatigue testing, Mg microstructural analysis was performed using SEM, TEM, optical microscopy, and X-ray diffraction techniques. Microstructural observations revealed significant grain refinement through a combination of zirconium (Zr) addition and hot-extrusion, producing fine equiaxed grain structure with grain sizes ranging between 1-5 microm. Texture analysis and partial compression testing results showed that the initial texture of the extruded alloy gradually evolved upon compressive loading along the c-axes inducing extension twinning creating a strong basal texture along the extrusion direction. Full tensile and compression testing at room temperature showed that the combination of hot extrusion and Zr addition can further refine the grains of the Mg alloys microstructure and enhance the texture while simultaneously enhancing the mechanical properties.

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.

Effect of heat treatment On Microstructure of steel AISI 01 Tools

NASA Astrophysics Data System (ADS)

Dyanasari Sebayang, Melya; Yudo, Sesmaro Max; Silitonga, Charlie

2018-03-01

This study discusses the influence of quenching, normalizing, and annealing to changes in hardness, tensile, and microstructure of materials tool steel AISI 01 after the material undergo heat treatment process. This heat treatment process includes an initial warming of 600° C and a 5-minute detention time, followed by heating to an austenisation temperature of 850°C. After that a different cooling process, including annealing process, normalizing and quenching oil SAE 40. Tests performed include tensile, hard, and microstructure with shooting using SEM (Scanning Electron Microscope). This is done to see the effect of different heat treatment and cooling process. The result of this research is difference of tensile test value, hard, and micro structure from influence of difference of each process. The quenching process obtains the highest tensile and hard values followed by the normalizing process, annealing, and the lowest is in the starting material, this is because the initial material does not undergo heat treatment process. The resulting microstructure is pearlit and cementite, the difference seen from the shape and size of the grains. The larger the grain size, the greater the hardness.

Metallurgical characterization of melt-spun ribbons of U-5.4 wt%Nb alloy

NASA Astrophysics Data System (ADS)

Ma, Rong; Ren, Zhiyong; Tang, Qingfu; Chen, Dong; Liu, Tingyi; Su, Bin; Wang, Zhenhong; Luo, Chao

2018-06-01

The microstructures and micro-mechanical properties of the melt-spun ribbons of U-5.4 wt%Nb alloy were characterized using optical microscopy, scanning electron microscopy, X-ray diffraction and nanoindentation. Observed variations in microstructures and properties are related to the changes in ribbon thicknesses and cooling rates. The microstructures of the melt-spun ribbon consist of fine-scale columnar grains (∼1 μm) adjacent to the chill surface and coarse cellular grains in the remainder of the ribbon. In addition, the formation of inclusions in the ribbon is suppressed kinetically due to the high cooling rate during melt spinning. Compared with the water-quenched specimen prepared by traditional gravity casting and solution heat treatment, the elastic modulus values of the U-5.4 wt%Nb alloy were examined to vary with grain size and exhibited diverse energy dissipation capacities.

Experimental and Numerical Analysis of Microstructures and Stress States of Shot-Peened GH4169 Superalloys

NASA Astrophysics Data System (ADS)

Hu, Dianyin; Gao, Ye; Meng, Fanchao; Song, Jun; Wang, Rongqiao

2018-04-01

Combining experiments and finite element analysis (FEA), a systematic study was performed to analyze the microstructural evolution and stress states of shot-peened GH4169 superalloy over a variety of peening intensities and coverages. A dislocation density evolution model was integrated into the representative volume FEA model to quantitatively predict microstructural evolution in the surface layers and compared with experimental results. It was found that surface roughness and through-depth residual stress profile are more sensitive to shot-peening intensity compared to coverage due to the high kinetic energy involved. Moreover, a surface nanocrystallization layer was discovered in the top surface region of GH4169 for all shot-peening conditions. However, the grain refinement was more intensified under high shot-peening coverage, under which enough time was permitted for grain refinement. The grain size gradient predicted by the numerical framework showed good agreement with experimental observations.

Microstructure evaluation for Dy-free Nd-Fe-B sintered magnets with high coercivity

NASA Astrophysics Data System (ADS)

Goto, R.; Matsuura, M.; Sugimoto, S.; Tezuka, N.; Une, Y.; Sagawa, M.

2012-04-01

Nd-Fe-B sintered magnets are used for motors of hybrid or electric vehicles due to their high energy products. Dy is added to Nd-Fe-B sintered magnets to work in a high temperature environment. Although the addition of Dy decreases the magnetization of Nd-Fe-B magnets, it increases coercivity; a decrease in the amount of Dy is strongly required. Recently, Nd-Fe-B sintered magnets with a grain size of 1 μm achieved high coercivity of ˜20 kOe without the addition of Dy or other heavy rare earth elements. In this paper, the microstructure of their magnets was observed and compared to magnets with a grain size of ˜3 μm. The coercivity of magnets consisting of larger particles was 17 kOe. Microstructures were observed by the scanning electron microscope and the shapes of grains and the distribution of the Nd-rich phase were evaluated. The observation was promoted in two directions. One direction is the plane perpendicular to the magnetically aligned direction (c plane side) and the other is the side parallel to the magnetically aligned direction (c axis side). For magnets consisting of smaller particles, the shapes of grains are isotropic for the c plane side and elongated for the c axis side. The angle of minor axis prefers to be parallel to magnetically aligned direction. The distribution of the Nd-rich phase for magnets was also evaluated for both magnets. The distribution of the Nd-rich phase at triple junctions for the magnets with smaller particles becomes homogeneous compared to that for magnets with larger particles. It is considered that Dy-free magnets with high coercivity were realized by the achievement of homogeneous distribution of Nd-rich phase besides decreasing grain size.

Improved wear resistance by phase transformation of surface nanocrystalline 1090 steel prepared by sandblasting technique

NASA Astrophysics Data System (ADS)

Peng, Rong; Fu, Licai; Zhou, Lingping

2016-12-01

A surface nanocrystalline 1090 steel has been fabricated by using sandblasting technique. The surface average grain size was about 78 nm. The high strain rate and strain in sandblasting were main reasons for surface nanocrystallization. The wear resistance of 1090 steel was considerably enhanced as grain size decreased. The microstructure and hardness of contact zones before and after wear tests have been examined by XRD, SEM and TEM. Except the higher hardness, the results demonstrated that parts of ferrite transferred to cementite and martensite. It was additional beneficial for improving the wear resistance of 1090 steel as the grain size decreased.

Effect of Cold Forging on Microstructure and MechanicalProperties of Al/SiC Composites

NASA Astrophysics Data System (ADS)

Hanamantraygouda, M. B.; Shivakumar, B. P., Dr; Siddappa, P. N.; Sampathkumar, L.; Prashanth, L.

2018-02-01

The objective of this work was to investigate the effect of cold forging on mechanical properties and microstructural study of Al MMCs, at different wt% of SiC and forging cycle. The Al-SiC composite material was fabricated by stir casting method at different weight percentage of SiC such as 2.5, 5, 7.5 and 10%. Further, the deformation characteristics during open-die forging of Al-SiC composite at cold conditions was investigated. Cast and forged composite material was subjected to hardness test, tensile test and impact test. The grain size, microstructure behaviour was investigated using optical microscope. The results show that hardness and strength of Al-SiC composite increases and ductility decreases as compared to Al alloy in both as-cast and forged conditions. Optical microscope images showed that the distribution of SiC in Al matrix was more homogeneous in a forged composite as compared to cast one and reduction of porosity was found. Further, it showed that due to forging cycle the grain size was reduced by 30% to 35% from initial size.

The effect of carbon on the microstructures, mechanical properties, and deformation mechanisms of thermo-mechanically treated Fe 40.4Ni 11.3Mn 34.8Al 7.5Cr 6 high entropy alloys

DOE PAGES

Wang, Zhangwei; Baker, Ian; Guo, Wei; ...

2017-03-01

We investigated the effects of cold rolling followed by annealing on the mechanical properties and dislocation substructure evolution of undoped and 1.1 at. % carbon-doped Fe 40.4Ni 11.3Mn 34.8Al 7.5Cr 6 high entropy alloys (HEAs). X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and atom probe tomography (APT) were employed to characterize the microstructures. The as-cast HEAs were coarse-grained and single phase f.c.c., whereas the thermo-mechanical treatment caused recrystallization (to fine grain sizes) and precipitation (a B2 phase for the undoped HEA; and a B2 phase, and M 23C 6 and M 7C 3 carbides for the C-dopedmore » HEA). Carbon, which was found to have segregated to the grain boundaries using APT, retarded recrystallization. The reduction in grain size resulted in a sharp increase in strength, while the precipitation, which produced only a small increase in strength, probably accounted for the small decrease in ductility for both undoped and C-doped HEAs. For both undoped and C-doped HEAs, the smaller grain-sized material initially exhibited higher strain hardening than the coarse-grained material but showed a much lower strain hardening at large tensile strains. Wavy slip in the undoped HEAs and planar slip in C-doped HEAs were found at the early stages of deformation irrespective of grain size. At higher strains, dislocation cell structures formed in the 19 μm grain-sized undoped HEA, while microbands formed in the 23 μm grain-sized C-doped HEA. Conversely, localized dislocation clusters were found in both HEAs at the finest grain sizes (5 μm). The inhibition of grain subdivision by the grain boundaries and precipitates lead to the transformation from regular dislocation configurations consisting of dislocation-cells and microbands to irregular dislocation configurations consisting of localized dislocation clusters, which further account for the decrease in ductility. Our investigation of the formation mechanism and strain hardening of dislocation cells and microbands could benefit future structural material design.« less

Fabrication, microstructure, properties and deformation mechanisms of a nanocrystalline aluminum-iron-chromium-titanium alloy by mechanical alloying

NASA Astrophysics Data System (ADS)

Luo, Hong

A multi-phase nanocrystalline Al93Fe3Cr2Ti 2 alloy containing 30 vol.% intermetallic particles was prepared via mechanical alloying starting from elemental powders, followed by hot extrusion. The grain size of 6-45 nm can be achieved after 30-hours of milling. Thermal stability of nanostructured Al93Fe3Ti2Cr 2 alloys was investigated using a variety of analytical techniques including modulated differential scanning calorimetry, X-ray diffraction, scanning electron microscopy, transmission electron microscopy. The MA-processed Al93Fe 3Ti2Cr2 alloy in the as-milled condition was composed of an Al-based supersaturated solid solution with high internal strains. Release of internal strains, intermetallic precipitation and grain growth occurred upon heating of the MA-processed Al alloy. Nevertheless, grain growth in the MA-processed Al alloy was very limited and fcc-Al grains with sizes in the range of 20 nm were still present in the alloys after exposure to 450°C (0.77 Tm). Systematic compressive tests and modulus measurements were performed as a function of temperature and strain rate to investigate the deformation behavior and mechanisms of the nc Al-Fe-Cr-Ti alloys. High strengths and moduli at both ambient and elevated temperatures have been demonstrated. The ductility of the nc Al93Fe3Cr2Ti2 alloy depends strongly on whether the oxide film at the prior powder particle boundary has been broken down or not. The MA-processed Al93Fe3Cr 2Ti2 alloy is brittle when the oxide film is continuous at PPB, and is ductile when the oxide film is broken down into discontinuous particles during extrusion. It is argued that the compressive strength at ambient temperature is controlled by propagation of dislocations into nc fcc-Al grains, whereas the compressive strength at elevated temperature is determined by dislocation propagation as well as dynamic recovery. Since the stress for dislocation propagation into nc fcc-Al grains increases with decreasing the grain size, the smaller the grain size, the higher the compressive strength. This new microstructural design approach could present opportunities for exploiting nc materials in structural applications at both ambient and elevated temperatures. The nanocrystalline Al-Fe-Cr-Ti alloy exhibited significant difference in deformation behavior between tension and compression at 25, 200 and 300°C. However, the strengths obtained in tension and compression were similar at 400°C. Systematic microstructure examinations and deformation mechanism analyses indicate that the asymmetry of this nc Al93Fe3Cr 2Ti2 alloy is related to its dislocation mediated plastic deformation mechanism, its nanoscale grain microstructure, and premature brittle failure in tension tests.

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.

Effect of the addition of B{sub 2}O{sub 3} and BaO-B{sub 2}O{sub 3}-SiO{sub 2} glasses on the microstructure and dielectric properties of giant dielectric constant material CaCu{sub 3}Ti{sub 4}O{sub 12}

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

Shri Prakash, B.; Varma, K.B.R.

2007-06-15

The effect of the addition of glassy phases on the microstructure and dielectric properties of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) ceramics was investigated. Both single-component (B{sub 2}O{sub 3}) and multi-component (30 wt% BaO-60 wt% B{sub 2}O{sub 3}-10 wt% SiO{sub 2} (BBS)) glass systems were chosen to study their effect on the density, microstructure and dielectric properties of CCTO. Addition of an optimum amount of B{sub 2}O{sub 3} glass facilitated grain growth and an increase in dielectric constant. However, further increase in the B{sub 2}O{sub 3} content resulted in its segregation at the grain boundaries associated with a reduction in themore » grain size. In contrast, BBS glass addition resulted in well-faceted grains and increase in the dielectric constant and decrease in the dielectric loss. An internal barrier layer capacitance (IBLC) model was invoked to correlate the dielectric constant with the grain size in these samples. - Graphical abstract: Scanning electron micrograph of 30 wt% BaO-60 wt% B{sub 2}O{sub 3}-10 wt% SiO{sub 2} (BBS) glass-added CaCu{sub 3}Ti{sub 4}O{sub 12} ceramic on sintering.« less

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.

The effect of SiO2, Pt, and Pt /Au templates on the microstructure and permittivity of BaxSr1-xTiO3 films

NASA Astrophysics Data System (ADS)

Rundqvist, Pär; Liljenfors, Tomas; Vorobiev, Andrei; Olsson, Eva; Gevorgian, Spartak

2006-12-01

Ba0.25Sr0.75TiO3 (BSTO) and SrTiO3 (STO) ferroelectric thin films were grown on templates of SiO2/Si, Pt /TiO2/SiO2/Si, and Pt /Au/Pt/TiO2/SiO2/Si using pulsed laser deposition. The microstructure and surface morphology of the multilayer stacks were studied using x-ray diffraction, atomic force microscopy, and transmission electron microscopy. The microstructural analysis shows that the ferroelectric films are polycrystalline textured with a columnar structure where the grain size is 50-100nm. The BSTO films deposited at 800°C on an amorphous SiO2/Si template reveal a textured structure with a dominant (110) orientation, which is explained by a dominant growth of BSTO (110) grains due to the lower surface energy of the (110) phase. The STO and BSTO films deposited at 650°C on the Pt /TiO2/SiO2/Si and Pt /Au/Pt/TiO2/SiO2/Si templates, respectively, reveal a structure with a dominant (111) orientation, which is explained by the dominant growth of BSTO (STO) (111) grains imposed by the underlying Pt (111) texture. In all cases the ferroelectric films are subject to compressive in-plane strain which is different for different grain orientations. Strain modified permittivities of ferroelectric films grown on different templates are calculated from first principles for different orientations and compared with measured results. The correlations between grain orientations, grain sizes, grain boundaries, strain, and dielectric permittivity of ferroelectric films on different templates are discussed.

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.

Contributions of Rare Earth Element (La,Ce) Addition to the Impact Toughness of Low Carbon Cast Niobium Microalloyed Steels

NASA Astrophysics Data System (ADS)

Torkamani, Hadi; Raygan, Shahram; Garcia Mateo, Carlos; Rassizadehghani, Jafar; Palizdar, Yahya; San-Martin, David

2018-07-01

In this research Rare Earth elements (RE), La and Ce (200 ppm), were added to a low carbon cast microalloyed steel to disclose their influence on the microstructure and impact toughness. It is suggested that RE are able to change the interaction between the inclusions and matrix during the solidification process (comprising peritectic transformation), which could affect the microstructural features and consequently the impact property; compared to the base steel a clear evolution was observed in nature and morphology of the inclusions present in the RE-added steel i.e. (1) they changed from MnS-based to (RE,Al)(S,O) and RE(S)-based; (2) they obtained an aspect ratio closer to 1 with a lower area fraction as well as a smaller average size. Besides, the microstructural examination of the matrix phases showed that a bimodal type of ferrite grain size distribution exists in both base and RE-added steels, while the mean ferrite grain size was reduced from 12 to 7 μm and the bimodality was redressed in the RE-added steel. It was found that pearlite nodule size decreases from 9 to 6 μm in the RE-added steel; however, microalloying with RE caused only a slight decrease in pearlite volume fraction. After detailed fractography analyses, it was found that, compared to the based steel, the significant enhancement of the impact toughness in RE-added steel (from 63 to 100 J) can be mainly attributed to the differences observed in the nature of the inclusions, the ferrite grain size distribution, and the pearlite nodule size. The presence of carbides (cementite) at ferrite grain boundaries and probable change in distribution of Nb-nanoprecipitation (promoted by RE addition) can be considered as other reasons affecting the impact toughness of steels under investigation.

Contributions of Rare Earth Element (La,Ce) Addition to the Impact Toughness of Low Carbon Cast Niobium Microalloyed Steels

NASA Astrophysics Data System (ADS)

Torkamani, Hadi; Raygan, Shahram; Garcia Mateo, Carlos; Rassizadehghani, Jafar; Palizdar, Yahya; San-Martin, David

2018-03-01

In this research Rare Earth elements (RE), La and Ce (200 ppm), were added to a low carbon cast microalloyed steel to disclose their influence on the microstructure and impact toughness. It is suggested that RE are able to change the interaction between the inclusions and matrix during the solidification process (comprising peritectic transformation), which could affect the microstructural features and consequently the impact property; compared to the base steel a clear evolution was observed in nature and morphology of the inclusions present in the RE-added steel i.e. (1) they changed from MnS-based to (RE,Al)(S,O) and RE(S)-based; (2) they obtained an aspect ratio closer to 1 with a lower area fraction as well as a smaller average size. Besides, the microstructural examination of the matrix phases showed that a bimodal type of ferrite grain size distribution exists in both base and RE-added steels, while the mean ferrite grain size was reduced from 12 to 7 μm and the bimodality was redressed in the RE-added steel. It was found that pearlite nodule size decreases from 9 to 6 μm in the RE-added steel; however, microalloying with RE caused only a slight decrease in pearlite volume fraction. After detailed fractography analyses, it was found that, compared to the based steel, the significant enhancement of the impact toughness in RE-added steel (from 63 to 100 J) can be mainly attributed to the differences observed in the nature of the inclusions, the ferrite grain size distribution, and the pearlite nodule size. The presence of carbides (cementite) at ferrite grain boundaries and probable change in distribution of Nb-nanoprecipitation (promoted by RE addition) can be considered as other reasons affecting the impact toughness of steels under investigation.

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.

Microstructures and Properties of W-Ti Alloys Prepared Under Different Cooling Conditions

NASA Astrophysics Data System (ADS)

Dai, Weili; Liang, Shuhua; Yang, Qing; Zou, Juntao; Zhuo, Longchao

2016-07-01

W-(10 to 15) wt.% Ti alloys were sintered at 1400 or 1500 °C and cooled under different cooling conditions. The microstructures and properties of W-Ti alloys were affected by the cooling conditions. XRD, SEM, EBSD, and TEM were carried out to investigate the effects of cooling conditions and sintering temperature on the microstructures of W-Ti alloys. The nanohardness and elastic modulus of the alloys were also investigated. The results showed that when the temperature was 1500 °C, the content of Ti-rich phase in W-(10 to 15) wt.% Ti alloys decreased obviously with the increase of cooling rate (the average cooling rate of furnace cooling, air cooling and water cooling was 0.2, 10, and 280 °C/s, respectively). For the W-10 wt.% Ti alloy, the content decreased from 20.5 to 9.7%, and the grain size decreased from 2.33 to 0.67 μm. When the temperature decreased to 1400 °C, the grain size was also decreased sharply with the increase of cooling rate, but there was a little change in the microstructure. Meanwhile, the grain sizes were smaller than those of the alloys sintered at 1500 °C. The nanohardness and elastic modulus increased with the increase of cooling rate, and the alloys sintered at different temperatures had different nanohardness and elastic modulus which depended on the cooling conditions. Sintering at a proper temperature and then cooling at a certain cooling condition was a useful method to fabricate alloy with less Ti-rich phase and high properties.

Influence of processing on the microstructure and mechanical properties of 14YWT

DOE PAGES

Hoelzer, David T.; Unocic, Kinga A.; Sokolov, Mikhail A.; ...

2015-12-15

In this study, the investigation of the mechanical alloying (MA) conditions for producing the advanced oxide dispersion strengthened (ODS) 14YWT ferritic alloy led to significant improvements in balancing the strength, ductility and fracture toughness properties while still maintaining the salient microstructural features consisting of ultra-fine grains and high concentration of Y-, Ti- and O-enriched nanoclusters. The implemented changes to the processing conditions included reducing the contamination of the powder during ball milling, applying a pre-extrusion annealing treatment on the ball milled powder and exploring different extrusion temperatures at 850 °C (SM170 heat), 1000 °C (SM185) and 1150 °C (SM200). Themore » microstructural studies of the three 14YWT heats showed similarities in the dispersion of nanoclusters and sub-micron size grains, indicating the microstructure was insensitive to the different extrusion conditions. Compared to past 14YWT heats, the three new heats showed lower strength, but higher ductility levels between 25 and 800 °C and significantly higher fracture toughness values between 25 °C and 700 °C. The lower contamination levels of O, C and N achieved with improved ball milling conditions plus the slightly larger grain size were identified as important factors for improving the balance in mechanical properties of the three heats of 14YWT.« less

Tailoring microstructure of Mg–Zn–Y alloys with quasicrystal and related phases for high mechanical strength

PubMed Central

Singh, Alok

2014-01-01

The occurrence of a stable icosahedral (i-) phase, which is quasicrystalline with an icosahedral (fivefold) symmetry, on the equilibrium phase diagram of Mg–Zn–RE (RE = Y, Gd, Tb, Dy, Ho or Er) alloys opened up an interesting possibility of developing a new series of magnesium alloys for structural applications. Alloys based on the i-phase have been studied for the past 14 years. Ultra-high strengths combined with good ductility have been shown. Here we show two strategies for tailoring microstructures for very high strengths in Mg–Zn–Y alloys. One of them involves strengthening by a fine distribution of rod-like precipitates, where the matrix grain size is not critical. The alloy is solutionized at a high temperature of 480 °C to dissolve a large part of the i-phase, followed by a high temperature extrusion (∼430 °C) and a low temperature ageing to reprecipitate phases with fine size distribution. At first, phase transformations involved in this procedure are described. The closeness of the structure of the precipitates to the i-phase is brought out. By this procedure, tensile yield strengths of over 370 MPa are obtained in grain sizes of 20 μm. In another strategy, the alloys are chill cast and then extruded at low temperatures of about 250 °C. Ultra-fine grains are produced by enhanced recrystallization due to presence of the i-phase. At the same time nano-sized precipitates are precipitated dynamically during extrusion from the supersaturated matrix. Ultra-high tensile strengths of up to 400 MPa are obtained in combination with ductility of 12 to 16%. Analysis of the microstructure shows that strengthening by the i-phase occurs by enhanced recrystallization during extrusion. It produces ultra-fine grain sizes to give very high strengths, and moderate texture for good ductility. Fine distribution of the i-phase and precipitates contribute to strengthening and provide microstructre stability. Ultra-high strength over a very wide range of grain sizes is thus demonstrated, by utilizing different strengthening effects. PMID:27877701

Microstructural and mechanical responses to various rolling speeds determined in multi-pass break-down rolling of AZ31B alloy

NASA Astrophysics Data System (ADS)

Jia, Weitao; Tang, Yan; Ning, Fangkun; Le, Qichi; Cui, Jianzhong

2018-04-01

Different rolling operations of as-cast AZ31B alloy were performed under different rolling speed (18 ∼ 72 m min‑1) and rolling pass conditions at 400 °C. Microstructural studies, tensile testing and formability evaluation relevant to each rolling operation were investigated. For 1-pass rolling, coarse average grain size (CAGS) region gradually approached the center layer as the rolling speed increased. Moreover, twins, shear bands and coarse-grain structures were the dominant components in the microstructure of plates rolled at 18, 48 and 72 m min‑1, respectively, indicating the severe deformation inhomogeneity under the high reduction per pass condition. For 2-pass rolling and 4-pass rolling, dynamic recrystallization was observed to be well and CAGS region has substantially disappeared, indicating the significant improvement in deformation uniformity and further the grain homogenization under the conditions. Microstructure uniformity degree of 2-pass rolled plates did not vary much as the rolling speed varied. On this basis, shear band distribution dominated the deformation behavior during the uniaxial tension of the 2-pass rolled plates. However, microstructure uniformity accompanied by twin distribution played a leading role in stretching the 4-pass rolled plates.

Biotite Comminution in Phyllosilicate Rich Mylonites: Microstructural and Nanostructural Observations

NASA Astrophysics Data System (ADS)

Aslin, J.; Mariani, E.; Dawson, K.

2017-12-01

Micas are one of the most important mineral groups with regard to the strength and rheology of the Earth's crust. This is a result of their distinct weakness relative to other silicate phases coupled with their generally high abundance at mid-crustal conditions. Despite this, relatively little is known regarding the mechanisms of viscous deformation in micas. The samples used in this study were collected from the Cossato-Mergozzo-Brissago (C-M-B) line, an amphibolite facies mylonitic shear zone in Northern Italy. The granitoid and metasedimentary protoliths of this 100 -150 m wide shear zone ensure a high but variable phyllosilicate content within predominantly quartzofelspathic lithologies. Initial microstructural analysis using optical and scanning electron microscopy (SEM) reveals a significant change in biotite deformation behaviour with increasing strain. At low strains kinking and basal glide dominate, however at higher strain biotite undergoes a dramatic grain size reduction which is at first concentrated along grain edges and kink band boundaries but later involves the entire grain. In the highest strain samples examined, biotite only survives as a component of a very fine grained matrix. In contrast, muscovite, also present in these rocks, remains coarse, forming kinked and bent mica fish even to high strains. The comminution of biotite is of critical importance to the microstructural evolution of these mylonites as it facilitates the development of an interconnected network of fine and potentially very weak grains. However, the mechanism responsible is not clear. We use transmission electron microscopy (TEM) to observe and characterise the intracrystalline structure of the biotite in these samples both prior to and after this grain size reduction has taken place. A better understanding of the nano-scale microstructures produced by natural deformation in micas will aid in determining the mechanisms which control the way these important crustal minerals accommodate strain.

Microstructure Evolution and Protrusion of Electroplated Cu-Filled Through-Silicon Vias Subjected to Thermal Cyclic Loading

NASA Astrophysics Data System (ADS)

Chen, Si; An, Tong; Qin, Fei; Chen, Pei

2017-10-01

Through-silicon vias (TSVs) have become an important technology for three-dimensional integrated circuit (3D IC) packaging. Protrusion of electroplated Cu-filled vias is a critical reliability issue for TSV technology. In this work, thermal cycling tests were carried out to identify how the microstructure affects protrusion during thermal cycling. Cu protrusion occurs when the loading temperature is higher than 149°C. During the first five thermal cycles, the grain size of Cu plays a dominant role in the protrusion behavior. Larger Cu grain size before thermal cycling results in greater Cu protrusion. With increasing thermal cycle number, the effect of the Cu grain size reduces and the microstrain begins to dominate the Cu protrusion behavior. Higher magnitude of microstrain within Cu results in greater protrusion increment during subsequent thermal cycles. When the thermal cycle number reaches 25, the protrusion rate of Cu slows down due to strain hardening. After 30 thermal cycles, the Cu protrusion stabilizes within the range of 1.92 μm to 2.09 μm.

Transformation-Induced, Geometrically Necessary, Dislocation-Based Flow Curve Modeling of Dual-Phase Steels: Effect of Grain Size

NASA Astrophysics Data System (ADS)

Ramazani, Ali; Mukherjee, Krishnendu; Prahl, Ulrich; Bleck, Wolfgang

2012-10-01

The flow behavior of dual-phase (DP) steels is modeled on the finite-element method (FEM) framework on the microscale, considering the effect of the microstructure through the representative volume element (RVE) approach. Two-dimensional RVEs were created from microstructures of experimentally obtained DP steels with various ferrite grain sizes. The flow behavior of single phases was modeled through the dislocation-based work-hardening approach. The volume change during austenite-to-martensite transformation was modeled, and the resultant prestrained areas in the ferrite were considered to be the storage place of transformation-induced, geometrically necessary dislocations (GNDs). The flow curves of DP steels with varying ferrite grain sizes, but constant martensite fractions, were obtained from the literature. The flow curves of simulations that take into account the GND are in better agreement with those of experimental flow curves compared with those of predictions without consideration of the GND. The experimental results obeyed the Hall-Petch relationship between yield stress and flow stress and the simulations predicted this as well.

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.

Influence of the microstructure on the physicomechanical properties of the aluminum alloy Al-Mg-Si nanostructured under severe plastic deformation

NASA Astrophysics Data System (ADS)

Mavlyutov, A. M.; Kasatkin, I. A.; Murashkin, M. Yu.; Valiev, R. Z.; Orlova, T. S.

2015-10-01

The microstructural features, strength, and electrical conductivity of the electrotechnical aluminum alloy 6201 of the Al-Mg-Si system was investigated. The alloy was nanostructured using severe plastic deformation by high pressure torsion at different temperatures and in different deformation regimes. As a result, the samples had an ultrafine-grain structure with nanoinclusions of secondary phases, which provided an excellent combination of high strength (conventional yield strength σ0.2 = 325-410 MPa) and electrical conductivity (55-52% IACS). The contributions from different mechanisms to the strengthening were analyzed. It was experimentally found that the introduction of an additional dislocation density (an increase from 2 × 1013 to 5 × 1013 m-2) with the same basic parameters of the ultrafine-grain structure (grain size, size and distribution of particles of secondary strengthening phases) leads to an increase in the strength of the alloy by ~15%, while the electrical conductivity of the material changes insignificantly. The contribution from grain boundaries to the electrical resistivity of the alloy with an ultrafine-grain structure upon the change in their state, most likely, due to a change in the degree of nonequilibrium was estimated.

Statistical electric field and switching time distributions in PZT 1Nb2Sr ceramics: Crystal- and microstructure effects

NASA Astrophysics Data System (ADS)

Zhukov, Sergey; Kungl, Hans; Genenko, Yuri A.; von Seggern, Heinz

2014-01-01

Dispersive polarization response of ferroelectric PZT ceramics is analyzed assuming the inhomogeneous field mechanism of polarization switching. In terms of this model, the local polarization switching proceeds according to the Kolmogorov-Avrami-Ishibashi scenario with the switching time determined by the local electric field. As a result, the total polarization reversal is dominated by the statistical distribution of the local field magnitudes. Microscopic parameters of this model (the high-field switching time and the activation field) as well as the statistical field and consequent switching time distributions due to disorder at a mesoscopic scale can be directly determined from a set of experiments measuring the time dependence of the total polarization switching, when applying electric fields of different magnitudes. PZT 1Nb2Sr ceramics with Zr/Ti ratios 51.5/48.5, 52.25/47.75, and 60/40 with four different grain sizes each were analyzed following this approach. Pronounced differences of field and switching time distributions were found depending on the Zr/Ti ratios. Varying grain size also affects polarization reversal parameters, but in another way. The field distributions remain almost constant with grain size whereas switching times and activation field tend to decrease with increasing grain size. The quantitative changes of the latter parameters with grain size are very different depending on composition. The origin of the effects on the field and switching time distributions are related to differences in structural and microstructural characteristics of the materials and are discussed with respect to the hysteresis loops observed under bipolar electrical cycling.

Microstructural control of FeCrAl alloys using Mo and Nb additions

DOE PAGES

Sun, Zhiqian; Bei, Hongbin; Yamamoto, Yukinori

2017-08-14

The effects of Mo and Nb additions on the microstructure and mechanical properties of two FeCrAl alloys were studied in this paper. Fine and uniform recrystallized grain structures (~ 20–30 μm) were achieved in both alloys through suitable annealing after warm-rolling. The formation of Fe 2Nb-type Laves phase precipitates in the Nb-containing FeCrAl alloy effectively stabilized the deformed and recrystallized microstructures. The Mo-containing FeCrAl alloy exhibited strong γ texture fiber after annealing at 650–900 °C, whereas the annealed Nb-containing FeCrAl alloy had much weaker texture. Finally, both strength and ductility decreased as the grain size increased in both alloys.

Modeling ductile metals under large strain, pressure and high strain rate incorporating damage and microstructure evolution

NASA Astrophysics Data System (ADS)

Iannitti, Gianluca; Bonora, Nicola; Ruggiero, Andrew; Dichiaro, Simone

2012-03-01

In this work, a constitutive modeling that couples plasticity, grain size evolution (due to plastic deformation and dynamic recrystallization) and ductile damage has been developed. The effect of grain size on the material yield stress (Hall-Petch) and on the melting temperature has been considered. The model has been used to investigate computationally the behavior of high purity copper in dynamic tensile extrusion test (DTE). An extensive numerical simulation work, using implicit finite element code with direct integration, has been performed and the results have been compared with available experimental data. The major finding is that the proposed model is capable to predict most of the observed features such as the increase of material ductility with the decreasing average grain size, the overall number and size of fragments and the average grain size distribution in the fragment trapped into the dime.

Modeling ductile metals under large strain, pressure and high strain rates incorporating damage and microstructure evolution

NASA Astrophysics Data System (ADS)

Iannitti, Gianluca; Bonora, Nicola; Ruggiero, Andrew; Dichiaro, Simone

2011-06-01

In this work, a constitutive modeling that couples plasticity, grain size evolution (due to plastic deformation and dynamic recrystallization) and ductile damage has been developed. The effect of grain size on the material yield stress (Hall-Petch) and on the melting temperature has been considered. The model has been used to investigate computationally the behaviour of high purity copper in dynamic tensile extrusion test (DTE). An extensive numerical simulation work, using implicit finite element code with direct integration, has been performed and the results have been compared with available experimental data. The major finding is that the proposed model is capable to predict most of the observed features such as the increase of material ductility with the decreasing average grain size, the overall number and size of fragments and the average grain size distribution in the fragment trapped into the dime.

PTCR characteristics and microstructure of porous (Ba,Sr)TiO3 ceramics prepared by spark plasma sintering

NASA Astrophysics Data System (ADS)

Lee, Ki-Ju; Tang, Dongxu; Park, K.; Cho, Won-Seung

2010-02-01

Porous Y-doped (Ba,Sr)TiO3 ceramics were prepared by the spark plasma sintering of (Ba,Sr)TiO3 powders with different amounts of carbon black, and by subsequently burning out the carbon black acting as a pore precursor. The microstructure, PTCR and gas-sensing characteristics for porous Y-doped (Ba,Sr)TiO3 ceramics were investigated. Spark plasma sintered (Ba,Sr)TiO3 ceramics revealed a very fine microstructure containing submicron-sized grains with a cubic phase and revealed an increased porosity after the carbon black was burned out. As a result of reoxidation treatment, the grain size of the (Ba,Sr)TiO3 ceramics increased to a few μm and the cubic phase transformed into a tetragonal phase. The phase transformation of (Ba,Sr)TiO3 ceramics was affected by grain size. The PTCR jump in the (Ba,Sr)TiO3 ceramics prepared by adding 40 vol.% carbon black showed an excellent value of 4.72 × 106, which was ten times higher than the PTCR jump in (Ba,Sr)TiO3 ceramics. The electrical resistivity of the porous (Ba,Sr)TiO3 ceramics was recovered as the atmosphere changed from a reducing gas (N2) to an oxidizing gas (O2) under consecutive heating and cooling cycles.

Influence of ECAP process on mechanical and corrosion properties of pure Mg and ZK60 magnesium alloy for biodegradable stent applications

PubMed Central

Mostaed, Ehsan; Vedani, Maurizio; Hashempour, Mazdak; Bestetti, Massimiliano

2014-01-01

Equal channel angular pressing (ECAP) was performed on ZK60 alloy and pure Mg in the temperature range 150–250 °C. A significant grain refinement was detected after ECAP, leading to an ultrafine grain size (UFG) and enhanced formability during extrusion process. Comparing to conventional coarse grained samples, fracture elongation of pure Mg and ZK60 alloy were significantly improved by 130% and 100%, respectively, while the tensile strength remained at high level. Extrusion was performed on ECAP processed billets to produce small tubes (with outer/inner diameter of 4/2.5 mm) as precursors for biodegradable stents. Studies on extruded tubes revealed that even after extrusion the microstructure and microhardness of the UFG ZK60 alloy were almost stable. Furthermore, pure Mg tubes showed an additional improvement in terms of grain refining and mechanical properties after extrusion. Electrochemical analyses and microstructural assessments after corrosion tests demonstrated two major influential factors in corrosion behavior of the investigated materials. The presence of Zn and Zr as alloying elements simultaneously increases the nobility by formation of a protective film and increase the local corrosion damage by amplifying the pitting development. ECAP treatment decreases the size of the second phase particles thus improving microstructure homogeneity, thereby decreasing the localized corrosion effects. PMID:25482411

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.

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

Domenichini, P.; Condó, A.M.; Centro Atómico Bariloche, Comisión Nacional de Energía Atómica, Av. Bustillo 9500, 8400 San Carlos de Bariloche

We report the influence of the microstructure on the martensitic transformation in polycrystalline Cu−Zn−Al thin films with 18R structure. The films are grown in two steps. First, Cu−Al thin films are obtained by DC sputtering. Second, the Zn is introduced in the Cu−Al thin films by the annealing them together with a bulk Cu−Zn−Al reference. The crystalline structure of the films was analyzed by X-ray diffraction and transmission electron microscopy. The martensitic transformation temperature was measured by electrical transport using conventional four probe geometry. It was observed that temperatures above 973 K are necessary for zincification of the samples tomore » occur. The resulting martensitic transformation and its hysteresis (barrier for the transformation) depend on the grain size, topology and films thickness. - Highlights: • Polycrystalline Cu−Al−Zn thin films with nanometric grain size are sintered. • Influence of thermal annealing process on the microstructure is analyzed. • Martensitic transformation of Cu−Al−Zn thin films is strongly affected by the microstructure.« less

Surface Roughening Behavior of 6063 Aluminum Alloy during Bulging by Spun Tubes

PubMed Central

Cai, Yang; Wang, Xiaosong; Yuan, Shijian

2017-01-01

Severe surface roughening during the hydroforming of aluminum alloy parts can produce surface defects that severely restrict their application in the automobile and aerospace industry. To understand the relation between strain, grain size and surface roughness under biaxial stress conditions, hydro-bulging tests of aluminum alloy tubes were carried out, and the tubes with different grain sizes were prepared by a spinning and annealing process. The surface roughness was measured by a laser scanning confocal microscope to evaluate the surface roughening macroscopical behavior, and the corresponding microstructures were observed using electron back-scattered diffraction (EBSD) to reveal the roughening microscopic behavior. The results obtained show that the surface roughness increased with both strain and grain size under biaxial stress. No surface defects were observed on the surface when the grain size was less than 105 μm if the strain was less than 18%, or when the grain size was between 130 and 175 μm if the strain was less than 15.88% and 7.15%, respectively. The surface roughening microscopic behavior was identified as an inhomogeneous grain size distribution, which became more pronounced with increasing grain size and resulted in greater local deformation. Concentrated grain orientation also results in severe inhomogeneous deformation during plastics deformation, and serious surface roughening. PMID:28772658

Microstructures and mechanical behavior of magnesium processed by ECAP at ice-water temperature

NASA Astrophysics Data System (ADS)

Zuo, Dai; Li, Taotao; Liang, Wei; Wen, Xiyu; Yang, Fuqian

2018-05-01

Magnesium of high purity is processed by equal channel angular pressing (ECAP) up to eight passes at the ice-water temperature, in which a core–shell-like structure is used. The core–shell-like structure consists of pure iron (Fe) of 1.5 mm in thickness as the shell and magnesium (Mg) as the core. The microstructure, texture and mechanical behavior of the ECAP-processed Mg are studied. The ECAP processing leads to the formation of fine and equiaxed grains of ~1.1 µm. The basal planes initially parallel to the extrusion direction evolve to slanted basal planes with the tilting angle in a range of 25°–45° to the extrusion direction. Increasing the number of the extrusion passes leads to the decreasing of twins and dislocation density in grains, while individual grains after eight passes still have high dislocation density. The large decreases of twins and the dislocation density make dynamic recrystallization (DRX) difficult, resulting in the decrease of the degree of DRX. Tension test reveals that the mechanical behavior of the ECAP-processed Mg is dependent on grain refinement and textures. The yield strength of the ECAP-extruded Mg first increases with the decrease of the grain size, and then decreases with further decrease of the grain size.

Grain growth effects on magnetic properties of Ni0.6Zn0.4Fe2O4 material prepared using mechanically alloyed nanoparticles

NASA Astrophysics Data System (ADS)

Syazwan, M. M.; Hapishah, A. N.; Azis, R. S.; Abbas, Z.; Hamidon, M. N.

2018-06-01

The effect of grain growth via sintering temperature on some magnetic properties is reported in this research. Ni0.6Zn0.4Fe2O4 nanoparticles were mechanically alloyed for 6 h and the sintering process starting from 600 to 1200 °C with 25 °C increment with only one sample subjected to all sintering scheme. The resulting change in the material was observed after each sintering. Single phase has been formed at 600 °C and above and the intensity peaks increased with sintering temperature as well as crystallinity increment. The morphological studies showed grain size increment as the sintering temperature increased. Moreover, the density increased while the porosity decreased with increasing sintering temperature. The saturation induction, Bs increased with the increased of grain size. On the other hand, the coercivity-vs-grain size plot reveals the critical single-domain-to-multidomain grain size to be about ∼400 nm. The initial permeability, μi value was increased with grain size enhancement. The microstructural grain growth, as exposed for the first time by this research, is shown as a process of multiple activation energy barriers.

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.

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.

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.

Strain Localization on Different Scales and their Related Microstructures - Comparison of Microfabrics of Calcite Mylonites from Naxos (Greece) and Helvetic Nappes (Switzerland)

NASA Astrophysics Data System (ADS)

Ebert, A.; Herwegh, M.; Karl, R.; Edwin, G.; Decrouez, D.

2007-12-01

In the upper crust, shear zones are widespread and appear at different scales. Although deformation conditions, shear zone history, and displacements vary in time and space between shear zones and also within them, in all shear zones similar trends in the evolution of large- to micro-scale fabrics can be observed. The microstructural analyses of calcite mylonites from Naxos and various Helvetic nappes show that microstructures from different metamorphic zones vary considerably on the outcrop- and even on the sample- scale. However, grain sizes tend to increase with metamorphic degree in case of Naxos and the Helvetic nappes. Although deformation conditions (e.g. deformation temperature, strain rate, and shear zone geometry, i.e. shear zone width and rock type above/below thrust) vary between the different tectonic settings, microstructural trends (e.g. grain size) correlate with each other. This is in contrast to many previous studies, where no corrections for second phase contents have been applied. In an Arrhenius-type diagram, the grain growth trends of calcite of all studied shear zones fit on a single trend, independent of the dimensions of localized large-scale structures, which is in the dm to m- and km-range in case of the Helvetic thrusts and the marble suite of Naxos, respectively. The calcite grain size increases continuously from few μm to >2mm with a temperature increase from <300°C to >700°C. In a field geologist's point of view, this is an important observation because it shows that natural dynamically stabilized steady state microfabrics can be used to estimate temperature conditions during deformation, although the tectonic settings are different (e.g. strain rate, fluid flow). The reason for this agreement might be related to a scale-dependence of the shear zone dimensions, where the widths increase with increasing metamorphic conditions. In this sense, the deformation volumes affected by localization must closely be linked to the strength of the affected rocks. In comparison to experiments, similar microstructural trends are observed. Here, however, shifts of these trends occur due to the higher strain rates.

Metamorphic reactions, grain size reduction and deformation of mafic lower crustal rocks

NASA Astrophysics Data System (ADS)

Degli Alessandrini, Giulia; Menegon, Luca; Beltrando, Marco; Dijkstra, Arjan; Anderson, Mark

2016-04-01

This study investigates grain-scale deformation mechanisms associated with strain localization in the mafic continental lower crust, with particular focus on the role of syn-kinematic metamorphic reactions and their product - symplectites - in promoting grain size reduction and phase mixing. The investigated shear zone is hosted in the Finero mafic-ultramafic complex in the Italian Southern Alps. Shearing occurred at T ≥ 650° C and P ≥ 0.4-0.6 GPa. The shear zone reworks both mafic and ultramafic lithologies and displays anastomosing patterns of (ultra)mylonitic high strain zones wrapping less foliated, weakly deformed low strain domains. Field and microstructural observations indicate that different compositional layers of the shear zone responded differently to deformation, resulting in strain partitioning. Four distinct microstructural domains have been identified: (1) an ultramylonitic domain characterized by an amph + pl matrix (grain size < 30μm) with large amphibole porphyroclasts (grain size between 200μm and 5000μm) and rare garnets; (2) a domain rich in garnet porphyroclasts embedded in a matrix of monomineralic plagioclase displaying a core and mantle structure (average grain size 45μm) (3) a metagabbroic domain with porphyroclasts of clinopyroxene, orthopyroxene and garnets (200μm average grain size) wrapped by monomineralic ribbons of recrystallized plagioclase and (4) a garnet-free ultramylonitic domain composed of an intermixed amph + cpx + opx + pl matrix (6μm average grain size). In these domains, each porphyroclastic mineral responds differently to deformation: amphibole readily breaks down to symplectitic intergrowths of amph + pl or opx + pl. Garnet undergoes fracturing (in domain 2) or reacts to give symplectites of pl + opx (in domain 3). Plagioclase dynamically recrystallizes in mono-phase aggregates, whereas clinopyroxene undergoes fracturing and orthopyroxene undergoes plastic deformation. The behaviour of the different phases and their relative abundance in the layers are believed to influence the deformation of the layers themselves. In symplectite-rich layers (domains 1, 4) deformation is localised, grain-size is below 30μm and phases are well mixed. On the other hand, in pyroxene or plagioclase-rich layers, deformation is less localised, the phases are less mixed and the grain size is larger (domain 2, 3). These preliminary results suggest that syn-kinematic metamorphic reactions forming symplectites played an essential role in grain size reduction, phase mixing and strain localization. We speculate that the compositional domains with symplectites localized deformation more efficiently, by activation of grain size sensitive creep, most likely because those domains were originally more hydrated than the others. On the contrary, domains without symplectites accommodated deformation less efficiently, either through fracturing (clinopyroxene, garnet) or dislocation creep + recrystallization (orthopyroxene, plagioclase).

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

Effects of annealing conditions on microstructure and mechanical properties of low carbon, manganese transformation-induced plasticity steel

NASA Astrophysics Data System (ADS)

Jang, Jae-Myeong; Kim, Sung-Joon; Kang, Nam Hyun; Cho, Kyung-Mox; Suh, Dong-Woo

2009-12-01

The effects of annealing conditions on microstructural evolution and mechanical properties have been investigated in low carbon, manganese TRIP (Mn TRIP) steel based on a 0.12C-6Mn-0.5Si-3Al alloy system. The microstructure of cold-rolled sheet subjected to annealing at 760 °C to 800 °C for 30 s to 1800 s consists of a recrystallized ferrite matrix and fine-grained austenite with a phase fraction of 25 % to 35 %. Variation of the annealing conditions remarkably influenced the characteristics of constituent phases and thus affected the tensile strength and elongation. Optimization of microstructural parameters such as grain size and fraction of constituent phases, which control the yield strength, overall work hardening, and the kinetics of strain-induced martensite formation, is thus critical for obtaining an exceptional mechanical balance of the alloy.

Method of producing improved microstructure and properties for ceramic superconductors

DOEpatents

Singh, Jitendra P.; Guttschow, Rob A.; Dusek, Joseph T.; Poeppel, Roger B.

1996-01-01

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). 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 approximately 4 .mu.m. Such a microstructure results in reduced microcracking, strengths as high as 191 MPa and high critical current density capacity.

Method of producing improved microstructure and properties for ceramic superconductors

DOEpatents

Singh, J.P.; Guttschow, R.A.; Dusek, J.T.; Poeppel, R.B.

1996-06-11

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}). 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 approximately 4 {micro}m. Such a microstructure results in reduced microcracking, strengths as high as 191 MPa and high critical current density capacity. 20 figs.

Rheology, microstructure and crystallographic preferred orientation of matrix containing a dispersed second phase: Insight from experimentally deformed ice

NASA Astrophysics Data System (ADS)

Cyprych, Daria; Piazolo, Sandra; Wilson, Christopher J. L.; Luzin, Vladimir; Prior, David J.

2016-09-01

We utilize in situ neutron diffraction to continuously track the average grain size and crystal preferred orientation (CPO) development in ice, during uniaxial compression of two-phase and pure ice samples. Two-phase samples are composed of ice matrix and 20 vol.% of second phases of two types: (1) rheologically soft, platy graphite, and (2) rigid, rhomb-shaped calcite. The samples were tested at 10 °C below the ice melting point, ambient pressures, and two strain rates (1 ×10-5 and 2.5 ×10-6 s-1), to 10 and 20% strain. The final CPO in the ice matrix, where second phases are present, is significantly weaker, and ice grain size is smaller than in an ice-only sample. The microstructural and rheological data point to dislocation creep as the dominant deformation regime. The evolution and final strength of the CPO in ice depend on the efficiency of the recrystallization processes, namely grain boundary migration and nucleation. These processes are markedly influenced by the strength, shape, and grain size of the second phase. In addition, CPO development in ice is further accentuated by strain partitioning into the soft second phase, and the transfer of stress onto the rigid second phase.

Virtual modeling of polycrystalline structures of materials using particle packing algorithms and Laguerre cells

NASA Astrophysics Data System (ADS)

Morfa, Carlos Recarey; Farias, Márcio Muniz de; Morales, Irvin Pablo Pérez; Navarra, Eugenio Oñate Ibañez de; Valera, Roberto Roselló

2018-04-01

The influence of the microstructural heterogeneities is an important topic in the study of materials. In the context of computational mechanics, it is therefore necessary to generate virtual materials that are statistically equivalent to the microstructure under study, and to connect that geometrical description to the different numerical methods. Herein, the authors present a procedure to model continuous solid polycrystalline materials, such as rocks and metals, preserving their representative statistical grain size distribution. The first phase of the procedure consists of segmenting an image of the material into adjacent polyhedral grains representing the individual crystals. This segmentation allows estimating the grain size distribution, which is used as the input for an advancing front sphere packing algorithm. Finally, Laguerre diagrams are calculated from the obtained sphere packings. The centers of the spheres give the centers of the Laguerre cells, and their radii determine the cells' weights. The cell sizes in the obtained Laguerre diagrams have a distribution similar to that of the grains obtained from the image segmentation. That is why those diagrams are a convenient model of the original crystalline structure. The above-outlined procedure has been used to model real polycrystalline metallic materials. The main difference with previously existing methods lies in the use of a better particle packing algorithm.

Kinetic model for dependence of thin film stress on growth rate, temperature, and microstructure

NASA Astrophysics Data System (ADS)

Chason, E.; Shin, J. W.; Hearne, S. J.; Freund, L. B.

2012-04-01

During deposition, many thin films go through a range of stress states, changing from compressive to tensile and back again. In addition, the stress depends strongly on the processing and material parameters. We have developed a simple analytical model to describe the stress evolution in terms of a kinetic competition between different mechanisms of stress generation and relaxation at the triple junction where the surface and grain boundary intersect. The model describes how the steady state stress scales with the dimensionless parameter D/LR where D is the diffusivity, R is the growth rate, and L is the grain size. It also explains the transition from tensile to compressive stress as the microstructure evolves from isolated islands to a continuous film. We compare calculations from the model with measurements of the stress dependence on grain size and growth rate in the steady state regime and of the evolution of stress with thickness for different temperatures.

Grain growth in uranium nitride prepared by spark plasma sintering

NASA Astrophysics Data System (ADS)

Johnson, Kyle D.; Lopes, Denise Adorno

2018-05-01

Uranium mononitride (UN) has long been considered a potential high density, high performance fuel candidate for light water reactor (LWR) and fast reactor (FR) applications. However, deployability of this fuel has been limited by the notable resistance to sintering and subsequent difficulty in producing a desirable microstructure, the high costs associated with 15N enrichment, as well as the known proclivity to oxidation and interaction with steam. In this study, the stimulation of grain growth in UN pellets sintered using SPS has been investigated. The results reveal that by using SPS and controlling temperature, time, and holding pressure, grain growth can be stimulated and controlled to produce a material featuring both a desired porosity and grain size, at least within the range of interest for nuclear fuel candidates. Grain sizes up to 31 μm were obtained using temperatures of 1650 °C and hold times of 15 min. Evaluation by EBSD reveal grain rotation and coalescence as the dominant mechanism in grain growth, which is suppressed by the application of higher external pressure. Moreover, complete closure of the porosity of the material was observed at relative densities of 96% TD, resulting in a material with sufficient porosity to accommodate LWR burnup. These results indicate that a method exists for the economic fabrication of an 15N-bearing uranium mononitride fuel with favorable microstructural characteristics compatible with use in a light water-cooled nuclear reactor.

[Microwave sintering of nanometer powder of alumina and zirconia-based dental ceramics].

PubMed

Chen, Yi-Fan; Lu, Dong-Mei; Wan, Qian-Bing; Jin, Yong; Zhu, Ju-Mu

2006-02-01

The objective of the present study was to investigate the feasibility and reliability of sintering alumina and zirconia-based all-ceramic materials through a recently introduced microwave heating technique. The variation of crystal phases, the growth of grain sizes and microstructural features of these materials were evaluated after sintering. Four different groups of powder (l00%Al2O3, 60%Al2O3+40%ZrO2, 40% Al2O3+60%ZrO2, 100% ZrO2) were respectively press-compacted to fabricate green disk samples, 5 specimen of each group were prepared. All the samples were surrounded by refractory materials for heat containment and processed at 1 600 degrees C in a domestic microwave oven (850 W, 2 450 MHz), 1 600 degrees C/5 min for heating rate, 10 min for holding time. After sintering, the phase composition and average grain size of these ceramics were examined using X-ray diffraction (XRD). Their microstructure characteristics were studied by scanning electron microscopy (SEM). All the specimens were successfully sintered with the application of microwave heating system in combination with a suitable thermal insulator. No phase change was found in alumina while monoclinic-zirconia was found to be transformed to tetragonal-zirconia. A little grain size growth of Al2O3 and ZrO2 has been observed with Al2O3 24.1 nm/before and 51.8 nm/after; ZrO2 25.3 nm/before and 29.7 nm/after. The SEM photos indicated that the microwave-sintered Al2O3-ZrO2 ceramics had a uniform crystal distribution and their crystal sizes could be maintained within the range of nanometers. It is expected that in the near future microwave heating system could be a promising substitute for conventional processing methods due to its unparalled advantages, including more rapid heating rate, shortened sintering time, superfine grain size, improved microstructure and much less expensive equipment.

Grain growth kinetics in liquid-phase-sintered zinc oxide-barium oxide ceramics

NASA Technical Reports Server (NTRS)

Yang, Sung-Chul; German, Randall M.

1991-01-01

Grain growth of ZnO in the presence of a liquid phase of the ZnO-BaO system has been studied for temperatures from 1300 to 1400 C. The specimens were treated in boiling water and the grains were separated by dissolving the matrix phase in an ultrasonic bath. As a consequence 3D grain size measurements were possible. Microstructural examination shows some grain coalescence with a wide range of neck size ratios and corresponding dihedral angles, however, most grains are isolated. Lognormal grain size distributions show similar shapes, indicating that the growth mechanism is invariant over this time and temperature. All regressions between G exp n and time for n = 2 and 3 proved statistically significant. The rate constants calculated with the growth exponent set to n = 3 are on the same order of magnitude as in metallic systems. The apparent activation energy for growth is estimated between 355 and 458 kJ/mol.

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.

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 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.

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.

Three-Dimensional Characterization and Modeling of Microstructural Weak Links for Spall Damage in FCC Metals

DOE PAGES

Krishnan, Kapil; Brown, Andrew; Wayne, Leda; ...

2014-11-25

Local microstructural weak links for spall damage were investigated using three-dimensional (3-D) characterization in multicrystalline copper samples (grain size ≈ 450 µm) shocked with laser-driven plates at low pressures (2 to 4 GPa). The thickness of samples and flyer plates, approximately 1000 and 500 µm respectively, led to short pressure pulses that allowed isolating microstructure effects on local damage characteristics. Electron Backscattering Diffraction and optical microscopy were used to relate the presence, size, and shape of porosity to local microstructure. The experiments were complemented with 3-D finite element simulations of individual grain boundaries (GBs) that resulted in large damage volumesmore » using crystal plasticity coupled with a void nucleation and growth model. Results from analysis of these damage sites show that the presence of a GB-affected zone, where strain concentration occurs next to a GB, correlates strongly with damage localization at these sites, most likely due to the inability of maintaining strain compatibility across these interfaces, with additional effects due to the inclination of the GB with respect to the shock. Results indicate that strain compatibility plays an important role on intergranular spall damage in metallic materials.« less

Metallographic examination of TD-nickel base alloys. [thermal and chemical etching technique evaluation

NASA Technical Reports Server (NTRS)

Kane, R. D.; Petrovic, J. J.; Ebert, L. J.

1975-01-01

Techniques are evaluated for chemical, electrochemical, and thermal etching of thoria dispersed (TD) nickel alloys. An electrochemical etch is described which yielded good results only for large grain sizes of TD-nickel. Two types of thermal etches are assessed for TD-nickel: an oxidation etch and vacuum annealing of a polished specimen to produce an etch. It is shown that the first etch was somewhat dependent on sample orientation with respect to the processing direction, the second technique was not sensitive to specimen orientation or grain size, and neither method appear to alter the innate grain structure when the materials were fully annealed prior to etching. An electrochemical etch is described which was used to observe the microstructures in TD-NiCr, and a thermal-oxidation etch is shown to produce better detail of grain boundaries and to have excellent etching behavior over the entire range of grain sizes of the sample.

A Rate-Theory-Phase-Field Model of Irradiation-Induced Recrystallization in UMo Nuclear Fuels

NASA Astrophysics Data System (ADS)

Hu, Shenyang; Joshi, Vineet; Lavender, Curt A.

2017-12-01

In this work, we developed a recrystallization model to study the effect of microstructures and radiation conditions on recrystallization kinetics in UMo fuels. The model integrates the rate theory of intragranular gas bubble and interstitial loop evolutions and a phase-field model of recrystallization zone evolution. A first passage method is employed to describe one-dimensional diffusion of interstitials with a diffusivity value several orders of magnitude larger than that of fission gas xenons. With the model, the effect of grain sizes on recrystallization kinetics is simulated. The results show that (1) recrystallization in large grains starts earlier than that in small grains, (2) the recrystallization kinetics (recrystallization volume fraction) decrease as the grain size increases, (3) the predicted recrystallization kinetics are consistent with the experimental results, and (4) the recrystallization kinetics can be described by the modified Avrami equation, but the parameters of the Avrami equation strongly depend on the grain size.

Microstructure and texture evolution in cold-rolled and annealed alloy MA-956

NASA Astrophysics Data System (ADS)

Hosoda, Takashi

The microstructural and texture development with thermomechanical processing, performed through a combination of cold-rolling and annealing, in MA-956 plate consisting of a layered and inhomogeneous microstructure was systematically assessed. The alloy contained in mass percent, 20 Cr, 4.8 Al, 0.4 Ti, 0.4 Y2O3, and the balance iron. The starting material was as-hot-rolled plate, 9.7 mm thick. The as-hot-rolled plate was subjected to 40%, 60%, and 80% cold-rolling reduction and subsequently annealed at 1000, 1200, or 1380. Assessment of microstructural and texture developments before and after cold-rolling and annealing was performed using light optical microscopy (LOM), Vickers hardness testing, and electron backscatter diffraction (EBSD). Locally introduced misorientations by cold-rolling in each region were evaluated by Kernel Average Misorientation (KAM) maps. The as-hot-rolled condition contained a layered and inhomogeneous microstructure consisting of thin and coarse elongated grains, and aggregated regions which consisted of fine grains and sub-grains with {100} texture parallel to the longitudinal direction. The microstructure of the 40% cold-rolled condition contained deformation bands, and the 60% and 80% cold-rolled conditions also contained highly deformed regions where the deformation bands were intricately tangled. A predominant orientation of (001) parallel to the rolling direction was developed during cold-rolling, becoming more prominent with increasing reduction. The magnitudes of KAM angles varied through the thickness depending on the initial microstructures. Recrystallization occurred in regions where high KAM angles were dense after annealing and nucleation sites were the aggregation regions, deformation bands, and highly deformed regions. The shape and size of the recrystallized grains varied depending on the nucleation sites.

The effect of grain size on aluminum anodes for Al-air batteries in alkaline electrolytes

NASA Astrophysics Data System (ADS)

Fan, Liang; Lu, Huimin

2015-06-01

Aluminum is an ideal material for metallic fuel cells. In this research, different grain sizes of aluminum anodes are prepared by equal channel angular pressing (ECAP) at room temperature. Microstructure of the anodes is examined by electron backscatter diffraction (EBSD) in scanning electron microscope (SEM). Hydrogen corrosion rates of the Al anodes in 4 mol L-1 NaOH are determined by hydrogen collection method. The electrochemical properties of the aluminum anodes are investigated in the same electrolyte using electrochemical impedance spectroscopy (EIS) and polarization curves. Battery performance is also tested by constant current discharge at different current densities. Results confirm that the electrochemical properties of the aluminum anodes are related to grain size. Finer grain size anode restrains hydrogen evolution, improves electrochemical activity and increases anodic utilization rate. The proposed method is shown to effectively improve the performance of Al-air batteries.

Effect of calcination temperature on microstructure and magnetic properties of Ni{sub 0.5}Zn{sub 0.25}Cu{sub 0.25} Fe{sub 2}O{sub 4} nanoparticles synthesized by sol-gel method

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

Pransisco, Prengki, E-mail: prengkipransisco@gmail.com, E-mail: afza@petronas.com.my; Shafie, Afza, E-mail: prengkipransisco@gmail.com, E-mail: afza@petronas.com.my; Guan, Beh Hoe, E-mail: beh.hoeguan@petronas.com.my

2014-10-24

This paper examines the effect of calcination process on the structural and magnetic properties material nanostructure composite of Ni{sub 0Ð}œ‡{sub 5}Zn{sub 0Ð}œ‡{sub 25}Cu{sub 0.25} Fe{sub 2}O{sub 4} ferrites. The samples were successfully prepared by sol-gel method at different calcination temperature, which are 600°C, 700°C, 800°C and 900°C. Morphological investigation, average crystallite size and microstructure of the material were examined by using X-ray diffraction (XRD) and confirmed by high resolution transmission electron microscope (HRTEM) and field emission scanning electron microscope (FESEM). The effects of calcination temperature on the magnetic properties were calculated by using vibrating sample magnetometer (VSM). The XRD resultmore » shows single-phase cubic spinel structure with interval average size 5.9-38 nm, and grain size microstructure of the material was increasing with temperature increases. The highest magnetization saturation was reached at a temperature 800°C with value 53.89 emu/g, and the value coercive force (Hc) was inversely with the grain size.« less

Effects of Zr on microstructure and mechanical properties of Al-Cu base ribbons spun by planar flow casting

NASA Astrophysics Data System (ADS)

Lee, S. M.; Hong, C. P.

1998-04-01

The effects of the Zr addition on the solidification behavior and mechanical properties of the AI-Cu alloy ribbon have been investigated. Zr addition reduced the average grain size of the ribbon at the wheel-side surface, and promoted the microstructural transition into cellular/dendritic structure. Another noteworthy effect of Zr was the homogenization of the microstructure. The addition of Zr up to 0.5 wt.% in the /U-4.3 wt.% Cu ribbon resulted in a considerable increase in hardness at both the wheel-side and the air-side surfaces. The yield strength increased with the addition of Zr due to the grain refincment and more homogeneous distribution of ZrAI, particles. despite no noticeable improvement of the ductility.

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

Microstructure and Mechanical Properties of Fe-18Mn-18Cr-0.5N Austenitic Nonmagnetic Stainless Steel in Asymmetric Hot Rolling

NASA Astrophysics Data System (ADS)

Song, Y. L.; Li, C. S.; Ma, B.; Han, Y. H.

2017-05-01

Asymmetric hot rolling (ASHR) with a mismatch speed ratio of 1.15 in a single pass was applied to Fe-18Mn-18Cr-0.5N steel and was compared with symmetric hot rolling (SHR). The results indicated that a through-thickness microstructure gradient was formed in the plate due to the shear strain (0.36) introduced by ASHR. A fine-grained layer with the average size of 3 μm was achieved at the top surface of ASHR plate, while numerous elongated grains with a few recrystallized grains were presented at the center layer. The texture was distributed randomly at the top surface of ASHR plate, and a weaker intensity of typical hot-rolled texture in austenitic steel was obtained at the center layer of ASHR plate compared to SHR plate. An excellent combination of microhardness, strength and ductility was obtained in the ASHR plate, which was attributed to gradient microstructure induced by ASHR.

Properties of Rolled AZ31 Magnesium Alloy Sheet Fabricated by Continuous Variable Cross-Section Direct Extrusion

NASA Astrophysics Data System (ADS)

Liu, Yang; Li, Feng; Li, Xue Wen; Shi, Wen Yong

2018-03-01

Rolling is currently a widely used method for manufacturing and processing high-performance magnesium alloy sheets and has received widespread attention in recent years. Here, we combined continuous variable cross-section direct extrusion (CVCDE) and rolling processes. The microstructure and mechanical properties of the resulting sheets rolled at different temperatures from CVCDE extrudate were investigated by optical microscopy, scanning electron microscope, transmission electron microscopy and electron backscatter diffraction. The results showed that a fine-grained microstructure was present with an average grain size of 3.62 μm in sheets rolled from CVCDE extrudate at 623 K. Dynamic recrystallization and a large strain were induced by the multi-pass rolling, which resulted in grain refinement. In the 573-673 K range, the yield strength, tensile strength and elongation initially increased and then declined as the CVCDE temperature increased. The above results provide an important scientific basis of processing, manufacturing and the active control on microstructure and property for high-performance magnesium alloy sheet.

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.

Chemical composition and microstructure of Bauhinia grains.

PubMed

Amonsou, Eric O; Siwela, Muthulisi; Dlamini, Nomusa

2014-09-01

Bauhinia is a leguminous plant species found in almost every part of the world, including southern Africa. In this study, grain composition and protein body microstructure of two indigenous southern African Bauhinia species, B. galpinii and B. petersiana were determined. Protein (38 g/100 g) and fat (23 g/100 g) were the major constituents of Bauhinia. Bauhinia grains also contained substantial amounts of zinc (6 mg/100 g) and iron (3 mg/100 g) when compared to FAO/WHO standards. The parenchyma cells of Bauhinia showed spherical protein bodies with globoids inclusions and these were surrounded by lipids. However, the protein bodies of B. petersiana were smaller in size (7 ± 3 μm) than those of B. galpinii (13 ± 4 μm). The microstructure of protein bodies in Bauhinia is very similar to that of soya, suggesting that the processing technology developed for soya protein may be adopted for Bauhinia.

Investigation of the Effect of Various Oxide and Fluoride Additives on the Microstructure, Electronic Properties, and Phase Shifting Ability of Ba(1-x) Sr(x)TiO3

DTIC Science & Technology

1993-09-01

AD-A271 756 ARMY RESEARCH LABORATORY Investigation of the Effect of Various Oxide and Flouride Additives on the Microstructure, Electronic Properties ...NUMBERS Investigation of the Effect of Various Oxide and Fluoride Additives on the Microstructure, Electronic Properties , and Phase Shifting Ability of...dielectric properties . tunability. hysteresis. and grain size have been investigated. The homogeneity of the doped materials has been verified using

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.

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.

Ferrite Formation Dynamics and Microstructure Due to Inclusion Engineering in Low-Alloy Steels by Ti2O3 and TiN Addition

NASA Astrophysics Data System (ADS)

Mu, Wangzhong; Shibata, Hiroyuki; Hedström, Peter; Jönsson, Pär Göran; Nakajima, Keiji

2016-08-01

The dynamics of intragranular ferrite (IGF) formation in inclusion engineered steels with either Ti2O3 or TiN addition were investigated using in situ high temperature confocal laser scanning microscopy. Furthermore, the chemical composition of the inclusions and the final microstructure after continuous cooling transformation was investigated using electron probe microanalysis and electron backscatter diffraction, respectively. It was found that there is a significant effect of the chemical composition of the inclusions, the cooling rate, and the prior austenite grain size on the phase fractions and the starting temperatures of IGF and grain boundary ferrite (GBF). The fraction of IGF is larger in the steel with Ti2O3 addition compared to the steel with TiN addition after the same thermal cycle has been imposed. The reason for this difference is the higher potency of the TiO x phase as nucleation sites for IGF formation compared to the TiN phase, which was supported by calculations using classical nucleation theory. The IGF fraction increases with increasing prior austenite grain size, while the fraction of IGF in both steels was the highest for the intermediate cooling rate of 70 °C/min, since competing phase transformations were avoided, the structure of the IGF was though refined with increasing cooling rate. Finally, regarding the starting temperatures of IGF and GBF, they decrease with increasing cooling rate and the starting temperature of GBF decreases with increasing grain size, while the starting temperature of IGF remains constant irrespective of grain size.

Cyclic Spin Testing of Superalloy Disks With a Dual Grain Microstructure

NASA Technical Reports Server (NTRS)

Gayda, John; Kantzos, Pete

2005-01-01

An aggressive cyclic spin test program was run to verify the reliability of superalloy disks with a dual grain structure, fine grain bore and coarse grain rim, utilizing a disk design with web holes bisecting the grain size transition zone. Results of these tests were compared with conventional disks with uniform grain structures. Analysis of the test results indicated the cyclic performance of disks with a dual grain structure could be estimated to a level of accuracy which does not appear to prohibit the use of this technology in advanced gas turbine engines, although further refinement of lifing methodology is clearly warranted.

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.

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.

Pre-aging time dependence of microstructure and mechanical properties in nanostructured Al-2wt%Cu alloy

NASA Astrophysics Data System (ADS)

Azad, Bahram; Borhani, Ehsan

2016-03-01

This work is focused on the effect of pre-aging time on the properties of Al-2wt%Cu alloy processed by accumulative roll bonding (ARB) process. Following aged at 190 °C for 10 or 30 min, the samples were deformed up to a strain of 4.8 by the ARB process. The microstructure evolution was investigated by transmission electron microscope and electron backscattering diffraction analyzes. The results showed that the Al2Cu precipitates were formed with different sizes due to the different pre-aging times and the finer precipitates were more effective on the formation of high angle grain boundaries during the ARB process. The grain size of Aged-10 min and Aged-30 min specimens decreased to 400 nm and 420 nm, respectively, after 6 cycles of the ARB process. Also, the final texture after 6 cycles of the ARB process, shown in the {111} pole figure, were different depending on the starting microstructures. The mechanical properties of specimens were investigated by the Vickers microhardness measurements and the tensile tests. The results showed that the mechanical properties are affected by the starting microstructure. The mechanical properties of Aged-10 min specimen were different compared to Aged-30 min specimen due to the different size of the pre-existing precipitates. Although by continuing process, the precipitates were probably dissolved due to the heavy deformation.

An Investigation of TIG welding parameters on microhardness and microstructure of heat affected zone of HSLA steel

NASA Astrophysics Data System (ADS)

Musa, M. H. A.; Maleque, M. A.; Ali, M. Y.

2018-01-01

Nowadays a wide variety of metal joining methods are used in fabrication industries. In this study, the effect of various welding parameters of the TIG welding process on microhardness, depth, and microstructure of the heat-affected zone (HAZ) of L450 HSLA steel and optimizing these process parameters following Taguchi experimental design was investigated. The microhardness tended to increase significantly with the increase of welding speed from 1.0 to 2.5 mm/s whereas the width of HAZ decreased. The current and arc voltage was found to be less significant in relative comparison. Microstructures of the welded samples were also studied to analyze the changes in the microstructure of the material in terms of ferrite, pearlite, bainite, and martensite formations. Welding speed was found to be the most significant factors leading to changes in microhardness and metallurgical properties. The increase of welding heat input caused an increase in width (depth) of HAZ and the growth of prior austenite grains and then enlarged the grain size of coarse grain heat affected zone (CGHAZ). However, the amount of martensite in the HAZ decreased accompanied by an opposite change of paint. It was observed that the hardness properties and the microstructural feature of HAZ area was strongly affected by the welding parameters.

A heat treatment procedure to produce fine-grained lamellar microstructures in a P/M titanium aluminide alloy

NASA Astrophysics Data System (ADS)

Au, Peter

A process for fabricating advanced aerospace titanium aluminide alloys starting from metal powders (the hot isostatically consolidated P/M process) is presented in this thesis. This process does not suffer the difficulties of chemical inhomogeneities and coarse grain structure of castings. In addition heat treatments which take advantage of the refined structure of HIP processed materials are developed to achieve microstructure control and subsequent mechanical property control. It is shown that a better "property balance" is possible after the heat treatment of HIP consolidated materials than it is with alternative processing. It is well understood that the standard microstructures (near-gamma, duplex, nearly lamellar, and fully lamellar) do not have the balanced mechanical properties (tensile, yield, creep and fatigue strength, ductility and fracture toughness) necessary for optimal performance in aero engine and automotive applications. In this work a fine-grained fully lamellar (FGFL) microstructure is developed for property control and in particular for achieving a much improved property balance. A heat treatment procedure for this purpose which consists of cyclic processing in the alpha transus temperature region to achieve an FGFL structure with grain sizes in the range of 50 mum to 150 mum is presented. Compared with conventional duplex structured materials, the minimum creep rate is an order of magnitude lower with only a 10% loss in tensile yield strength. Moreover, a three-fold increase in tensile elongation is possible by converting to an FGFL structure with only a 30% loss in minimum creep rate. These are attractive trade-offs when considering the use of these alloys for aerospace purposes. A thorough literature review of the mechanisms of formation of standard microstructures and their deformation under mechanical loading is contained in the thesis. In addition, conventional techniques to produce FGFL microstructures in wrought and cast materials are discussed in detail. Beyond the review, the results of experiments are described for determining the alpha transus temperature, the phase transformation kinetics in this region and the effects of heat treatment time and cooling rate on microstructure. Based on this preliminary work, a heat treatment to achieve a FGFL microstructure with grain sizes in the range of 50 mum to 150 mum is proposed and confirmed. The room temperature and high temperature mechanical properties of these materials are compared with those of conventional duplex and fully lamellar structures. The results of this experimentation are discussed in terms of the fundamental mechanisms for controlling microstructure and mechanical properties in these materials. The potential for applying cyclic heat treatments to cast and wrought materials to improve the mechanical property balance in engineering practice is discussed.

Fundamental Investigation of the Microstructural Parameters to Improve Dynamic Response in Al-Cu Model System

DTIC Science & Technology

2014-05-01

grain size. Recrystallization was then induced via annealing just above the solvus temperature. After quenching , the bars were immediately placed into...that the values were statistically significant. Precipitate sizes ranged from approximately 100 nanometers in diameter up to 2-5 microns in diameter

Development of the Microstructure Based Stochastic Life Prediction Models

DTIC Science & Technology

1991-06-27

sizes and shapes of the recrystallized and unrecrystallized grains and also measure sizes of subgrains. We will also determine the degree of...J. Lankford et al., STP 811, ASTM STP 811. ASTM, 1983. 5. M. R. James and W. L. Morris, "The Role of Microplastic Deformation in Fatigue Crack

Particle Size Effects on the Quality of Flour Tortillas Enriched with Whole Grain Waxy Barley

USDA-ARS?s Scientific Manuscript database

Wheat tortillas were enriched with whole barley flour (WBF) of different particle sizes including 237 micros (regular-R), 131 micros (intermediate-IM), and 68 micros (microground-MG). Topographical and fluorescent microstructure images of flours, doughs and tortillas were examined. Flours and tort...

Effect of Al on Grain Refinement and Mechanical Properties of Mg-3Nd Casting Alloy

NASA Astrophysics Data System (ADS)

Wang, Lei; Feng, Yicheng; Wang, Liping; Chen, Yanhong; Guo, Erjun

2018-05-01

The effect of Al on the grain refinement and mechanical properties of as-cast Mg-3Nd alloy was investigated systematically by a series of microstructural analysis, solidification analysis and tensile tests. The results show that Al has an obvious refining effect on the as-cast Mg-3Nd alloy. With increasing Al content, the grain size of the as-cast Mg-3Nd alloy decreases firstly, then increases slightly after the Al content reaching 3 wt.%, and the minimum grain size of the Mg-3Nd alloy is 48 ± 4.0 μm. The refining mechanism can be attributed to the formation of Al2Nd particles, which play an important role in the heterogeneous nucleation. The strength and elongation of the Mg-3Nd alloy refined by Al also increase with increasing Al content and slightly decrease when the Al content is more than 3 wt.%, and the strengthening mechanism is attributed to the grain refinement as well as dispersed intermetallic particles. Furthermore, the microstructural thermal stability of the Mg-3Nd-3Al alloy is higher than that of the Mg-3Nd-0.5Zr alloy. Overall, the Mg-3Nd alloy with Al addition is a novel alloy with wide and potential application prospects.

Irradiation Induced Microstructure Evolution in Nanostructured Materials: A Review

PubMed Central

Liu, Wenbo; Ji, Yanzhou; Tan, Pengkang; Zang, Hang; He, Chaohui; Yun, Di; Zhang, Chi; Yang, Zhigang

2016-01-01

Nanostructured (NS) materials may have different irradiation resistance from their coarse-grained (CG) counterparts. In this review, we focus on the effect of grain boundaries (GBs)/interfaces on irradiation induced microstructure evolution and the irradiation tolerance of NS materials under irradiation. The features of void denuded zones (VDZs) and the unusual behavior of void formation near GBs/interfaces in metals due to the interactions between GBs/interfaces and irradiation-produced point defects are systematically reviewed. Some experimental results and calculation results show that NS materials have enhanced irradiation resistance, due to their extremely small grain sizes and large volume fractions of GBs/interfaces, which could absorb and annihilate the mobile defects produced during irradiation. However, there is also literature reporting reduced irradiation resistance or even amorphization of NS materials at a lower irradiation dose compared with their bulk counterparts, since the GBs are also characterized by excess energy (compared to that of single crystal materials) which could provide a shift in the total free energy that will lead to the amorphization process. The competition of these two effects leads to the different irradiation tolerance of NS materials. The irradiation-induced grain growth is dominated by irradiation temperature, dose, ion flux, character of GBs/interface and nanoprecipitates, although the decrease of grain sizes under irradiation is also observed in some experiments. PMID:28787902

Microstructure characterization of the stir zone of submerged friction stir processed aluminum alloy 2219

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

Feng, Xiuli, E-mail: feng.97@osu.edu; State Key Laboratory of Advanced Welding and Joining, Harbin Institute of Technology, Harbin 150001; Liu, Huijie, E-mail: liuhj@hit.edu.cn

Aluminum alloy 2219-T6 was friction stir processed using a novel submerged processing technique to facilitate cooling. Processing was conducted at a constant tool traverse speed of 200 mm/min and spindle rotation speeds in the range from 600 to 800 rpm. The microstructural characteristics of the base metal and processed zone, including grain structure and precipitation behavior, were studied using optical microscopy (OM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Microhardness maps were constructed on polished cross sections of as-processed samples. The effect of tool rotation speed on the microstructure and hardness of the stir zone was investigated. Themore » average grain size of the stir zone was much smaller than that of the base metal, but the hardness was also lower due to the formation of equilibrium θ precipitates from the base metal θ′ precipitates. Stir zone hardness was found to decrease with increasing rotation speed (heat input). The effect of processing conditions on strength (hardness) was rationalized based on the competition between grain refinement strengthening and softening due to precipitate overaging. - Highlights: • SZ grain size (∼ 1 μm) is reduced by over one order of magnitude relative to the BM. • Hardness in the SZ is lower than that of the precipitation strengthened BM. • Metastable θ′ in the base metal transforms to equilibrium θ in the stir zone. • Softening in the SZ results from a decrease of precipitation strengthening.« less

Structure and thermomechanical behavior of NiTiPt shape memory alloy wires.

PubMed

Lin, Brian; Gall, Ken; Maier, Hans J; Waldron, Robbie

2009-01-01

The objective of this work is to understand the structure-property relationships in polycrystalline NiTiPt (Ti 42.7 at.% Ni 7.5 at %Pt) with a composition showing pseudoelasticity at ambient temperatures. Structural characterization of the alloy includes grain size determination and texture analysis while the thermomechanical properties are explored using tensile testing. Variation in heat treatment is used as a vehicle to modify microstructure. The results are compared to experiments on Ni-rich NiTi alloy wires (Ti-51.0 at.% Ni), which are in commercial use in various biomedical applications. With regards to microstructure, both alloys exhibit a <111> fiber texture along the wire drawing axis; however, the NiTiPt alloy grain size is smaller than that of the Ni-rich NiTi wires, while the latter materials contain second-phase precipitates. Given the nanometer-scale grain size in NiTiPt and the dispersed, nanometer-scale precipitate size in NiTi, the overall strength and ductility of the alloys are essentially identical when given appropriate heat treatments. Property differences include a much smaller stress hysteresis and smaller temperature dependence of the transformation stress for NiTiPt alloys compared to NiTi alloys. Potential benefits and implications for use in vascular stent applications are discussed.

Electrochemical Behavior Assessment of Micro- and Nano-Grained Commercial Pure Titanium in H2SO4 Solutions

NASA Astrophysics Data System (ADS)

Fattah-alhosseini, Arash; Ansari, Ali Reza; Mazaheri, Yousef; Karimi, Mohsen

2017-02-01

In this study, the electrochemical behavior of commercial pure titanium with both coarse-grained (annealed sample with the average grain size of about 45 µm) and nano-grained microstructure was compared by potentiodynamic polarization, electrochemical impedance spectroscopy (EIS), and Mott-Schottky analysis. Nano-grained Ti, which typically has a grain size of about 90 nm, is successfully made by six-cycle accumulative roll-bonding process at room temperature. Potentiodynamic polarization plots and impedance measurements revealed that as a result of grain refinement, the passive behavior of the nano-grained sample was improved compared to that of annealed pure Ti in H2SO4 solutions. Mott-Schottky analysis indicated that the passive films behaved as n-type semiconductors in H2SO4 solutions and grain refinement did not change the semiconductor type of passive films. Also, Mott-Schottky analysis showed that the donor densities decreased as the grain size of the samples reduced. Finally, all electrochemical tests showed that the electrochemical behavior of the nano-grained sample was improved compared to that of annealed pure Ti, mainly due to the formation of thicker and less defective oxide film.

Mechanistic Prediction of the Effect of Microstructural Coarsening on Creep Response of SnAgCu Solder Joints

NASA Astrophysics Data System (ADS)

Mukherjee, S.; Chauhan, P.; Osterman, M.; Dasgupta, A.; Pecht, M.

2016-07-01

Mechanistic microstructural models have been developed to capture the effect of isothermal aging on time dependent viscoplastic response of Sn3.0Ag0.5Cu (SAC305) solders. SnAgCu (SAC) solders undergo continuous microstructural coarsening during both storage and service because of their high homologous temperature. The microstructures of these low melting point alloys continuously evolve during service. This results in evolution of creep properties of the joint over time, thereby influencing the long term reliability of microelectronic packages. It is well documented that isothermal aging degrades the creep resistance of SAC solder. SAC305 alloy is aged for (24-1000) h at (25-100)°C (~0.6-0.8 × T melt). Cross-sectioning and image processing techniques were used to periodically quantify the effect of isothermal aging on phase coarsening and evolution. The parameters monitored during isothermal aging include size, area fraction, and inter-particle spacing of nanoscale Ag3Sn intermetallic compounds (IMCs) and the volume fraction of micronscale Cu6Sn5 IMCs, as well as the area fraction of pure tin dendrites. Effects of microstructural evolution on secondary creep constitutive response of SAC305 solder joints were then modeled using a mechanistic multiscale creep model. The mechanistic phenomena modeled include: (1) dispersion strengthening by coarsened nanoscale Ag3Sn IMCs in the eutectic phase; and (2) load sharing between pro-eutectic Sn dendrites and the surrounding coarsened eutectic Sn-Ag phase and microscale Cu6Sn5 IMCs. The coarse-grained polycrystalline Sn microstructure in SAC305 solder was not captured in the above model because isothermal aging does not cause any significant change in the initial grain size and orientation of SAC305 solder joints. The above mechanistic model can successfully capture the drop in creep resistance due to the influence of isothermal aging on SAC305 single crystals. Contribution of grain boundary sliding to the creep strain of coarse grained joints has not been modeled in this study.

Microstructural Characterization of Friction Stir Welded Aluminum-Steel Joints

NASA Astrophysics Data System (ADS)

Patterson, Erin E.; Hovanski, Yuri; Field, David P.

2016-06-01

This work focuses on the microstructural characterization of aluminum to steel friction stir welded joints. Lap weld configuration coupled with scribe technology used for the weld tool have produced joints of adequate quality, despite the significant differences in hardness and melting temperatures of the alloys. Common to friction stir processes, especially those of dissimilar alloys, are microstructural gradients including grain size, crystallographic texture, and precipitation of intermetallic compounds. Because of the significant influence that intermetallic compound formation has on mechanical and ballistic behavior, the characterization of the specific intermetallic phases and the degree to which they are formed in the weld microstructure is critical to predicting weld performance. This study used electron backscatter diffraction, energy dispersive spectroscopy, scanning electron microscopy, and Vickers micro-hardness indentation to explore and characterize the microstructures of lap friction stir welds between an applique 6061-T6 aluminum armor plate alloy and a RHA homogeneous armor plate steel alloy. Macroscopic defects such as micro-cracks were observed in the cross-sectional samples, and binary intermetallic compound layers were found to exist at the aluminum-steel interfaces of the steel particles stirred into the aluminum weld matrix and across the interfaces of the weld joints. Energy dispersive spectroscopy chemical analysis identified the intermetallic layer as monoclinic Al3Fe. Dramatic decreases in grain size in the thermo-mechanically affected zones and weld zones that evidenced grain refinement through plastic deformation and recrystallization. Crystallographic grain orientation and texture were examined using electron backscatter diffraction. Striated regions in the orientations of the aluminum alloy were determined to be the result of the severe deformation induced by the complex weld tool geometry. Many of the textures observed in the weld zone and thermo-mechanically affected zones exhibited shear texture components; however, there were many textures that deviated from ideal simple shear. Factors affecting the microstructure which are characteristic of the friction stir welding process, such as post-recrystallization deformation and complex deformation induced by tool geometry were discussed as causes for deviation from simple shear textures.

High-performance formamidinium-based perovskite solar cells via microstructure-mediated δ-to-α phase transformation

DOE PAGES

Liu, Tanghao; Zong, Yingxia; Zhou, Yuanyuan; ...

2017-03-14

The δ → α phase transformation is a crucial step in the solution-growth process of formamidinium-based lead triiodide (FAPbI 3) hybrid organic–inorganic perovskite (HOIP) thin films for perovskite solar cells (PSCs). Because the addition of cesium (Cs) stabilizes the α phase of FAPbI 3-based HOIPs, here our research focuses on FAPbI 3(Cs) thin films. We show that having a large grain size in the δ-FAPbI 3(Cs) non-perovskite intermediate films is essential for the growth of high-quality α-FAPbI 3(Cs) HOIP thin films. Here grain coarsening and phase transformation occur simultaneously during the thermal annealing step. A large starting grain size inmore » the δ-FAPbI 3(Cs) thin films suppresses grain coarsening, precluding the formation of voids at the final α-FAPbI 3(Cs)–substrate interfaces. PSCs based on the interface void-free α-FAPbI 3(Cs) HOIP thin films are much more efficient and stable in the ambient atmosphere. This interesting finding inspired us to develop a simple room-temperature aging method for preparing coarse-grained δ-FAPbI 3(Cs) intermediate films, which are subsequently converted to coarse-grained, high-quality α-FAPbI 3(Cs) HOIP thin films. As a result, this study highlights the importance of microstructure meditation in the processing of formamidinium-based PSCs.« less

Effect of initial grain size on inhomogeneous plastic deformation and twinning behavior in high manganese austenitic steel with a polycrystalline microstructure

NASA Astrophysics Data System (ADS)

Ueji, R.; Tsuchida, N.; Harada, K.; Takaki, K.; Fujii, H.

2015-08-01

The grain size effect on the deformation twinning in a high manganese austenitic steel which is so-called TWIP (twining induced plastic deformation) steel was studied in order to understand how to control deformation twinning. The 31wt%Mn-3%Al-3% Si steel was cold rolled and annealed at various temperatures to obtain fully recrystallized structures with different mean grain sizes. These annealed sheets were examined by room temperature tensile tests at a strain rate of 10-4/s. The coarse grained sample (grain size: 49.6μm) showed many deformation twins and the deformation twinning was preferentially found in the grains in which the tensile axis is parallel near to [111]. On the other hand, the sample with finer grains (1.8 μm) had few grains with twinning even after the tensile deformation. The electron back scattering diffraction (EB SD) measurements clarified the relationship between the anisotropy of deformation twinning and that of inhomogeneous plastic deformation. Based on the EBSD analysis, the mechanism of the suppression of deformation twinning by grain refinement was discussed with the concept of the slip pattern competition between the slip system governed by a grain boundary and that activated by the macroscopic load.

Polarization and microstructural effects of ceramic hydroxyapatite electrets

NASA Astrophysics Data System (ADS)

Tanaka, Yumi; Iwasaki, Takeshi; Nakamura, Miho; Nagai, Akiko; Katayama, Keiichi; Yamashita, Kimihiro

2010-01-01

To provide bioelectrets with controlled electrical energy, the polarization and relaxation characteristics of hydroxyapatite (HA) ceramic electrets were investigated in terms of poling conditions and microstructures. HA electrets were prepared between 250 and 500 °C for 5-120 min under a 5 kV cm-1 dc electrical field. Poling conditions and grain size of HA ceramics significantly influenced the thermally stimulated depolarization current (TSDC) spectra and charge storage (Q). Under a poling field of 5 kV cm-1, varying the poling temperature from 250 to 500 °C drastically shifted the TSDC peak temperature from 250 to 620 °C and increased Q from 0.5 to 45 μC cm-2. The change in the average grain size from 2 to 11 μm increased the Q value from 15 to 60 μC cm-2 with a negligible shift in the TSDC peak position. The measured difference of the TSDC peak shapes and positions, as well as the Q values, was theoretically due to the four polarization states with different activation energies (Edr) of dipole relaxation and the pre-exponential factor of relaxation times (τ0). The dependences on the poling conditions and grain size indicated that the four states were due to the orientation polarization of absorbed water (state 1), the localizations of displaced protons around PO43- and OH- in the grains (states 2 and 3), and the localization of displaced protons in the grain boundaries (state 4).

Modeling the microstructural changes during hot tandem rolling of AA5 XXX aluminum alloys: Part I. Microstructural evolution

NASA Astrophysics Data System (ADS)

Wells, M. A.; Samarasekera, I. V.; Brimacombe, J. K.; Hawbolt, E. B.; Lloyd, D. J.

1998-06-01

A comprehensive mathematical model of the hot tandem rolling process for aluminum alloys has been developed. Reflecting the complex thermomechanical and microstructural changes effected in the alloys during rolling, the model incorporated heat flow, plastic deformation, kinetics of static recrystallization, final recrystallized grain size, and texture evolution. The results of this microstructural engineering study, combining computer modeling, laboratory tests, and industrial measurements, are presented in three parts. In this Part I, laboratory measurements of static recrystallization kinetics and final recrystallized grain size are described for AA5182 and AA5052 aluminum alloys and expressed quantitatively by semiempirical equations. In Part II, laboratory measurements of the texture evolution during static recrystallization are described for each of the alloys and expressed mathematically using a modified form of the Avrami equation. Finally, Part III of this article describes the development of an overall mathematical model for an industrial aluminum hot tandem rolling process which incorporates the microstructure and texture equations developed and the model validation using industrial data. The laboratory measurements for the microstructural evolution were carried out using industrially rolled material and a state-of-the-art plane strain compression tester at Alcan International. Each sample was given a single deformation and heat treated in a salt bath at 400 °C for various lengths of time to effect different levels of recrystallization in the samples. The range of hot-working conditions used for the laboratory study was chosen to represent conditions typically seen in industrial aluminum hot tandem rolling processes, i.e., deformation temperatures of 350 °C to 500 °C, strain rates of 0.5 to 100 seconds and total strains of 0.5 to 2.0. The semiempirical equations developed indicated that both the recrystallization kinetics and the final recrystallized grain size were dependent on the deformation history of the material i.e., total strain and Zener-Hollomon parameter ( Z), where Z = dot \\varepsilon exp left( {{Q_{def} }/{RT_{def }}} right) and time at the recrystallization temperature.

Role of grain-size in phyllonitisation: Insights from mineralogy, microstructures, strain analyses and numerical modeling

NASA Astrophysics Data System (ADS)

Bose, Narayan; Dutta, Dripta; Mukherjee, Soumyajit

2018-07-01

Brittle Y- and P-planes exist in an exposure of greywacke in the Garhwal Lesser Himalaya, India. Although, Y-planes are well developed throughout, the P-planes are prominent only in some parts (domain-A), and not elsewhere (domain-B). To investigate why the P-planes developed selectively, the following studies were undertaken: 1. Clay-separated XRD analyses: clinochlore and illite are present in both the domains. 2. Strain analyses by Rf-φ method: it deduces strain magnitudes of ∼1.8 for the ductile deformed quartz grains from both the domains A and B. 3. Grain size analyses of quartz clasts: domain-A is mostly composed of finer grains (area up to 40,000 μm2), whereas domain-B consists of a population of coarser grains (area >45,000 μm2). A 2D finite element modeling of linear elastic material was performed using COMSOL software to investigate the control of grain-size variation on the generation brittle shear planes. The results of numerical modeling corroborate the known fact that an increase in grain-size reduces the elastic strain energy density. A broader grain-size distribution increases the effects of diffusion creep and resists the onset of dislocation creep. Thus, rocks with coarser grain population (domain B) tend to resist the generation of shear fractures, unlike their fine-grained counterpart (domain A).

Computational prediction of probabilistic ignition threshold of pressed granular Octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) under shock loading

NASA Astrophysics Data System (ADS)

Kim, Seokpum; Miller, Christopher; Horie, Yasuyuki; Molek, Christopher; Welle, Eric; Zhou, Min

2016-09-01

The probabilistic ignition thresholds of pressed granular Octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine explosives with average grain sizes between 70 μm and 220 μm are computationally predicted. The prediction uses material microstructure and basic constituent properties and does not involve curve fitting with respect to or prior knowledge of the attributes being predicted. The specific thresholds predicted are James-type relations between the energy flux and energy fluence for given probabilities of ignition. Statistically similar microstructure sample sets are computationally generated and used based on the features of micrographs of materials used in actual experiments. The predicted thresholds are in general agreement with measurements from shock experiments in terms of trends. In particular, it is found that grain size significantly affects the ignition sensitivity of the materials, with smaller sizes leading to lower energy thresholds required for ignition. For example, 50% ignition threshold of the material with an average grain size of 220 μm is approximately 1.4-1.6 times that of the material with an average grain size of 70 μm in terms of energy fluence. The simulations account for the controlled loading of thin-flyer shock experiments with flyer velocities between 1.5 and 4.0 km/s, constituent elasto-viscoplasticity, fracture, post-fracture contact and friction along interfaces, bulk inelastic heating, interfacial frictional heating, and heat conduction. The constitutive behavior of the materials is described using a finite deformation elasto-viscoplastic formulation and the Birch-Murnaghan equation of state. The ignition thresholds are determined via an explicit analysis of the size and temperature states of hotspots in the materials and a hotspot-based ignition criterion. The overall ignition threshold analysis and the microstructure-level hotspot analysis also lead to the definition of a macroscopic ignition parameter (J) and a microscopic ignition risk parameter (R) which are statistically related. The relationships between these parameters are established and delineated.

Nano/ultrafine grained austenitic stainless steel through the formation and reversion of deformation-induced martensite: Mechanisms, microstructures, mechanical properties, and TRIP effect

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

A comprehensive study was carried out on the strain-induced martensitic transformation, its reversion to austenite, the resultant grain refinement, and the enhancement of strength and strain-hardening ability through the transformation-induced plasticity (TRIP) effect in a commercial austenitic 304L stainless steel with emphasis on the mechanisms and the microstructural evolution. A straightforward magnetic measurement device, which is based on the measurement of the saturation magnetization, for evaluating the amount of strain-induced martensite after cold rolling and reversion annealing in metastable austenitic stainless steels was used, which its results were in good consistency with those of the X-ray diffraction (XRD) method. Amore » new parameter called the effective reduction in thickness was introduced, which corresponds to the reasonable upper bound on the obtainable martensite fraction based on the saturation in the martensitic transformation. By means of thermodynamics calculations, the reversion mechanisms were estimated and subsequently validated by experimental results. The signs of thermal martensitic transformation at cooling stage after reversion at 850 °C were found, which was attributed to the rise in the martensite start temperature due to the carbide precipitation. After the reversion treatment, the average grain sizes were around 500 nm and the nanometric grains of the size of ~ 65 nm were also detected. The intense grain refinement led to the enhanced mechanical properties and observation of the change in the work-hardening capacity and TRIP effect behavior. A practical map as a guidance for grain refining and characterizing the stability against grain growth was proposed, which shows the limitation of the reversion mechanism for refinement of grain size. - Graphical abstract: Display Omitted - Highlights: • Nano/ultrafine grained austenitic stainless steel through martensite treatment • A parameter descriptive of a reasonable upper bound on the obtainable martensite • Characterization of martensite by virtue of a new developed magnetic device • Investigation of mechanical properties and TRIP effect and the effect of grain size.« less

Ultrasound scatter in heterogeneous 3D microstructures: Parameters affecting multiple scattering

NASA Astrophysics Data System (ADS)

Engle, B. J.; Roberts, R. A.; Grandin, R. J.

2018-04-01

This paper reports on a computational study of ultrasound propagation in heterogeneous metal microstructures. Random spatial fluctuations in elastic properties over a range of length scales relative to ultrasound wavelength can give rise to scatter-induced attenuation, backscatter noise, and phase front aberration. It is of interest to quantify the dependence of these phenomena on the microstructure parameters, for the purpose of quantifying deleterious consequences on flaw detectability, and for the purpose of material characterization. Valuable tools for estimation of microstructure parameters (e.g. grain size) through analysis of ultrasound backscatter have been developed based on approximate weak-scattering models. While useful, it is understood that these tools display inherent inaccuracy when multiple scattering phenomena significantly contribute to the measurement. It is the goal of this work to supplement weak scattering model predictions with corrections derived through application of an exact computational scattering model to explicitly prescribed microstructures. The scattering problem is formulated as a volume integral equation (VIE) displaying a convolutional Green-function-derived kernel. The VIE is solved iteratively employing FFT-based con-volution. Realizations of random microstructures are specified on the micron scale using statistical property descriptions (e.g. grain size and orientation distributions), which are then spatially filtered to provide rigorously equivalent scattering media on a length scale relevant to ultrasound propagation. Scattering responses from ensembles of media representations are averaged to obtain mean and variance of quantities such as attenuation and backscatter noise levels, as a function of microstructure descriptors. The computational approach will be summarized, and examples of application will be presented.

Novel superconducting phases of Tl-based compounds

NASA Technical Reports Server (NTRS)

Kostadinov, I. Z.; Mateev, M.; Michov, M.; Skumriev, V.; Tsakin, E.

1991-01-01

Researchers report the measurements of the I(sub c)(T) of the 102 K phase. They also discuss briefly the composition of the lattice parameters and the ac susceptibility relation to the grain size and microstructure.

Microstructural modification of pure Mg for improving mechanical and biocorrosion properties.

PubMed

Ahmadkhaniha, D; Järvenpää, A; Jaskari, M; Sohi, M Heydarzadeh; Zarei-Hanzaki, A; Fedel, M; Deflorian, F; Karjalainen, L P

2016-08-01

In this study, the effect of microstructural modification on mechanical properties and biocorrosion resistance of pure Mg was investigated for tailoring a load-bearing orthopedic biodegradable implant material. This was performed utilizing the friction stir processing (FSP) in 1-3 passes to refine the grain size. Microstructure was examined in an optical microscope and scanning electron microscope with an electron backscatter diffraction unit. X-ray diffraction method was used to identify the texture. Mechanical properties were measured by microhardness and tensile testing. Electrochemical impedance spectroscopy was applied to evaluate corrosion behavior. The results indicate that even applying a single pass of FSP refined the grain size significantly. Increasing the number of FSP passes further refined the structure, increased the mechanical strength and intensified the dominating basal texture. The best combination of mechanical properties and corrosion resistance were achieved after three FSP passes. In this case, the yield strength was about six times higher than that of the as-cast Mg and the corrosion resistance was also improved compared to that in the as-cast condition. Copyright © 2016 Elsevier Ltd. All rights reserved.

Development of nano/sub-micron grain structures in metastable austenitic stainless steels

NASA Astrophysics Data System (ADS)

Rajasekhara, Shreyas

2007-12-01

This dissertation is a part of a collaborative work between the University of Texas, Austin-Texas, the University of Oulu, Oulu-Finland, and Outokumpu Stainless Oy, Tornio-Finland, to develop commercial austenitic stainless steels with high strength and ductility. The idea behind this work involves cold-rolling a commercial metastable austenitic stainless steel - AISI 301LN stainless steel to produce strain-induced martensite, followed by an annealing treatment to generate nano/sub-micron grained austenite. AISI 301LN stainless steel sheets are cold-rolled to 63% reduction and subsequently annealed at 600°C, 700°C, 800°C, 900°C and 1000°C for 1, 10 and 100 seconds. The samples are analyzed by X-Ray diffraction, SQUID, transmission electron microscopy, and tensile testing to fundamentally understand the microstructural evolution, the mechanism for the martensite → austenite reversion, the formation of nano/sub-micron austenite grains, and the relationship between the microstructure and the strength obtained in this stainless steel. The results show that cold-rolled AISI 301LN stainless steel consist of dislocation-cell martensite, heavily deformed lath-martensite and austenite shear bands. Subsequent annealing at 600°C for short durations of 1 and 10 seconds leads to negligible martensite to austenite reversion. These 600°C samples exhibit a similar microstructure to the cold-rolled sample. However, for samples annealed at 600°C for 100 seconds and those annealed at higher temperatures (700°C, 800°C, 900°C and 1000°C) exhibit equiaxed austenitic grains of sizes 0.2mum-10mum and secondary phase precipitates. The microstructural analysis also reveals that the martensite → austenite reversion occurs via a diffusion-type reversion mechanism. In this regard, a generalized form of Avrami's equation is used to model the kinetics of martensite → austenite phase reversion. The results from the model agree reasonably well with the experiments. Furthermore, the activation energy for grain growth in nano/sub-micron grained AISI 301LN stainless steel is found to be ˜ 205kJ/mol, which is comparable to values observed in coarse grained commercial stainless steels (AISI 304, 316). However, the driving force for grain growth in nano/sub-micron grained AISI 301LN stainless steel is considerably higher when compared to other stainless steels. Finally, the average grain sizes in AISI 301LN stainless steels are related to the mechanical properties obtained, through the Hall-Petch relationship.

Effect of Process Variables on the Grain Size and Crystallographic Texture of Hot-Dip Galvanized Coatings

NASA Astrophysics Data System (ADS)

Kaboli, Shirin; McDermid, Joseph R.

2014-08-01

A galvanizing simulator was used to determine the effect of galvanizing bath antimony (Sb) content, substrate surface roughness, and cooling rate on the microstructural development of metallic zinc coatings. Substrate surface roughness was varied through the use of relatively rough hot-rolled and relatively smooth bright-rolled steels, cooling rates were varied from 0.1 to 10 K/s, and bulk bath Sb levels were varied from 0 to 0.1 wt pct. In general, it was found that increasing bath Sb content resulted in coatings with a larger grain size and strongly promoted the development of coatings with the close-packed {0002} basal plane parallel to the substrate surface. Increasing substrate surface roughness tended to decrease the coating grain size and promoted a more random coating crystallographic texture, except in the case of the highest Sb content bath (0.1 wt pct Sb), where substrate roughness had no significant effect on grain size except at higher cooling rates (10 K/s). Increased cooling rates tended to decrease the coating grain size and promote the {0002} basal orientation. Calculations showed that increasing the bath Sb content from 0 to 0.1 wt pct Sb increased the dendrite tip growth velocity from 0.06 to 0.11 cm/s by decreasing the solid-liquid interface surface energy from 0.77 to 0.45 J/m2. Increased dendrite tip velocity only partially explains the formation of larger zinc grains at higher Sb levels. It was also found that the classic nucleation theory cannot completely explain the present experimental observations, particularly the effect of increasing the bath Sb, where the classical theory predicts increased nucleation and a finer grain size. In this case, the "poisoning" theory of nucleation sites by segregated Sb may provide a partial explanation. However, any analysis is greatly hampered by the lack of fundamental thermodynamic information such as partition coefficients and surface energies and by a lack of fundamental structural studies. Overall, it was concluded that the fundamental mechanisms behind the microstructural development of solidified metallic zinc coatings have yet to be completely elucidated and require further investigation.

Reliability Evaluation of Base-Metal-Electrode (BME) Multilayer Ceramic Capacitors for Space Applications

NASA Technical Reports Server (NTRS)

Liu, David (Donghang)

2011-01-01

This paper reports reliability evaluation of BME ceramic capacitors for possible high reliability space-level applications. The study is focused on the construction and microstructure of BME capacitors and their impacts on the capacitor life reliability. First, the examinations of the construction and microstructure of commercial-off-the-shelf (COTS) BME capacitors show great variance in dielectric layer thickness, even among BME capacitors with the same rated voltage. Compared to PME (precious-metal-electrode) capacitors, BME capacitors exhibit a denser and more uniform microstructure, with an average grain size between 0.3 and approximately 0.5 micrometers, which is much less than that of most PME capacitors. The primary reasons that a BME capacitor can be fabricated with more internal electrode layers and less dielectric layer thickness is that it has a fine-grained microstructure and does not shrink much during ceramic sintering. This results in the BME capacitors a very high volumetric efficiency. The reliability of BME and PME capacitors was investigated using highly accelerated life testing (HALT) and regular life testing as per MIL-PRF-123. Most BME capacitors were found to fail· with an early dielectric wearout, followed by a rapid wearout failure mode during the HALT test. When most of the early wearout failures were removed, BME capacitors exhibited a minimum mean time-to-failure of more than 10(exp 5) years. Dielectric thickness was found to be a critical parameter for the reliability of BME capacitors. The number of stacked grains in a dielectric layer appears to play a significant role in determining BME capacitor reliability. Although dielectric layer thickness varies for a given rated voltage in BME capacitors, the number of stacked grains is relatively consistent, typically between 10 and 20. This may suggest that the number of grains per dielectric layer is more critical than the thickness itself for determining the rated voltage and the life expectancy of the BME capacitor. Since BME capacitors have a much smaller grain size than PME capacitors, it is reasonable to predict that BME capacitors with thinner dielectric layers may have an equivalent life expectancy to that of PME capacitors with thicker dielectric layers.

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 numerical multi-scale model to predict macroscopic material anisotropy of multi-phase steels from crystal plasticity material definitions

NASA Astrophysics Data System (ADS)

Ravi, Sathish Kumar; Gawad, Jerzy; Seefeldt, Marc; Van Bael, Albert; Roose, Dirk

2017-10-01

A numerical multi-scale model is being developed to predict the anisotropic macroscopic material response of multi-phase steel. The embedded microstructure is given by a meso-scale Representative Volume Element (RVE), which holds the most relevant features like phase distribution, grain orientation, morphology etc., in sufficient detail to describe the multi-phase behavior of the material. A Finite Element (FE) mesh of the RVE is constructed using statistical information from individual phases such as grain size distribution and ODF. The material response of the RVE is obtained for selected loading/deformation modes through numerical FE simulations in Abaqus. For the elasto-plastic response of the individual grains, single crystal plasticity based plastic potential functions are proposed as Abaqus material definitions. The plastic potential functions are derived using the Facet method for individual phases in the microstructure at the level of single grains. The proposed method is a new modeling framework and the results presented in terms of macroscopic flow curves are based on the building blocks of the approach, while the model would eventually facilitate the construction of an anisotropic yield locus of the underlying multi-phase microstructure derived from a crystal plasticity based framework.

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.

Effects of substrate microstructure on the formation of oriented oxide nanotube arrays on Ti and Ti alloys

NASA Astrophysics Data System (ADS)

Ferreira, C. P.; Gonçalves, M. C.; Caram, R.; Bertazzoli, R.; Rodrigues, C. A.

2013-11-01

The formation of nanotubular oxide layers on Ti and Ti alloys has been widely investigated for the photocatalytic degradation of organic compounds due to their excellent catalytic efficiency, chemical stability, and low cost and toxicity. Aiming to improve the photocatalytic efficiency of this nanostructured oxide, this work investigated the influence of substrate grain size on the growth of nanotubular oxide layers. Ti and Ti alloys (Ti-6Al, Ti-6Al-7Nb) were produced by arc melting with non-consumable tungsten electrode and water-cooled copper hearth under argon atmosphere. Some of the ingots were heat-treated at 1000 °C for 12 and 24 h in argon atmosphere, followed by slow cooling rates to reduce crystalline defects and increase the grain size of their microstructures. Three types of samples were anodized: commercial substrate, as-prepared and heat-treated samples. The anodization was performed using fluoride solution and a cell potential of 20 V. The samples were characterized by optical microscopy, field-emission scanning electron microscopy and X-ray diffraction. The heat treatment preceding the anodization process increased the grain size of pure Ti and Ti alloys and promoted the formation of Widmanstätten structures in Ti6Al7Nb. The nanotubes layers grown on smaller grain and thermally untreated samples were more regular and homogeneous. In the case of Ti-6Al-7Nb alloy, which presents a α + β phase microstructure, the morphology of nanotubes nucleated on α matrix was more regular than those of nanotubes nucleated on β phase. After the annealing process, the Ti-6Al-7Nb alloy presented full diffusion process and the growth of equilibrium phases resulting in the appearance of regions containing higher concentrations of Nb, i.e. beta phase. In those regions the dissolution rate of Nb2O5 is lower than that of TiO2, resulting in a nanoporous layer. In general, heat treating reduces crystalline defects and promotes the increasing of the grain sizes, not favoring the process of nanotube nucleation and growth on the metallic surface.

Tailoring Magnetic Properties in Bulk Nanostructured Solids

NASA Astrophysics Data System (ADS)

Morales, Jason Rolando

Important magnetic properties and behaviors such as coercivity, remanence, susceptibility, energy product, and exchange coupling can be tailored by controlling the grain size, composition, and density of bulk magnetic materials. At nanometric length scales the grain size plays an increasingly important role since magnetic domain behavior and grain boundary concentration determine bulk magnetic behavior. This has spurred a significant amount of work devoted to developing magnetic materials with nanometric features (thickness, grain/crystallite size, inclusions or shells) in 0D (powder), 1D (wires), and 2D (thin films) materials. Large 3D nanocrystalline materials are more suitable for many applications such as permanent magnets, magneto-optical Faraday isolators etc. Yet there are relatively few successful demonstrations of 3D magnetic materials with nanoscale influenced properties available in the literature. Making dense 3D bulk materials with magnetic nanocrystalline microstructures is a challenge because many traditional densification techniques (HIP, pressureless sintering, etc.) move the microstructure out of the "nano" regime during densification. This dissertation shows that the Current Activated Pressure Assisted Densification (CAPAD) method, also known as spark plasma sintering, can be used to create dense, bulk, magnetic, nanocrystalline solids with varied compositions suited to fit many applications. The results of my research will first show important implications for the use of CAPAD for the production of exchange-coupled nanocomposite magnets. Decreases in grain size were shown to have a significant role in increasing the magnitude of exchange bias. Second, preferentially ordered bulk magnetic materials were produced with highly anisotropic material properties. The ordered microstructure resulted in changing magnetic property magnitudes (ex. change in coercivity by almost 10x) depending on the relative orientation (0° vs. 90°) of an externally applied magnetic field to the sample. Third, a dense magneto-optical material (rare earth oxide) was produced that rotates transmitted polarized light under an externally applied magnetic field, called the Faraday Effect. The magnitude of the rare earth oxide Faraday Effect surpasses that of the current market leader (terbium gallium garnet) in Faraday isolators by ˜2.24x.

Solution-mass transfer and grain boundary sliding in mafic shear zones - comparison between experiments and nature

NASA Astrophysics Data System (ADS)

Marti, Sina; Heilbronner, Renée; Stünitz, Holger; Plümper, Oliver; Drury, Martyn

2017-04-01

Grain size sensitive creep (GSSC) mechanisms are widely recognized to be the most efficient deformation mechanisms in shear zones. With or without initial fracturing and fluid infiltration, the onset of heterogeneous nucleation leading to strong grain size reduction is a frequently described process for the initiation of GSSC. Phase mixing due to reaction and heterogeneous nucleation during GSSC impedes grain growth, sustaining small grain sizes as a prerequisite for GSSC. Here we present rock deformation experiments on 'wet' plagioclase - pyroxene mixtures at T=800°C, P=1.0 and 1.5GPa and strain rates of 2e-5 - 2e-6 1/s, performed with a Griggs-type solid medium deformation apparatus. Microstructural criteria are used to show that both, grain boundary sliding (GBS) and solution-mass transfer processes are active and are interpreted to be the dominant strain accommodating processes. Displacement is localized within shear bands formed by fine-grained ( 300 - 500nm) plagioclase (Pl) and the syn-kinematic reaction products amphibole (Amph), quartz (Qz) and zoisite (Zo). We compare our experiments with a natural case - a sheared mafic pegmatite (P-T during deformation 0.7 - 0.9 GPa, 610 - 710 °C; Getsinger et al., 2013) from Northern Norway. Except for the difference in grain size of the experimental and natural samples, microstructures are strikingly alike. The experimental and natural P- and especially T-conditions are very similar. Consequently, extrapolation from experiments to nature must be made without a significant 'temperature-time' trade-off, which is normally taken advantage of when relating experimental to natural strain rates. We will discuss under which assumptions extrapolation to nature in our case is likely feasible. Syn-kinematic reactions during GBS and solution-mass transport are commonly interpreted to result in an ordered (anticlustered) phase mixture. However, phase mixing in our case is restricted: Mixing is extensive between Pl + Zo + Qz and Amph + Qz, but clustering is common between Pl + Amph. We present microstructural evidences, that phase mixing between Pl and Amph (the most abundant phases) is enhanced by the presence of quartz. Accordingly, quartz forming reactions or external sources (e.g. through fluid infiltration) may play a crucial role in deformation of mafic rocks, which has not been recognized thus far. Getsinger, A.J., Hirth, G., Stünitz, H., Goergen, E.T., 2013. The Influence of Water on Rheology and Strain Localization in the Lower Continental Crust. Geochemistry Geophysics Geosystems 14, 2247 - 2264.

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.

Pressure-induced stiffness of Au nanoparticles to 71 GPa under quasi-hydrostatic loading

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

Hong, Xinguo; Duffy, Thomas S.; Ehm, Lars

2015-11-16

The compressibility of nanocrystalline gold (n-Au, 20 nm) has been studied by x-ray total scattering using high-energy monochromatic x-rays in the diamond anvil cell under quasi-hydrostatic conditions up to 71 GPa. The bulk modulus, K 0, of the n-Au obtained from fitting to a Vinet equation of state is ~196(3) GPa, which is about 17% higher than for the corresponding bulk materials (K 0: 167 GPa). At low pressures (<7 GPa), the compression behavior of n-Au shows little difference from that of bulk Au. With increasing pressure, the compressive behavior of n-Au gradually deviates from the equation of state (EOS)more » of bulk gold. Analysis of the pair distribution function, peak broadening and Rietveld refinement reveals that the microstructure of n-Au is nearly a single-grain/domain at ambient conditions, but undergoes substantial pressure-induced reduction in grain size until 10 GPa. The results indicate that the nature of the internal microstructure in n-Au is associated with the observed EOS difference from bulk Au at high pressure. Full-pattern analysis confirms that significant changes in grain size, stacking faults, grain orientation and texture occur in n-Au at high pressure. We have observed direct experimental evidence of a transition in compressional mechanism for n-Au at ~20 GPa, i.e. from a deformation dominated by nucleation and motion of lattice dislocations (dislocation-mediated) to a prominent grain boundary mediated response to external pressure. In conclusion, the internal microstructure inside the nanoparticle (nanocrystallinity) plays a critical role for the macro-mechanical properties of nano-Au.« less

Pressure-induced stiffness of Au nanoparticles to 71 GPa under quasi-hydrostatic loading.

PubMed

Hong, Xinguo; Duffy, Thomas S; Ehm, Lars; Weidner, Donald J

2015-12-09

The compressibility of nanocrystalline gold (n-Au, 20 nm) has been studied by x-ray total scattering using high-energy monochromatic x-rays in the diamond anvil cell under quasi-hydrostatic conditions up to 71 GPa. The bulk modulus, K0, of the n-Au obtained from fitting to a Vinet equation of state is ~196(3) GPa, which is about 17% higher than for the corresponding bulk materials (K0: 167 GPa). At low pressures (<7 GPa), the compression behavior of n-Au shows little difference from that of bulk Au. With increasing pressure, the compressive behavior of n-Au gradually deviates from the equation of state (EOS) of bulk gold. Analysis of the pair distribution function, peak broadening and Rietveld refinement reveals that the microstructure of n-Au is nearly a single-grain/domain at ambient conditions, but undergoes substantial pressure-induced reduction in grain size until 10 GPa. The results indicate that the nature of the internal microstructure in n-Au is associated with the observed EOS difference from bulk Au at high pressure. Full-pattern analysis confirms that significant changes in grain size, stacking faults, grain orientation and texture occur in n-Au at high pressure. We have observed direct experimental evidence of a transition in compressional mechanism for n-Au at ~20 GPa, i.e. from a deformation dominated by nucleation and motion of lattice dislocations (dislocation-mediated) to a prominent grain boundary mediated response to external pressure. The internal microstructure inside the nanoparticle (nanocrystallinity) plays a critical role for the macro-mechanical properties of nano-Au.

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.

Shear-Coupled Grain Growth and Texture Development in a Nanocrystalline Ni-Fe Alloy during Cold Rolling

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

Li, Li; Ungár, Tamás; Toth, Laszlo S.

The evolution of texture, grain size, grain shape, dislocation and twin density has been determined by synchrotron X-ray diffraction and line profile analysis in a nanocrystalline Ni- Fe alloy after cold rolling along different directions related to the initial fiber and the long axis of grains. The texture evolution has been simulated by the Taylor-type relaxed constraints viscoplastic polycrystal model. The simulations were based on the activity of partial dislocations in correlation with the experimental results of dislocation density determination. The concept of stress-induced shear-coupling is supported and strengthened by both the texture simulations and the experimentally determined evolution ofmore » the microstructure parameters. Grain-growth and texture evolution are shown to proceed by the shear-coupling mechanism supported by dislocation activity as long as the grain size is not smaller than about 20 nm.« less

A new insight into high-strength Ti62Nb12.2Fe13.6Co6.4Al5.8 alloys with bimodal microstructure fabricated by semi-solid sintering

PubMed Central

Liu, L. H.; Yang, C.; Kang, L. M.; Qu, S. G.; Li, X. Q.; Zhang, W. W.; Chen, W. P.; Li, Y. Y.; Li, P. J.; Zhang, L. C.

2016-01-01

It is well known that semi-solid forming could only obtain coarse-grained microstructure in a few alloy systems with a low melting point, such as aluminum and magnesium alloys. This work presents that semi-solid forming could also produce novel bimodal microstructure composed of nanostructured matrix and micro-sized (CoFe)Ti2 twins in a titanium alloy, Ti62Nb12.2Fe13.6Co6.4Al5.8. The semi-solid sintering induced by eutectic transformation to form a bimodal microstructure in Ti62Nb12.2Fe13.6Co6.4Al5.8 alloy is a fundamentally different approach from other known methods. The fabricated alloy exhibits high yield strength of 1790 MPa and plastic strain of 15.5%. The novel idea provides a new insight into obtaining nano-grain or bimodal microstructure in alloy systems with high melting point by semi-solid forming and into fabricating high-performance metallic alloys in structural applications. PMID:27029858

Deformation mechanisms in experimentally deformed Boom Clay

NASA Astrophysics Data System (ADS)

Desbois, Guillaume; Schuck, Bernhard; Urai, Janos

2016-04-01

Bulk mechanical and transport properties of reference claystones for deep disposal of radioactive waste have been investigated since many years but little is known about microscale deformation mechanisms because accessing the relevant microstructure in these soft, very fine-grained, low permeable and low porous materials remains difficult. Recent development of ion beam polishing methods to prepare high quality damage free surfaces for scanning electron microscope (SEM) is opening new fields of microstructural investigation in claystones towards a better understanding of the deformation behavior transitional between rocks and soils. We present results of Boom Clay deformed in a triaxial cell in a consolidated - undrained test at a confining pressure of 0.375 MPa (i.e. close to natural value), with σ1 perpendicular to the bedding. Experiments stopped at 20 % strain. As a first approximation, the plasticity of the sample can be described by a Mohr-Coulomb type failure envelope with a coefficient of cohesion C = 0.117 MPa and an internal friction angle ϕ = 18.7°. After deformation test, the bulk sample shows a shear zone at an angle of about 35° from the vertical with an offset of about 5 mm. We used the "Lamipeel" method that allows producing a permanent absolutely plane and large size etched micro relief-replica in order to localize and to document the shear zone at the scale of the deformed core. High-resolution imaging of microstructures was mostly done by using the BIB-SEM method on key-regions identified after the "Lamipeel" method. Detailed BIB-SEM investigations of shear zones show the following: the boundaries between the shear zone and the host rock are sharp, clay aggregates and clastic grains are strongly reoriented parallel to the shear direction, and the porosity is significantly reduced in the shear zone and the grain size is smaller in the shear zone than in the host rock but there is no evidence for broken grains. Comparison of microstructures within the host rock and the undeformed sample shows that the sample underwent compaction prior shearing that results in a change of power law exponent of the pore size distribution within the clay matrix and a slight reorientation of clastic grains' long axis perpendicular to σ1. Microstructures in the shear zone indicate ductile behavior before the specimen's failure. Deformation mechanisms are bending of clay plates and sliding along clay-clay contacts. Strain is strongly localised in thin, anastomosing zones of strong preferred orientation, producing slickensided shear surfaces common in shallow clays. There is no evidence for intragranular cracking.We propose that the deformation localizes in regions without hard quartz grains.

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.

Influence of Solution Treatment Duration on Microstructural Features of an Industrial Forged UNS S32750/1.4410/F53 Super Duplex Stainless Steel (SDSS) Alloy

NASA Astrophysics Data System (ADS)

Cojocaru, Vasile Dănuţ; Răducanu, Doina; Angelescu, Mariana Lucia; Vintilă, Adrian Nicolae; Şerban, Nicolae; Dan, Ioan; Cojocaru, Elisabeta Mirela; Cinca, Ion

2017-08-01

The microstructural changes induced by solution treatment of an industrial forged F53 Super Duplex Stainless Steel alloy were studied, in order to emphasize how component phases are influenced by heat treatment temperature and duration. The solution treatment was done at a temperature of 1100°C, with variable holding times: 0.6 ks (10 min), 3.6 ks (60 min) and 10.8 ks (180 min). Scanning electron microscopy-electron backscattered diffraction was used as main characterization technique, to obtain and analyse data referring to microstructural features, such as: nature and morphology of constituent phases, average grain-size and grain misorientation. It was shown that in all studied cases the microstructure consisted of a mixture of about 45% δ-Fe (ferrite) and 55% γ-Fe (austenite). Besides δ-Fe and γ-Fe phases, other phases were also identified, such as τ-phase (chromium-iron carbide), σ-phase (chromium-iron) and δ-(Cr-Fe) (ferrite).

Interface-Driven Phenomena in Solids: Thermodynamics, Kinetics and Chemistry

DOE PAGES

Abdeljawad, Fadi; Foiles, Stephen M.

2016-05-04

The study of materials interfaces dates back over a century. In solid systems and from an engineering perspective, free surfaces and internal (grain and/or phase) boundaries influence a wide range of properties, such as thermal, electrical and optical transport, and mechanical ones. The properties and the role of interfaces has been discussed extensively in various reviews such as by Sutton and Balluffi. As the characteristic feature size of a materials system (i.e., grain size) is decreased to the nanometer scale, interface-driven physics is expected to dominate due to the increased density of such planar defects. Moreover, interfacial attributes, thermodynamics, andmore » mobility play a key role in phase transformations, such as solidification dynamics and structural transitions in solids, and in homogenization and microstructural evolution processes, such as grain growth, coarsening, and recrystallization. In summary, the set of articles published in this special topic titled: “Interface-Driven Phenomena in Solids: Thermodynamics, Kinetics and Chemistry” covers topics related to microstructure evolution, segregation/adsorption phenomena and interface interactions with other materials defects.« less

Interface-Driven Phenomena in Solids: Thermodynamics, Kinetics and Chemistry

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

Abdeljawad, Fadi; Foiles, Stephen M.

The study of materials interfaces dates back over a century. In solid systems and from an engineering perspective, free surfaces and internal (grain and/or phase) boundaries influence a wide range of properties, such as thermal, electrical and optical transport, and mechanical ones. The properties and the role of interfaces has been discussed extensively in various reviews such as by Sutton and Balluffi. As the characteristic feature size of a materials system (i.e., grain size) is decreased to the nanometer scale, interface-driven physics is expected to dominate due to the increased density of such planar defects. Moreover, interfacial attributes, thermodynamics, andmore » mobility play a key role in phase transformations, such as solidification dynamics and structural transitions in solids, and in homogenization and microstructural evolution processes, such as grain growth, coarsening, and recrystallization. In summary, the set of articles published in this special topic titled: “Interface-Driven Phenomena in Solids: Thermodynamics, Kinetics and Chemistry” covers topics related to microstructure evolution, segregation/adsorption phenomena and interface interactions with other materials defects.« less

Influence of microstructure and surface topography on the electrical conductivity of Cu and Ag thin films obtained by magnetron sputtering

NASA Astrophysics Data System (ADS)

Polonyankin, D. A.; Blesman, A. I.; Postnikov, D. V.

2017-05-01

Conductive thin films formation by copper and silver magnetron sputtering is one of high technological areas for industrial production of solar energy converters, energy-saving coatings, flat panel displays and touch control panels because of their high electrical and optical properties. Surface roughness and porosity, average grain size, internal stresses, orientation and crystal lattice type, the crystallinity degree are the main physical properties of metal films affecting their electrical resistivity and conductivity. Depending on the film thickness, the dominant conduction mechanism can affect bulk conductivity due to the flow of electron gas, and grain boundary conductivity. The present investigation assesses the effect of microstructure and surface topography on the electrical conductivity of magnetron sputtered Cu and Ag thin films using X-ray diffraction analysis, scanning electron and laser interference microscopy. The highest specific conductivity (78.3 MS m-1 and 84.2 MS m-1, respectively, for copper and silver films at the thickness of 350 nm) were obtained with the minimum values of roughness and grain size as well as a high degree of lattice structuredness.

Flame-resistant Ca-containing AZ31 magnesium alloy sheets with good mechanical properties fabricated by a combination of strip casting and high-ratio differential speed rolling methods

NASA Astrophysics Data System (ADS)

Kim, Y. H.; Kim, W. J.

2015-03-01

This study reported that a combination of strip casting and high-ratio differential speed rolling (HRDSR) can produce flame-resistant Mg alloy sheets (0.7 wt%Ca-AZ31: 0.7Ca-AZ31) with good room-temperature mechanical properties and high-temperature formability. HRDSR effectively refined the coarse microstructure of the strip-casting processed 0.7Ca-AZ31 alloy. As the result, the (true) grain size was reduced to as small as 2.7 μm and the (Mg, Al)2Ca phase was broken up to fine particles with an average sizes of 0.5 μm. Due to the advantage of having such a highly refined microstructure, the HRDSR-processed 0.7Ca-AZ31 alloy sheet exhibited a high yield stress over 300 MPa and good superplasticity at elevated temperatures. The deformation mechanism of the fine-grained 0.7Ca-AZ31 alloy in the superplastic regime was identified to be grainboundary-diffusion or lattice-diffusion controlled grain boundary sliding.

Optimization of mechanical strength of titania fibers fabricated by direct drawing

NASA Astrophysics Data System (ADS)

Hanschmidt, Kelli; Tätte, Tanel; Hussainova, Irina; Part, Marko; Mändar, Hugo; Roosalu, Kaspar; Chasiotis, Ioannis

2013-11-01

Nanostructured polycrystalline titania (TiO2) microfibers were produced by direct drawing from visco-elastic alkoxide precursors. The fiber crystallinity and grain size were shown to depend on post-treatment calcination temperature. Tensile tests with individual fibers showed strong sensitivity of the elastic modulus and the tensile strength to microstructural details of the fibers. The elastic modulus of as-fabricated fibers increased about 10 times after calcination at 700 ∘C, while the strain at failure remained almost the same at ˜1.4 %. The highest tensile strength of more than 800 MPa was exhibited by nanoscale grained fibers with a bimodal grain size distribution consisting of rutile grains embedded into an anatase matrix. This structure is believed to have reduced the critical defect size, and thus increased the tensile strength. The resultant fibers showed properties that were appropriate for reinforcement of different matrixes.

Microstructures of Ni-AlN composite coatings prepared by pulse electrodeposition technology

NASA Astrophysics Data System (ADS)

Xia, Fafeng; Xu, Huibin; Liu, Chao; Wang, Jinwu; Ding, Junjie; Ma, Chunhua

2013-04-01

Ni-AlN composite coating was fabricated onto the surface of steel substrates by using pulse electrodeposition (PED) technique in this work. The effect of pulse current on the nucleation and growth of grains was investigated using transmission electronic microscopy (TEM), X-ray diffraction (XRD), scanning electronic microscopy (SEM) and atomic force microscopy (AFM), respectively. The results show that the contents of AlN nanoparticles increase with density of pulse current and on-duty ratio of pulse current increasing. Whereas the size of nickel grains decreases with density of pulse current increasing and on-duty ratio of pulse current decreasing. Ni-AlN composite coating consists of crystalline nickel (˜68 nm) and AlN particles (˜38 nm). SEM and AFM observations show that the composite coatings obtained by PED showed more compact surfaces and less grain sizes, whereas those obtained by direct current electrodepositing have rougher surfaces and bigger grain sizes.

Collaborative Research and Development (CR&D). Delivery Order 0031: Basic Research and Development of Ti-B Alloys

DTIC Science & Technology

2006-09-01

September 2005 Abstract The grain size of as-cast Ti- 6Al - 4V is reduced by about an order of magnitude from 1700 to 200 /lm with an addition of 0.1 wt...and enhances subsequent mechanical working response [l J. The grain sizes of conventional cast titanium alloys (e.g, Ti-6AI- 4V ) are rather coarse...microstructure; Serial sectioning 1. Introduction The addition of boron to titanium alloys such as Ti­ 6AI- 4V can significantly enhance their strength

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

El-Atwani, Osman; Nathaniel II, James E.; Leff, Asher C.

Nanocrystalline materials are radiation-tolerant materials’ candidates due to their high defect sink density. Here, nanocrystalline iron films were irradiated with 10 keV helium ions in situ in a transmission electron microscope at elevated temperatures. Grain-size-dependent bubble density changes and denuded zone occurrence were observed at 700 K, but not at 573 K. This transition, attributed to increased helium–vacancy migration at elevated temperatures, suggests that nanocrystalline microstructures are more resistant to swelling at 700 K due to decreased bubble density. Finally, denuded zone formation had no correlation with grain size and misorientation angle under the conditions studied.

International Conference (4th) on Nanostructured Materials Held in Stockholm, Sweden on 14-19 June 1998. Special Volume - Part A. Volume 12, Numbers 1-4, 1999

DTIC Science & Technology

1998-06-19

correlation was found between the X - ray grain size and the TEM grain size. Table 2 contains the hardness and density data for the nanocrystalline 5083...temperature with a Neophot hardness tester and a load of 0.2 N. RESULTS AND DISCUSSION X - ray diffraction and transmission electron microscopy combined with...For Single- Wall Carbon Nanotubes by Raman Scattering Technique Microstructure Change in Co46AI19035 Granular Thin Films by Annealing X - Ray

Microstructural design in low alloy steels

NASA Technical Reports Server (NTRS)

Honeycombe, R. W. K.

1982-01-01

The evolution of microalloyed steels from plain carbon steels is examined with emphasis on grain size control by use of Nb, Ti and V additions and by the application of controlled rolling. The structural changes during controlled rolling are described as well as the influence of alloying elements on these changes, and on the final microstructure. The achievement of high strength and toughness is discussed including the role of inclusions.

Simultaneous Strength-Ductility Enhancement of a Nano-Lamellar AlCoCrFeNi2.1 Eutectic High Entropy Alloy by Cryo-Rolling and Annealing.

PubMed

Bhattacharjee, T; Wani, I S; Sheikh, S; Clark, I T; Okawa, T; Guo, S; Bhattacharjee, P P; Tsuji, N

2018-02-19

Nano-lamellar (L1 2  + B2) AlCoCrFeNi 2.1 eutectic high entropy alloy (EHEA) was processed by cryo-rolling and annealing. The EHEA developed a novel hierarchical microstructure featured by fine lamellar regions consisting of FCC lamellae filled with ultrafine FCC grains (average size ~200-250 nm) and B2 lamellae, and coarse non-lamellar regions consisting of ultrafine FCC (average size ~200-250 nm), few coarse recrystallized FCC grains and rather coarse unrecrystallized B2 phase (~2.5 µm). This complex and hierarchical microstructure originated from differences in strain-partitioning amongst the constituent phases, affecting the driving force for recrystallization. The hierarchical microstructure of the cryo-rolled and annealed material resulted in simultaneous enhancement in strength (Yield Strength/YS: 1437 ± 26 MPa, Ultimate Tensile Strength/UTS: 1562 ± 33 MPa) and ductility (elongation to failure/e f  ~ 14 ± 1%) as compared to the as-cast as well as cold-rolled and annealed materials. The present study for the first time demonstrated that cryo-deformation and annealing could be a novel microstructural design strategy for overcoming strength-ductility trade off in multiphase high entropy alloys.

Effect of Zn addition on bulk microstructure of lead-free solder SN100C

NASA Astrophysics Data System (ADS)

Nur Nadirah M., K.; Nurulakmal M., S.

2017-12-01

This paper reports the effect of adding Zn (0.5 wt% Zn, 1.0 wt% Zn) to the bulk microstructure and intermetallic compound (IMC) formation of commercial SN100C (Sn-0.7Cu-0.05Ni+Ge) lead-free solder alloy. Solder alloys were prepared by melting SN100C ingot and Zn shots, and subsequently casted into steel mold. Samples were ground and polished for XRF, and polished samples were then etched for microstructure analysis. Microstructure of bulk solder and the IMC were observed using SEM equipped with EDX. SEM result showed the addition of 0.5 wt% Zn resulted in increased grain size of β-Sn matrix but further addition of Zn (1 wt%) reduced the size of β-Sn dendrites in the bulk solder. Several intermetallic compounds (IMCs) were observed distributed in the Sn matrix; Cu-Zn, Ni-Zn and Cu-Zn-Ni IMC but in relatively small percentage compared to Cu-Zn and Ni-Zn. These particles could be considered as effective nucleating agent that led to finer β-Sn grains. It is expected that the finer β-Sn will contribute towards higher solder strength and the various IMCs present could act as suppressant for Sn diffusion which will then tend to reduce the IMC growth during thermal aging.

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.

Microstructure Analysis of Bismuth Absorbers for Transition-Edge Sensor X-ray Microcalorimeters

NASA Astrophysics Data System (ADS)

Yan, Daikang; Divan, Ralu; Gades, Lisa M.; Kenesei, Peter; Madden, Timothy J.; Miceli, Antonino; Park, Jun-Sang; Patel, Umeshkumar M.; Quaranta, Orlando; Sharma, Hemant; Bennett, Douglas A.; Doriese, William B.; Fowler, Joseph W.; Gard, Johnathon D.; Hays-Wehle, James P.; Morgan, Kelsey M.; Schmidt, Daniel R.; Swetz, Daniel S.; Ullom, Joel N.

2018-03-01

Given its large X-ray stopping power and low specific heat capacity, bismuth (Bi) is a promising absorber material for X-ray microcalorimeters and has been used with transition-edge sensors (TESs) in the past. However, distinct X-ray spectral features have been observed in TESs with Bi absorbers deposited with different techniques. Evaporated Bi absorbers are widely reported to have non-Gaussian low-energy tails, while electroplated ones do not show this feature. In this study, we fabricated Bi absorbers with these two methods and performed microstructure analysis using scanning electron microscopy and X-ray diffraction microscopy. The two types of material showed the same crystallographic structure, but the grain size of the electroplated Bi was about 40 times larger than that of the evaporated Bi. This distinction in grain size is likely to be the cause of their different spectral responses.

Mechanical properties and microstructures of China low activation martensitic steel compared with JLF-1

NASA Astrophysics Data System (ADS)

Li, Y.; Huang, Q.; Wu, Y.; Nagasaka, T.; Muroga, T.

2007-08-01

The tensile and impact properties of CLAM steel are compared to those of JLF-1 steel. Tensile testing revealed that the ultimate and yield strengths of the CLAM steel are 670 MPa and 512 MPa at room temperature, and 373 MPa and 327 MPa at 873 K, respectively. These values are higher than those measured for JLF-1. The ductile-to-brittle transition temperature (DBTT) of CLAM was found to be 171 K using one-third size Charpy V-notch specimens, which is 16 K lower than that of JLF-1. Microstructural analysis by SEM and TEM indicated that the prior austenite grain size and lath width for CLAM are smaller than those for JLF-1. The finer grain and lath structure is considered to be one of the main reasons for the higher strength and lower DBTT of the CLAM steel.

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.

DISFRAC Version 2.0 Users Guide

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

Cochran, Kristine B; Erickson, Marjorie A; Williams, Paul T

2013-01-01

DISFRAC is the implementation of a theoretical, multi-scale model for the prediction of fracture toughness in the ductile-to-brittle transition temperature (DBTT) region of ferritic steels. Empirically-derived models of the DBTT region cannot legitimately be extrapolated beyond the range of existing fracture toughness data. DISFRAC requires only tensile properties and microstructural information as input, and thus allows for a wider range of application than empirical, toughness data dependent models. DISFRAC is also a framework for investigating the roles of various microstructural and macroscopic effects on fracture behavior, including carbide particle sizes, grain sizes, strain rates, and material condition. DISFRAC s novelmore » approach is to assess the interaction effects of macroscopic conditions (geometry, loading conditions) with variable microstructural features on cleavage crack initiation and propagation. The model addresses all stages of the fracture process, from microcrack initiation within a carbide particle, to propagation of that crack through grains and across grain boundaries, finally to catastrophic failure of the material. The DISFRAC procedure repeatedly performs a deterministic analysis of microcrack initiation and propagation within a macroscopic crack plastic zone to calculate a critical fracture toughness value for each microstructural geometry set. The current version of DISFRAC, version 2.0, is a research code for developing and testing models related to cleavage fracture and transition toughness. The various models and computations have evolved significantly over the course of development and are expected to continue to evolve as testing and data collection continue. This document serves as a guide to the usage and theoretical foundations of DISFRAC v2.0. Feedback is welcomed and encouraged.« less

Nondestructive ultrasonic characterization of armor grade silicon carbide

NASA Astrophysics Data System (ADS)

Portune, Andrew Richard

Ceramic materials have traditionally been chosen for armor applications for their superior mechanical properties and low densities. At high strain rates seen during ballistic events, the behavior of these materials relies upon the total volumetric flaw concentration more so than any single anomalous flaw. In this context flaws can be defined as any microstructural feature which detriments the performance of the material, potentially including secondary phases, pores, or unreacted sintering additives. Predicting the performance of armor grade ceramic materials depends on knowledge of the absolute and relative concentration and size distribution of bulk heterogeneities. Ultrasound was chosen as a nondestructive technique for characterizing the microstructure of dense silicon carbide ceramics. Acoustic waves interact elastically with grains and inclusions in large sample volumes, and were well suited to determine concentration and size distribution variations for solid inclusions. Methodology was developed for rapid acquisition and analysis of attenuation coefficient spectra. Measurements were conducted at individual points and over large sample areas using a novel technique entitled scanning acoustic spectroscopy. Loss spectra were split into absorption and scattering dominant frequency regimes to simplify analysis. The primary absorption mechanism in polycrystalline silicon carbide was identified as thermoelastic in nature. Correlations between microstructural conditions and parameters within the absorption equation were established through study of commercial and custom engineered SiC materials. Nonlinear least squares regression analysis was used to estimate the size distributions of boron carbide and carbon inclusions within commercial SiC materials. This technique was shown to additionally be capable of approximating grain size distributions in engineered SiC materials which did not contain solid inclusions. Comparisons to results from electron microscopy exhibited favorable agreement between predicted and observed distributions. Developed techniques were applied to large sample areas using scanning acoustic spectroscopy to map variations in the size distribution and concentration of grains and solid inclusions within the bulk microstructure. The experiments performed in this thesis form the foundation of a novel characterization technique capable of mapping variations in sample composition which could be extended to a wide range of dense polycrystalline heterogeneous materials.

Grain size effect on Lcr elastic wave for surface stress measurement of carbon steel

NASA Astrophysics Data System (ADS)

Liu, Bin; Miao, Wenbing; Dong, Shiyun; He, Peng

2018-04-01

Based on critical refraction longitudinal wave (Lcr wave) acoustoelastic theory, correction method for grain size effect on surface stress measurement was discussed in this paper. Two fixed distance Lcr wave transducers were used to collect Lcr wave, and difference in time of flight between Lcr waves was calculated with cross-correlation coefficient function, at last relationship of Lcr wave acoustoelastic coefficient and grain size was obtained. Results show that as grain size increases, propagation velocity of Lcr wave decreases, one cycle is optimal step length for calculating difference in time of flight between Lcr wave. When stress value is within stress turning point, relationship of difference in time of flight between Lcr wave and stress is basically consistent with Lcr wave acoustoelastic theory, while there is a deviation and it is higher gradually as stress increasing. Inhomogeneous elastic plastic deformation because of inhomogeneous microstructure and average value of surface stress in a fixed distance measured with Lcr wave were considered as the two main reasons for above results. As grain size increasing, Lcr wave acoustoelastic coefficient decreases in the form of power function, then correction method for grain size effect on surface stress measurement was proposed. Finally, theoretical discussion was verified by fracture morphology observation.

Micromechanics of pressure-induced grain crushing in porous rocks

NASA Astrophysics Data System (ADS)

Davis, Daniel M.

1990-01-01

The hydrostatic compaction behavior of a suite of porous sandstones was investigated at confining pressures up to 600 MPa and constant pore pressures ranging up to 50 MPa. These five sandstones (Boise, Kayenta, St. Peter, Berea, and Weber) were selected because of their wide range of porosity (5-35%) and grain size (60-460 μm). We tested the law of effective stress for the porosity change as a function of pressure. Except for Weber sandstone (which has the lowest porosity and smallest grain size), the hydrostat of each sandstone shows an inflection point corresponding to a critical effective pressure beyond which an accelerated, irrecoverable compaction occurs. Our microstructural observations show that brittle grain crushing initiates at this critical pressure. We also observed distributed cleavage cracking in calcite and intensive kinking in mica. The critical pressures for grain crushing in our sandstones range from 75 to 380 MPa. In general, a sandstone with higher porosity and larger grain size has a critical pressure which is lower than that of a sandstone with lower porosity and smaller grain size. We formulate a Hertzian fracture model to analyze the micromechanics of grain crushing. Assuming that the solid grains have preexisting microcracks with dimensions which scale with grain size, we derive an expression for the critical pressure which depends on the porosity, grain size, and fracture toughness of the solid matrix. The theoretical prediction is in reasonable agreement with our experimental data as well as other data from soil and rock mechanics studies for which the critical pressures range over 3 orders of magnitude.

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.

Tools for Material Design and Selection

NASA Astrophysics Data System (ADS)

Wehage, Kristopher

The present thesis focuses on applications of numerical methods to create tools for material characterization, design and selection. The tools generated in this work incorporate a variety of programming concepts, from digital image analysis, geometry, optimization, and parallel programming to data-mining, databases and web design. The first portion of the thesis focuses on methods for characterizing clustering in bimodal 5083 Aluminum alloys created by cryomilling and powder metallurgy. The bimodal samples analyzed in the present work contain a mixture of a coarse grain phase, with a grain size on the order of several microns, and an ultra-fine grain phase, with a grain size on the order of 200 nm. The mixing of the two phases is not homogeneous and clustering is observed. To investigate clustering in these bimodal materials, various microstructures were created experimentally by conventional cryomilling, Hot Isostatic Pressing (HIP), Extrusion, Dual-Mode Dynamic Forging (DMDF) and a new 'Gradient' cryomilling process. Two techniques for quantitative clustering analysis are presented, formulated and implemented. The first technique, the Area Disorder function, provides a metric of the quality of coarse grain dispersion in an ultra-fine grain matrix and the second technique, the Two-Point Correlation function, provides a metric of long and short range spatial arrangements of the two phases, as well as an indication of the mean feature size in any direction. The two techniques are implemented on digital images created by Scanning Electron Microscopy (SEM) and Electron Backscatter Detection (EBSD) of the microstructures. To investigate structure--property relationships through modeling and simulation, strategies for generating synthetic microstructures are discussed and a computer program that generates randomized microstructures with desired configurations of clustering described by the Area Disorder Function is formulated and presented. In the computer program, two-dimensional microstructures are generated by Random Sequential Adsorption (RSA) of voxelized ellipses representing the coarse grain phase. A simulated annealing algorithm is used to geometrically optimize the placement of the ellipses in the model to achieve varying user-defined configurations of spatial arrangement of the coarse grains. During the simulated annealing process, the ellipses are allowed to overlap up to a specified threshold, allowing triple junctions to form in the model. Once the simulated annealing process is complete, the remaining space is populated by smaller ellipses representing the ultra-fine grain phase. Uniform random orientations are assigned to the grains. The program generates text files that can be imported in to Crystal Plasticity Finite Element Analysis Software for stress analysis. Finally, numerical methods and programming are applied to current issues in green engineering and hazard assessment. To understand hazards associated with materials and select safer alternatives, engineers and designers need access to up-to-date hazard information. However, hazard information comes from many disparate sources and aggregating, interpreting and taking action on the wealth of data is not trivial. In light of these challenges, a Framework for Automated Hazard Assessment based on the GreenScreen list translator is presented. The framework consists of a computer program that automatically extracts data from the GHS-Japan hazard database, loads the data into a machine-readable JSON format, transforms the JSON document in to a GreenScreen JSON document using the GreenScreen List Translator v1.2 and performs GreenScreen Benchmark scoring on the material. The GreenScreen JSON documents are then uploaded to a document storage system to allow human operators to search for, modify or add additional hazard information via a web interface.

Fragments of deeper parts of the hanging wall mantle preserved as orogenic peridotites in the central belt of the Seve Nappe Complex, Sweden

NASA Astrophysics Data System (ADS)

Clos, Frediano; Gilio, Mattia; van Roermund, Herman L. M.

2014-04-01

Formation conditions of olivine microstructures are investigated in the Kittelfjäll spinel peridotite (KSP), a fragment of lithospheric mantle which occurs as an isolated body within high grade metamorphic crustal rocks of the Seve Nappe Complex (SNC), southern Västerbotten, central Sweden. The KSP is an orogenic peridotite containing a well developed penetrative compositional layering, defined by highly depleted dunite with olivine Mg# (100 × Mg/Mg + Fe) of 92.0-93.5 and harzburgite with lower Mg# (91.0-92.5). Dunite is characterized by three contrasting olivine microstructures formed in response to different tectonometamorphic events: Coarse-grained, highly strained olivine porphyroclasts (M1) up to 20 cm long are surrounded by dynamically recrystallized olivine grains (M2) defining a characteristic olivine "foam" microstructure (grain size: 200-2000 μm). An olivine "mortar" (M3) microstructure (10-50 μm) forms a penetrative fabric element only in strongly localized, cm-to-m sized shear zones that crosscut earlier structures/foliations. Olivine fabric analysis in synergy, with mineralogical and chemical analyses, reveals that the KSP body represents old, possibly Archean, sub-continental lithospheric mantle that was crustally emplaced into the Caledonian tectonic edifice from the hanging wall mantle during exhumation of the subducted Seve Nappe Complex (Jämtlandian orogeny ~ 454 Ma). Olivine porphyroclasts (M1) grew at high temperature during dominant isobaric cooling after extensive polybaric melt extraction (> 40%) and subsequent refertilization. The onset of the early Caledonian deformation is interpreted to be related to the crustal emplacement of the KSP during eduction of the SNC. This phase is characterized by the development of the olivine M2 foam microstructure, formed at 650-830 °C/1-2 GPa by dislocation creep processes producing an E-type CPO's by the operation of the [100](001) and subordinate [001](100) slip systems with operating flow stress levels around 8-48 MPa. In contrast the M3 olivine "mortar" microstructure formed at 550-600 °C/0.45-0.6 GPa and represents deformation after the subducted slab had returned to shallow crustal levels. It is proposed here that the presence of a penetrative olivine M2 "foam" microstructure can be used as an easy tool in the field to discriminate between mantle wedge (i.e. sub-continental affinity), ophiolite (i.e. sub-oceanic affinity), and/or hyper-extensional peridotite in the Scandinavian Caledonides. The latter two peridotite subtypes may have similar M2 microstructures, but exclusively restricted to the structural base of the bodies. Alternatively in basal parts of ophiolites, M3 microstructures directly overprint coarser grained proto-granular olivine microstructures.

Control of Microstructures and the Practical Properties of API X80 Grade Heavy-Wall High-Frequency Electric Resistance-Welded Pipe with Excellent Low-Temperature Toughness

NASA Astrophysics Data System (ADS)

Goto, Sota; Nakata, Hiroshi; Toyoda, Shunsuke; Okabe, Takatoshi; Inoue, Tomohiro

2017-10-01

This paper describes development of heavy-walled API X80 grade high-frequency electric resistance-welded (HFW) line pipes and conductor-casing pipes with wall thicknesses up to 20.6 mm. A fine bainitic-ferrite microstructure, which is preferable for low-temperature toughness, was obtained by optimizing the carbon content and applying the thermomechanical controlled hot-rolling process. As a result, the Charpy ductile-brittle transition temperature (DBTT) was well below 227 K (-46 °C) in the base metal of the HFW line pipe. When the controlled hot-rolling ratio (CR) was increased from 23 to 48 pct, the area average grain size decreased from 15 to 8 μm. The dependence of CTOD properties on CR was caused by the largest grain which is represented by the area average grain size. No texture development due to the increase of CR from 23 to 48 pct was observed. In addition, because controlled in-line heat treatment of the longitudinal weld seam also produced the fine bainitic-ferrite microstructure at the weld seam, DBTT was lower than 227 K (-46 °C) at the weld portion. The developed pipes showed good girth weldability without preheat treatment, and fracture in the tensile test initiated from the base metal in all cases.

Mechanical Properties and Microstructure of AZ31B Magnesium Alloy Processed by I-ECAP

NASA Astrophysics Data System (ADS)

Gzyl, Michal; Rosochowski, Andrzej; Pesci, Raphael; Olejnik, Lech; Yakushina, Evgenia; Wood, Paul

2014-03-01

Incremental equal channel angular pressing (I-ECAP) is a severe plastic deformation process used to refine grain size of metals, which allows processing very long billets. As described in the current article, an AZ31B magnesium alloy was processed for the first time by three different routes of I-ECAP, namely, A, BC, and C, at 523 K (250 °C). The structure of the material was homogenized and refined to ~5 microns of the average grain size, irrespective of the route used. Mechanical properties of the I-ECAPed samples in tension and compression were investigated. Strong influence of the processing route on yield and fracture behavior of the material was established. It was found that texture controls the mechanical properties of AZ31B magnesium alloy subjected to I-ECAP. SEM and OM techniques were used to obtain microstructural images of the I-ECAPed samples subjected to tension and compression. Increased ductility after I-ECAP was attributed to twinning suppression and facilitation of slip on basal plane. Shear bands were revealed in the samples processed by I-ECAP and subjected to tension. Tension-compression yield stress asymmetry in the samples tested along extrusion direction was suppressed in the material processed by routes BC and C. This effect was attributed to textural development and microstructural homogenization. Twinning activities in fine- and coarse-grained samples have also been studied.

Quasi-static Tensile and Compressive Behavior of Nanocrystalline Tantalum based on Miniature Specimen Testing—Part I: Materials Processing and Microstructure

NASA Astrophysics Data System (ADS)

Ligda, J.; Scotto D'Antuono, D.; Taheri, M. L.; Schuster, B. E.; Wei, Q.

2016-11-01

Grain size reduction of metals into ultrafine-grained (UFG, grain size 100 nm < d < 1000 nm) and nanocrystalline (NC, d < 100 nm) regimes results in considerable increase in strength along with other changes in mechanical behavior such as vanishing strain hardening and limited ductility. Severe plastic deformation (SPD) has been among the favored technologies for the fabrication of UFG/NC metals. Primary past research efforts on SPD UFG/NC metals have been focused on easy-to-work metals, especially face-centered cubic metals such as copper, nickel, etc., and the limited efforts on body-centered cubic metals have mainly focused on high strain rate behavior where these metals are shown to deform via adiabatic shear bands. Except for the work on Fe, only a few papers can be found associated with UFG/NC refractory metals. In the first part of the present work (Part I), high-pressure torsion (HPT) is used to process UFG/NC tantalum, a typical refractory metal. The microstructure of the HPT disk as a function of radial location as well as orientation will be examined. In the subsequent part (Part II), the location-specific mechanical behavior will be presented and discussed. It is suggested that refractory metals such as Ta are ideal to employ SPD technology for microstructure refinement because of the extremely high melting point and relatively good workability.

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

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

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

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

Microstructural and mechanical evolution during deformation and annealing of poly-phase marbles - constraints from laboratory experiments and field observations

NASA Astrophysics Data System (ADS)

Austin, N. J.; Evans, B.; Dresen, G. H.; Rybacki, E.

2009-12-01

Deformed rocks commonly consist of several mineral phases, each with dramatically different mechanical properties. In both naturally and experimentally deformed rocks, deformation mechanisms and, in turn, strength, are commonly investigated by analyzing microstructural elements such as crystallographic preferred orientation (CPO) and recrystallized grain size. Here, we investigated the effect of variations in the volume fraction and the geometry of rigid second phases on the strength and evolution of CPO and grain size of synthetic calcite rocks. Experiments using triaxial compression and torsional loading were conducted at 1023 K and equivalent strain rates between ~2e-6 and 1e-3 s-1. The second phases in these synthetic assemblages are rigid carbon spheres or splinters with known particle size distributions and geometries, which are chemically inert at our experimental conditions. Under hydrostatic conditions, the addition of as little as 1 vol.% carbon spheres poisons normal grain growth. Shape is also important: for an equivalent volume fraction and grain dimension, carbon splinters result in a finer calcite grain size than carbon spheres. In samples deformed at “high” strain rates, or which have “large” mean free spacing of the pinning phase, the final recrystallized grain size is well explained by competing grain growth and grain size reduction processes, where the grain-size reduction rate is determined by the rate that mechanical work is done during deformation. In these samples, the final grain size is finer than in samples heat-treated hydrostatically for equivalent durations. The addition of 1 vol.% spheres to calcite has little effect on either the strength or CPO development. Adding 10 vol.% splinters increases the strength at low strains and low strain rates, but has little effect on the strength at high strains and/or high strain rates, compared to pure samples. A CPO similar to that in pure samples is observed, although the intensity is reduced in samples containing 10 vol.% splinters. When 10 vol.% spheres are added to calcite, the strength of the aggregate is reduced, and a distinct and strong CPO develops. Viscoplastic self consistent calculations were used to model the evolution of CPO in these materials, and these suggest a variation in the activity of the various slip systems within pure samples and those containing 10 vol.% spheres. The applicability of these laboratory observations has been tested with field-based observations made in the Morcles Nappe (Swiss Helvetic Alps). In the Morcles Nappe, calcite grain size becomes progressively finer as the thrust contact is approached, and there is a concomitant increase in CPO intensity, with the strongest CPO’s in the finest-grained, quartz-rich limestones, nearest the thrust contact, which are interpreted to have been deformed to the highest strains. Thus, our laboratory results may be used to provide insight into the distribution of strain observed in natural shear zones.

Effect of thermo-mechanical treatments on the microstructure and mechanical properties of an ODS ferritic steel

NASA Astrophysics Data System (ADS)

Oksiuta, Z.; Mueller, P.; Spätig, P.; Baluc, N.

2011-05-01

The Fe-14Cr-2W-0.3Ti-0.3Y 2O 3 oxide dispersion strengthened (ODS) reduced activation ferritic (RAF) steel was fabricated by mechanical alloying of a pre-alloyed, gas atomised powder with yttria nano-particles, followed by hot isostatic pressing and thermo-mechanical treatments (TMTs). Two kinds of TMT were applied: (i) hot pressing, or (ii) hot rolling, both followed by annealing in vacuum at 850 °C. The use of a thermo-mechanical treatment was found to yield strong improvement in the microstructure and mechanical properties of the ODS RAF steel. In particular, hot pressing leads to microstructure refinement, equiaxed grains without texture, and an improvement in Charpy impact properties, especially in terms of the upper shelf energy (about 4.5 J). Hot rolling leads to elongated grains in the rolling direction, with a grain size ratio of 6:1, higher tensile strength and reasonable ductility up to 750 °C, and better Charpy impact properties, especially in terms of the ductile-to-brittle transition temperature (about 55 °C).

Three Dimensional Characterization of Tin Crystallography and Cu6Sn5 Intermetallics in Solder Joints by Multiscale Tomography

NASA Astrophysics Data System (ADS)

Kirubanandham, A.; Lujan-Regalado, I.; Vallabhaneni, R.; Chawla, N.

2016-11-01

Decreasing pitch size in electronic packaging has resulted in a drastic decrease in solder volumes. The Sn grain crystallography and fraction of intermetallic compounds (IMCs) in small-scale solder joints evolve much differently at the smaller length scales. A cross-sectional study limits the morphological analysis of microstructural features to two dimensions. This study utilizes serial sectioning technique in conjunction with electron backscatter diffraction to investigate the crystallographic orientation of both Sn grains and Cu6Sn5 IMCs in Cu/Pure Sn/Cu solder joints in three dimensional (3D). Quantification of grain aspect ratio is affected by local cooling rate differences within the solder volume. Backscatter electron imaging and focused ion beam serial sectioning enabled the visualization of morphology of both nanosized Cu6Sn5 IMCs and the hollow hexagonal morphology type Cu6Sn5 IMCs in 3D. Quantification and visualization of microstructural features in 3D thus enable us to better understand the microstructure and deformation mechanics within these small scale solder joints.

Reverse-transformation austenite structure control with micro/nanometer size

NASA Astrophysics Data System (ADS)

Wu, Hui-bin; Niu, Gang; Wu, Feng-juan; Tang, Di

2017-05-01

To control the reverse-transformation austenite structure through manipulation of the micro/nanometer grain structure, the influences of cold deformation and annealing parameters on the microstructure evolution and mechanical properties of 316L austenitic stainless steel were investigated. The samples were first cold-rolled, and then samples deformed to different extents were annealed at different temperatures. The microstructure evolutions were analyzed by optical microscopy, scanning electron microscopy (SEM), magnetic measurements, and X-ray diffraction (XRD); the mechanical properties are also determined by tensile tests. The results showed that the fraction of stain-induced martensite was approximately 72% in the 90% cold-rolled steel. The micro/nanometric microstructure was obtained after reversion annealing at 820-870°C for 60 s. Nearly 100% reversed austenite was obtained in samples annealed at 850°C, where grains with a diameter ≤ 500 nm accounted for 30% and those with a diameter > 0.5 μm accounted for 70%. The micro/nanometer-grain steel exhibited not only a high strength level (approximately 959 MPa) but also a desirable elongation of approximately 45%.

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.

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.

Stress in recrystallized quartz by electron backscatter diffraction mapping

NASA Astrophysics Data System (ADS)

Llana-Fúnez, S.

2017-07-01

The long-term state of stress at middle and lower crustal depths can be estimated through the study of the microstructure of exhumed rocks from active and/or ancient shear zones. Constitutive equations for deformation mechanisms in experimentally deformed rocks relate differential stress to the size of recrystallized grains. Cross et al. (2017) take advantage of electron backscatter diffraction mapping to systematically separate new recrystallized grains from host grains on the basis of the measurable lattice distorsion within the grains. They produce the first calibrated piezometer for quartz with this technique, reproducing within error a previous calibration based on optical microscopy.

Formation and characterization of metallic iron grains in coal-based reduction of oolitic iron ore

NASA Astrophysics Data System (ADS)

Sun, Yong-sheng; Han, Yue-xin; Li, Yan-feng; Li, Yan-jun

2017-02-01

To reveal the formation and characteristics of metallic iron grains in coal-based reduction, oolitic iron ore was isothermally reduced in various reduction times at various reduction temperatures. The microstructure and size of the metallic iron phase were investigated by scanning electron microscopy, energy-dispersive X-ray spectroscopy, and a Bgrimm process mineralogy analyzer. In the results, the reduced Fe separates from the ore and forms metallic iron protuberances, and then the subsequent reduced Fe diffuses to the protuberances and grows into metallic iron grains. Most of the metallic iron grains exist in the quasi-spherical shape and inlaid in the slag matrix. The cumulative frequency of metallic iron grain size is markedly influenced by both reduction time and temperature. With increasing reduction temperature and time, the grain size of metallic iron obviously increases. According to the classical grain growth equation, the growth kinetic parameters, i.e., time exponent, growth activation energy, and pre-exponential constant, are estimated to be 1.3759 ± 0.0374, 103.18 kJ·mol-1, and 922.05, respectively. Using these calculated parameters, a growth model is established to describe the growth behavior of metallic iron grains.

Kinetic model for thin film stress including the effect of grain growth

NASA Astrophysics Data System (ADS)

Chason, Eric; Engwall, A. M.; Rao, Z.; Nishimura, T.

2018-05-01

Residual stress during thin film deposition is affected by the evolution of the microstructure. This can occur because subsurface grain growth directly induces stress in the film and because changing the grain size at the surface affects the stress in new layers as they are deposited. We describe a new model for stress evolution that includes both of these effects. It is used to explain stress in films that grow with extensive grain growth (referred to as zone II) so that the grain size changes throughout the thickness of the layer as the film grows. Equations are derived for different cases of high or low atomic mobility where different assumptions are used to describe the diffusion of atoms that are incorporated into the grain boundary. The model is applied to measurements of stress and grain growth in evaporated Ni films. A single set of model parameters is able to explain stress evolution in films grown at multiple temperatures and growth rates. The model explains why the slope of the curvature measurements changes continuously with thickness and attributes it to the effect of grain size on new layers deposited on the film.

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

Processing, microstructure evolution and properties of nanoscale aluminum alloys

NASA Astrophysics Data System (ADS)

Han, Jixiong

In this project, phase transformations and precipitation behavior in age-hardenable nanoscale materials systems, using Al-Cu alloys as model materials, were first studied. The Al-Cu nanoparticles were synthesized by a Plasma Ablation process and found to contain a 2˜5 nm thick adherent aluminum oxide scale, which prevented further oxidation. On aging of the particles, a precipitation sequence consisting of, nearly pure Cu precipitates to the metastable theta' to equilibrium theta was observed, with all three forming along the oxide-particle interface. The structure of theta' and its interface with the Al matrix has been characterized in detail. Ultrafine Al-Cu nanoparticles (5˜25 nm) were also synthesized by inert gas condensation (IGC) and their aging behavior was studied. These particles were found to be quite stable against precipitation. Secondly, pure Al nanoparticles were prepared by the Exploding Wire process and their sintering and consolidation behavior were studied. It was found that nanopowders of Al could be processed to bulk structures with high hardness and density. Sintering temperature was found to have a dominant effect on density, hardness and microstructure. Sintering at temperatures >600°C led to breakup of the oxide scale, leading to an interesting nanocomposite composed of 100˜200 nm Al oxide dispersed in a bimodal nanometer-micrometer size Al matrix grains. Although there was some grain growth, the randomly dispersed oxide fragments were quite effective in pinning the Al grain boundaries, preventing excessive grain growth and retaining high hardness. Cold rolling and hot rolling were effective methods for attaining full densification and high hardness. Thirdly, the microstructure evolution and mechanical behavior of Al-Al 2O3 nanocomposites were studied. The composites can retain high strength at elevated temperature and thermal soaking has practically no detrimental effect on strength. Although the ductility of the composite remains quite low, there was substantial evidence for high localized plasticity. The strengthening mechanisms of the composite include: Orowan strengthening, grain size strengthening and Forest strengthening. Finally, the microstructure evolution and mechanical behavior of 2024Al-Al 2O3 nanocomposites were studied. This 2024Al-Al2O 3 composite exhibits similar thermal stability and high strength at elevated temperature as Al-Al2O3. On aging, the matrix of 2024Al-Al2O3 composites revealed a precipitation sequence of: alphaAl → GP/GPB → theta'/S' → theta/S. The strengthening mechanisms of the 2024Al-Al2O3 composites include precipitation strengthening, Orowan strengthening, grain size strengthening and Forest strengthening.

Evolution of microstructure, texture and inhibitor along the processing route for grain-oriented electrical steels using strip casting

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

Liu, Hai-Tao, E-mail: liuht@ral.neu.edu.cn; Institute of Research of Iron and Steel, Shasteel, Zhangjiagang 215625, Jiangsu; Yao, Sheng-Jie

2015-08-15

In the present work, a regular grade GO sheet was produced successively by strip casting, hot rolling, normalizing annealing, two-stage cold rolling with intermediate annealing, primary recrystallization annealing, secondary recrystallization annealing and purification. The aim of this paper was to characterize the evolution of microstructure, texture and inhibitor along the new processing route by comprehensive utilization of optical microscopy, X-ray diffraction and transmission electron microscopy. It was found that a fine microstructure with the ferrite grain size range of 7–12 μm could be obtained in the primary recrystallization annealed sheet though a very coarse microstructure was produced in the initialmore » as-cast strip. The main finding was that the “texture memory” effect on Goss texture started on the through-thickness intermediate annealed strip after first cold rolling, which was not similar to the “texture memory” effect on Goss texture starting on the surface layers of the hot rolled strip in the conventional production route. As a result, the origin of Goss nuclei capable of secondary recrystallization lied in the grains already presented in Goss orientation in the intermediate annealed strip after first cold rolling. Another finding was that fine and dispersive inhibitors (mainly AlN) were easy to be produced in the primary recrystallization microstructure due to the initial rapid solidification during strip casting and the subsequent rapid cooling, and the very high temperature reheating usually used before hot rolling in the conventional production route could be avoided. - Highlights: • A regular grade grain-oriented electrical steel was produced. • Evolution of microstructure, texture and inhibitor was characterized. • Origin of Goss nuclei lied in the intermediate annealed strip. • A fine primary recrystallization microstructure could be produced. • Effective inhibitors were easy to be obtained in the new processing route.« less

Magnetic properties and microstructure of gas atomized MRE2(Fe, Co)14B powder with ZrC addition (MRE=Nd + Y + Dy)

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

Tang, W.; Wu, Y. Q.; Dennis, K.

2009-05-12

Gas atomization powder with Zr substitutions for the MRE and ZrC additions were systematically studied. The results show that the partial substitutions of Zr and the ZrC additions effectively improved glass formability in the alloys. Scanning electron microscopy (SEM) revealed that the as-atomized powder with a particle size of less than 32 {micro}m is predominately uniform equiaxed grains with an average grain size of 1.5 {micro}m. X-ray diffraction and differential thermal analysis measurements detected very tiny amounts of amorphous phase. After annealing at 700 C for 15 min, the SEM grain microstructure exhibits a minor change, but magnetic properties aremore » substantially improved. M versus T measurements reveal that the phase composition evolved from 2:14:1 plus a small amount of 2:17 phases to a single 2:14:1 phase during the annealing process. The sieve analysis of the powders showed a particle size distribution with 90 wt % of the powder less than 45 {micro}m. The magnetic properties of the annealed powder varied with particle size. (BH){sub max} first increases with increasing particle size from 5 {micro}m, reaches the peak value in the size range of 20-25 {micro}m, and then decreases with increasing particle size. For the 20-25 {micro}m powder sample annealed at 700 C for 15 min, the (BH){sub max} of 9.6 MG Oe at room temperature and 5.6 MG Oe at 200 C were obtained, respectively.« less

Scaling ice microstructures from the laboratory to nature: cryo-EBSD on large samples.

NASA Astrophysics Data System (ADS)

Prior, David; Craw, Lisa; Kim, Daeyeong; Peyroux, Damian; Qi, Chao; Seidemann, Meike; Tooley, Lauren; Vaughan, Matthew; Wongpan, Pat

2017-04-01

Electron backscatter diffraction (EBSD) has extended significantly our ability to conduct detailed quantitative microstructural investigations of rocks, metals and ceramics. EBSD on ice was first developed in 2004. Techniques have improved significantly in the last decade and EBSD is now becoming more common in the microstructural analysis of ice. This is particularly true for laboratory-deformed ice where, in some cases, the fine grain sizes exclude the possibility of using a thin section of the ice. Having the orientations of all axes (rather than just the c-axis as in an optical method) yields important new information about ice microstructure. It is important to examine natural ice samples in the same way so that we can scale laboratory observations to nature. In the case of ice deformation, higher strain rates are used in the laboratory than those seen in nature. These are achieved by increasing stress and/or temperature and it is important to assess that the microstructures produced in the laboratory are comparable with those observed in nature. Natural ice samples are coarse grained. Glacier and ice sheet ice has a grain size from a few mm up to several cm. Sea and lake ice has grain sizes of a few cm to many metres. Thus extending EBSD analysis to larger sample sizes to include representative microstructures is needed. The chief impediments to working on large ice samples are sample exchange, limitations on stage motion and temperature control. Large ice samples cannot be transferred through a typical commercial cryo-transfer system that limits sample sizes. We transfer through a nitrogen glove box that encloses the main scanning electron microscope (SEM) door. The nitrogen atmosphere prevents the cold stage and the sample from becoming covered in frost. Having a long optimal working distance for EBSD (around 30mm for the Otago cryo-EBSD facility) , by moving the camera away from the pole piece, enables the stage to move without crashing into either the EBSD camera or the SEM pole piece (final lens). In theory a sample up to 100mm perpendicular to the tilt axis by 150mm parallel to the tilt axis can be analysed. In practice, the motion of our stage is restricted to maximum dimensions of 100 by 50mm by a conductive copper braid on our cold stage. Temperature control becomes harder as the samples become larger. If the samples become too warm then they will start to sublime and the quality of EBSD data will reduce. Large samples need to be relatively thin ( 5mm or less) so that conduction of heat to the cold stage is more effective at keeping the surface temperature low. In the Otago facility samples of up to 40mm by 40mm present little problem and can be analysed for several hours without significant sublimation. Larger samples need more care, e.g. fast sample transfer to keep the sample very cold. The largest samples we work on routinely are 40 by 60mm in size. We will show examples of EBSD data from glacial ice and sea ice from Antarctica and from large laboratory ice samples.

Loop and void damage during heavy ion irradiation on nanocrystalline and coarse grained tungsten: Microstructure, effect of dpa rate, temperature, and grain size

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

El-Atwani, O.; Esquivel, E.; Efe, M.

Displacement damage, through heavy ion irradiation was studied on two tungsten grades (coarse grained tungsten (CGW) and nanocrystalline and ultrafine grained tungsten (NCW)) using different displacement per atom rates and different irradiation temperatures (RT and 1050 K). Percentage of <111> and <100> type loops at the irradiation conditions was determined. Irradiation damage in the microstructure was quantified using average loop areas and densities (method A) and loop areal fraction in the grain matrices under 2-beam diffraction conditions (method B). Average values of <111> and <100> loops were calculated from method A. Loop coalescence was shown to occur for CGW atmore » 0.25 dpa. Using both methods of quantifying microstructural damage, no effect of dpa rate was observed and damage in CGW was shown to be the same at RT and 1050 K. Swelling from voids observed at 1050 K was quantified. The loop damage in NCW was compared to CGW at the same diffraction and imaging conditions. NCW was shown to possess enhanced irradiation resistance at RT regarding loop damage and higher swelling resistance at 1050 K compared to CGW. For irradiation at 1050 K, the NCW was shown to have a similar defect densities to the CGW which is attributed to higher surface effects in the CGW, vacancy loop growth to voids and a better sink efficiency in the CGW deduced from the vacancy distribution profiles from Kinetic Monte Carlo simulations. Loop density and swelling was shown to have similar values in grains sizes that range from 80-600 nm. No loop or void denuded zones occurred at any of the irradiation conditions. This work has a collection of experiments and conclusions that are of vital importance to materials and nuclear communities.« less

Loop and void damage during heavy ion irradiation on nanocrystalline and coarse grained tungsten: Microstructure, effect of dpa rate, temperature, and grain size

DOE PAGES

El-Atwani, O.; Esquivel, E.; Efe, M.; ...

2018-02-20

Displacement damage, through heavy ion irradiation was studied on two tungsten grades (coarse grained tungsten (CGW) and nanocrystalline and ultrafine grained tungsten (NCW)) using different displacement per atom rates and different irradiation temperatures (RT and 1050 K). Percentage of <111> and <100> type loops at the irradiation conditions was determined. Irradiation damage in the microstructure was quantified using average loop areas and densities (method A) and loop areal fraction in the grain matrices under 2-beam diffraction conditions (method B). Average values of <111> and <100> loops were calculated from method A. Loop coalescence was shown to occur for CGW atmore » 0.25 dpa. Using both methods of quantifying microstructural damage, no effect of dpa rate was observed and damage in CGW was shown to be the same at RT and 1050 K. Swelling from voids observed at 1050 K was quantified. The loop damage in NCW was compared to CGW at the same diffraction and imaging conditions. NCW was shown to possess enhanced irradiation resistance at RT regarding loop damage and higher swelling resistance at 1050 K compared to CGW. For irradiation at 1050 K, the NCW was shown to have a similar defect densities to the CGW which is attributed to higher surface effects in the CGW, vacancy loop growth to voids and a better sink efficiency in the CGW deduced from the vacancy distribution profiles from Kinetic Monte Carlo simulations. Loop density and swelling was shown to have similar values in grains sizes that range from 80-600 nm. No loop or void denuded zones occurred at any of the irradiation conditions. This work has a collection of experiments and conclusions that are of vital importance to materials and nuclear communities.« less

Equal Channel Angular Pressing (ECAP) and Its Application to Grain Refinement of Al-Zn-Mg-Cu Alloy

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

Tekeli, Sueleyman; Gueral, Ahmet

Microstructure of a metal can be considerably changed by severe plastic deformation techniques such as high pressure torsion, extrusion and equal-channel angular pressing (ECAP). Among these methods, ECAP is particularly attractive because it has a potential for introducing significant grain refinement and homogeneous microstructure into bulk materials. Typically, it reduces the grain size to the submicrometer level or even nanometer range and thus produces materials that are capable of exhibiting unusual mechanical properties. In the present study, a test unites for equal channel angular pressing was constructed and this system was used for Al-Zn-Mg-Cu alloy. After the optimization tests, itmore » was seen that the most effective lubricant for the dies was MoS{sub 2}, the pressing pressure was around 25-35 ton and the pressing speed was 2 mm/s. By using these parameters, the Al-Zn-Mg-Cu alloy was successfully ECAPed up to 14 passes at 200 deg. C using route C. After ECAP tests, the specimens were characterized by transmission electron microscope (TEM), hardness and macrostructural investigations. It was seen that the plastic deformation in the ECAPed specimens occurred from edge to the centre like whirlpool. In addition, the deformation intensity increased with increasing pass number. The grain size of the specimens effectively also decreased with increasing pass number. That is, while the grain size of unECAPed specimen was 10 {mu}m, this value decreased to 300 nm after 14 passes. At the beginning, while there was a banding tendency in the grains toward deformation direction, homogeneous and equiaxed grains were formed with increasing pass number. This grain refinement was as a result of an interaction between shear strain and thermal recovery during ECAP processing. Hardness measurements showed that the hardness values increased up to 4 passes, decreased effectively at 6th pass, again increased at 8th pass and after this pass, the hardness again decreased due to dynamic recrystallization.« less

Micromagnetic Modeling: a Tool for Studying Remanence in Magnetite

NASA Astrophysics Data System (ADS)

ter Maat, G. W.; Fabian, K.; Church, N. S.; McEnroe, S. A.

2017-12-01

Micromagnetic modeling is a useful tool in understanding magnetic particle behavior. The domain state of, and interaction between, particles is influenced by their shape, size and spacing. Rocks contain a collection of grains with varying geometries. This study presents models of true geometries obtained by dual-beam focused ion beam scanning electron microscopy (FIB-SEM). Using focused ion beam nanotomography (FIB-nT) the shape and size of individual grains and their spacing are accurately determined. The particle assemblages discussed here are basalts from the Stardalur volcano in Iceland. The main carrier of the magnetization is oxy-exsolved magnetite which contains extensive microstructures from the micron to nanometer scale. The complex morphologies vary in shape from spherical to elongated to sheet-like shapes with SD to PSD domain states. We investigate large oxy-exsolved magnetite grains as well as smaller oxy-exsolved dendritic grains. The obtained 3D volumes are modeled using finite element micromagnetics software MERRILL, to calculate magnetization structures. By modeling a full hysteresis loop we can observe the complete switching process and visualize the mechanism of the reversal of the magnetization. Micromagnetic simulation of hysteresis loops of grains with varying geometry and spacing shows the magnetization state of, and magnetostatic interaction between, different grains. From the simulations the remanence state of the modeled reconstructed geometry is obtained. Modeling the behavior of separate individual grains is compared with modeling assemblages of grains with varying spacing to study the effect of interaction. The use of realistic geometries of oxy-exsolved magnetite in micromagnetic models allows the examination of the influence of shape, size and spacing on the magnetic properties of single particles, and magnetostatic interactions between them.These parameters are varied and tested to find if there is an increase in remanence-carrying capacity. The use of modeling of the realistic representation of the widespread microstructures allow us to test proposed enhancement of remanence, and more stable paleomagnetic recorders.

Microstructure Characterization of Weakly Textured and Fine Grained AZ61 Sheet

NASA Astrophysics Data System (ADS)

Berman, T. D.; Donlon, W.; Hung, C. K.; Milligan, P.; Decker, R.; Pollock, T. M.; Jones, J. W.

Formability in magnesium alloy sheet is strongly limited by a strong basal texture in the as-rolled material, which is difficulty to remove by thermal processing. We introduce a new process to the control of texture by combining Thixomolding and Thermomechanical Processing (TTMP). Plates of AZ61L with a divorced β-Mg17Al12 eutectic are produced by Thixomolding, resulting in a non-textured, fine grained (2.8 µm) precursor. Sheet produced from the plate by single pass warm-rolling exhibits a weaker texture, and more isotropic tensile deformation than generally observed in AZ-series alloy sheet. Recrystallization annealing produces a further reduction in texture and average grain size (2.3 µm) and results in nearly isotropic room temperature deformation, a yield strength of 220 MPa, and an elongation of 23%. Particle stimulated nucleation of new grains by the β-phase during both dynamic and static recrystallization, is critical for achieving the low levels of texture. The influence of β-phase distribution in microstructure development is discussed.

Microstructure and Strengthening Mechanisms in an Ultrafine Grained Al-Mg-Sc Alloy Produced by Powder Metallurgy

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

Tammy J. Harrell; Troy D. Topping; Haiming Wen

2014-12-01

Additions of Sc to an Al-Mg matrix were investigated, paying particular attention to the influence of Al3Sc precipitates and other dispersoids, as well as grain size, on mechanical behavior. Prior studies have shown that Sc significantly increases the strength of coarse-grained Al-Mg alloys. Prompted by these findings, we hypothesized that it would be of fundamental and technological interest to study the behavior of Sc additions to an ultrafine-grained (UFG) microstructure (e.g., 100’s nm). Accordingly, we investigated the microstructural evolution and mechanical behavior of a cryomilled ultrafine grained Al-5Mg-0.4Sc (wt pct) and compared the results to those of an equivalent fine-grainedmore » material (FG) produced by powder metallurgy. Experimental materials were consolidated by hot isostatic pressing (HIP’ing) followed by extrusion or dual mode dynamic forging. Under identical processing conditions, UFG materials generate large Al3Sc precipitates with an average diameter of 154 nm and spaced approximately 1 to 3 µm apart, while precipitates in the FG materials have a diameter of 24 nm and are spaced 50 to 200 nm apart. The strengthening mechanisms are calculated for all materials and it is determined that the greatest strengthening contributions for the UFG and FG materials are Mg-O/N dispersion strengthening and precipitate strengthening, respectively.« less

Delamination Effect on Impact Properties of Ultrafine-Grained Low-Carbon Steel Processed by Warm Caliber Rolling

NASA Astrophysics Data System (ADS)

Inoue, Tadanobu; Yin, Fuxing; Kimura, Yuuji; Tsuzaki, Kaneaki; Ochiai, Shojiro

2010-02-01

Bulk ultrafine-grained (UFG) low-carbon steel bars were produced by caliber rolling, and the impact and tensile properties were investigated. Initial samples with two different microstructures, ferrite-pearlite and martensite (or bainite), were prepared and then caliber rolling was conducted at 500 °C. The microstructures in the rolled bars consisted of an elongated UFG structure with a strong α-fiber texture. The rolled bar consisting of spheroidal cementite particles that distributed uniformly in the elongated ferrite matrix of transverse grain sizes 0.8 to 1.0 μm exhibited the best strength-ductility balance and impact properties. Although the yield strength in the rolled bar increased 2.4 times by grain refinement, the upper-shelf energy did not change, and its value was maintained from 100 °C to -40 °C. In the rolled bars, cracks during an impact test branched parallel to the longitudinal direction of the test samples as temperatures decreased. Delamination caused by such crack branching appeared, remarkably, near the ductile-to-brittle transition temperature (DBTT). The effect of delamination on the impact properties was associated with crack propagation on the basis of the microstructural features in the rolled bars. In conclusion, the strength-toughness balance is improved by refining crystal grains and controlling their shape and orientation; in addition, delamination effectively enhances the low-temperature toughness.

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.

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

Phase transformation during surface ablation of cobalt-cemented tungsten carbide with pulsed UV laser

NASA Astrophysics Data System (ADS)

Li, T.; Lou, Q.; Dong, J.; Wei, Y.; Liu, J.

Surface ablation of cobalt-cemented tungsten carbide hard metal has been carried out in this work using a 308 nm, 20 ns XeCl excimer laser. Surface microphotography and XRD, as well as an electron probe have been used to investigate the transformation of phase and microstructure as a function of the pulse-number of laser shots at a laser fluence of 2.5 J/cm2. The experimental results show that the microstructure of cemented tungsten carbide is transformed from the original polygonal grains of size 3 μm to interlaced large, long grains with an increase in the number of laser shots up to 300, and finally to gross grains of size 10 μm with clear grain boundaries after 700 shots of laser irradiation. The crystalline structure of the irradiated area is partly transformed from the original WC to βWC1-x, then to αW2C and CW3, and finally to W crystal. It is suggested that the undulating `hill-valley' morphology may be the result of selective removal of cobalt binder from the surface layer of the hard metal. The formation of non-stoichiometric tungsten carbide may result from the escape of elemental carbon due to accumulated heating of the surface by pulsed laser irradiation.

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.

Quantification of the Barkhausen noise method for the evaluation of time-dependent degradation

NASA Astrophysics Data System (ADS)

Kim, Dong-Won; Kwon, Dongil

2003-02-01

The Barkhausen noise (BN) method has long been applied to measure the bulk magnetic properties of magnetic materials. Recently, this important nondestructive testing (NDT) method has been applied to evaluate microstructure, stress distribution analysis, fatigue, creep and fracture characteristics. Until now the BN method has been used only qualitatively in evaluating the variation of BN with variations in material properties. For this reason, few NDT methods have been applied in industrial plants and laboratories. The present investigation studied the coercive force and BN while varying the microstructure of ultrafine-grained steels and SA508 cl.3 steels. This variation was carried out according to the second heat-treatment condition with rolling of ultrafine-grained steels and the simulated time-dependent degradation of SA 508 cl.3 steels. An attempt was also made to quantify BN from the relationship between the velocity of magnetic domain walls and the retarding force, using the coercive force of the domain wall movement. The microstructure variation was analyzed according to time-dependent degradation. Fracture toughness was evaluated quantitatively by measuring the BN from two intermediary parameters; grain size and distribution of nonmagnetic particles. From these measurements, the variation of microstructure and fracture toughness can be directly evaluated by the BN method as an accurate in situ NDT method.

Thermal Stability of Nanocrystalline Alloys by Solute Additions and A Thermodynamic Modeling

NASA Astrophysics Data System (ADS)

Saber, Mostafa

Nanocrystalline alloys show superior properties due to their exceptional microstructure. Thermal stability of these materials is a critical aspect. It is well known that grain boundaries in nanocrystalline microstructures cause a significant increase in the total free energy of the system. A driving force provided to reduce this excess free energy can cause grain growth. The presence of a solute addition within a nanocrystalline alloy can lead to the thermal stability. Kinetic and thermodynamic stabilization are the two basic mechanisms with which stability of a nanoscale grain size can be achieved at high temperatures. The basis of this thesis is to study the effect of solute addition on thermal stability of nanocrystalline alloys. The objective is to determine the effect of Zr addition on the thermal stability of mechanically alloyed nanocrysatillne Fe-Cr and Fe-Ni alloys. In Fe-Cr-Zr alloy system, nanoscale grain size stabilization was maintained up to 900 °C by adding 2 at% Zr. Kinetic pinning by intermetallic particles in the nanoscale range was identified as a primary mechanism of thermal stabilization. In addition to the grain size strengthening, intermetallic particles also contribute to strengthening mechanisms. The analysis of microhardness, XRD data, and measured grain sizes from TEM micrographs suggested that both thermodynamic and kinetic mechanisms are possible mechanisms. It was found that alpha → gamma phase transformation in Fe-Cr-Zr system does not influence the grain size stabilization. In the Fe-Ni-Zr alloy system, it was shown that the grain growth in Fe-8Ni-1Zr alloy is much less than that of pure Fe and Fe-8Ni alloy at elevated temperatures. The microstructure of the ternary Fe-8Ni-1Zr alloy remains in the nanoscale range up to 700 °C. Using an in-situ TEM study, it was determined that drastic grain growth occurs when the alpha → gamma phase transformation occurs. Accordingly, there can be a synergistic relationship between grain growth and alpha → gamma phase transformation in Fe-Ni-Zr alloys. In addition to the experimental study of thermal stabilization of nanocrystalline Fe-Cr-Zr or Fe-Ni-Zr alloys, the thesis presented here developed a new predictive model, applicable to strongly segregating solutes, for thermodynamic stabilization of binary alloys. This model can serve as a benchmark for selecting solute and evaluating the possible contribution of stabilization. Following a regular solution model, both the chemical and elastic strain energy contributions are combined to obtain the mixing enthalpy. The total Gibbs free energy of mixing is then minimized with respect to simultaneous variations in the grain boundary volume fraction and the solute concentration in the grain boundary and the grain interior. The Lagrange multiplier method was used to obtained numerical solutions. Application are given for the temperature dependence of the grain size and the grain boundary solute excess for selected binary system where experimental results imply that thermodynamic stabilization could be operative. This thesis also extends the binary model to a new model for thermodynamic stabilization of ternary nanocrystalline alloys. It is applicable to strongly segregating size-misfit solutes and uses input data available in the literature. In a same manner as the binary model, this model is based on a regular solution approach such that the chemical and elastic strain energy contributions are incorporated into the mixing enthalpy DeltaHmix, and the mixing entropy DeltaSmix is obtained using the ideal solution approximation. The Gibbs mixing free energy Delta Gmix is then minimized with respect to simultaneous variations in grain growth and solute segregation parameters. The Lagrange multiplier method is similarly used to obtain numerical solutions for the minimum Delta Gmix. The temperature dependence of the nanocrystalline grain size and interfacial solute excess can be obtained for selected ternary systems. As an example, model predictions are compared to experimental results for Fe-Cr-Zr and Fe-Ni-Zr alloy systems. Consistency between the experimental results and the present model predictions provide a more rigorous criterion for investigating thermal stabilization. However, other possible contributions for grain growth stabilization should still be considered.

Spin Testing of Superalloy Disks With Dual Grain Structure

NASA Technical Reports Server (NTRS)

Hefferman, Tab M.

2006-01-01

This 24-month program was a joint effort between Allison Advanced Development Company (AADC), General Electric Aircraft (GEAE), and NASA Glenn Research Center (GRC). AADC led the disk and spin hardware design and analysis utilizing existing Rolls-Royce turbine disk forging tooling. Testing focused on spin testing four disks: two supplied by GEAE and two by AADC. The two AADC disks were made of Alloy 10, and each was subjected to a different heat treat process: one producing dual microstructure with coarse grain size at the rim and fine grain size at the bore and the other produced single fine grain structure throughout. The purpose of the spin tests was to provide data for evaluation of the impact of dual grain structure on disk overspeed integrity (yielding) and rotor burst criteria. The program culminated with analysis and correlation of the data to current rotor overspeed criteria and advanced criteria required for dual structure disks.

Solidification Microstructure, Segregation, and Shrinkage of Fe-Mn-C Twinning-Induced Plasticity Steel by Simulation and Experiment

NASA Astrophysics Data System (ADS)

Lan, Peng; Tang, Haiyan; Zhang, Jiaquan

2016-06-01

A 3D cellular automaton finite element model with full coupling of heat, flow, and solute transfer incorporating solidification grain nucleation and growth was developed for a multicomponent system. The predicted solidification process, shrinkage porosity, macrosegregation, grain orientation, and microstructure evolution of Fe-22Mn-0.7C twinning-induced plasticity (TWIP) steel match well with the experimental observation and measurement. Based on a new solute microsegregation model using the finite difference method, the thermophysical parameters including solid fraction, thermal conductivity, density, and enthalpy were predicted and compared with the results from thermodynamics and experiment. The effects of flow and solute transfer in the liquid phase on the solidification microstructure of Fe-22Mn-0.7C TWIP steel were compared numerically. Thermal convection decreases the temperature gradient in the liquid steel, leading to the enlargement of the equiaxed zone. Solute enrichment in front of the solid/liquid interface weakens the thermal convection, resulting in a little postponement of columnar-to-equiaxed transition (CET). The CET behavior of Fe-Mn-C TWIP steel during solidification was fully described and mathematically quantized by grain morphology statistics for the first time. A new methodology to figure out the CET location by linear regression of grain mean size with least-squares arithmetic was established, by which a composition design strategy for Fe-Mn-C TWIP steel according to solidification microstructure, matrix compactness, and homogeneity was developed.

Development of ultrafine-grained microstructure in Al-Cu-Mg alloy through equal-channel angular pressing

NASA Astrophysics Data System (ADS)

Sai Anuhya, Danam; Gupta, Ashutosh; Nayan, Niraj; Narayana Murty, S. V. S.; Manna, R.; Sastry, G. V. S.

2014-08-01

Al-Cu-Mg alloys are extensively used for riveting applications in aerospace industries due to their relatively high shear strength coupled with high plasticity. The significant advantage of using V65 aluminum alloy ((Al-4Cu-0.2Mg) for rivet application also stems from its significantly slower natural aging kinetics, which gives operational flexibility to carryout riveting operation even after 4 days of solution heat treatment, in contrast to its equivalent alloy AA2024.Rivets are usually made by cold heading of wire rods. In order to form a defect free rivet head, grain size control in wire rods is essential at each and every stage of processing right from casting onwards upto the final wire drawing stage. Wire drawing is carried out at room temperature to reduce diameter as well as impart good surface finish. In the present study, different microstructures in V65 alloy bars were produced by rolling at different temperatures (room temperature to 523K) and subsequently deformed by equal channel angular pressing (ECAP) at 423K upto an equivalent strain of 7. ECAP was carried out to study the effect of initial microstructure on grain refinement and degree of deformation on the evolution of ultrafine grain structure. The refinement of V65 alloy by ECAP is significantly influenced by Initial microstructure but amount of deformation strongly affects the evolution processes as revealed by optical microscopy and transmission electron microscopy.

Microstructure examination of Fe-14Cr ODS ferritic steels produced through different processing routes

NASA Astrophysics Data System (ADS)

Oksiuta, Z.; Hosemann, P.; Vogel, S. C.; Baluc, N.

2014-08-01

Various thermo-mechanical treatments were applied to refine and homogenise grain size and improve mechanical properties of hot-isostatically pressed (HIP) 14%Cr ODS ferritic steel. The grain size was reduced, improving mechanical properties, tensile strength and Charpy impact, however bimodal-like distribution was also observed. As a result, larger, frequently elongated grains with size above 1 μm and refined, equiaxed grains with a diameter ranging from 250 to 500 nm. Neutron diffraction measurements revealed that for HIP followed by hydrostatic extrusion material the strongest fiber texture was observed oriented parallel to the extrusion direction. In comparison with hot rolling and hot pressing methods, this material exhibited promising mechanical properties: the ultimate tensile strength of 1350 MPa, yield strength of 1280 MPa, total elongation of 21.7% and Charpy impact energy of 5.8 J. Inferior Charpy impact energy of ∼3.0 J was measured for HIP and hot rolled material, emphasising that parameters of this manufacturing process still have to be optimised. As an alternative manufacturing route, due to the uniform microstructure and simplicity of the process, hot pressing might be a promising method for production of smaller parts of ODS ferritic steels. Besides, the ductile-to-brittle transition temperature of all thermo-mechanically treated materials, in comparison with as-HIPped ODS steel, was improved by more than 50%, the transition temperature ranging from 50 to 70 °C (323 and 343 K) remains still unsatisfactory.

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.

Research on Microstructure and Properties of Welded Joint of High Strength Steel

NASA Astrophysics Data System (ADS)

Zhu, Pengxiao; Li, Yi; Chen, Bo; Ma, Xuejiao; Zhang, Dongya; Tang, Cai

2018-01-01

BS960 steel plates were welded by Laser-MAG and MAG. The microstructure and properties of the welded joints were investigated by optical microscope, micro-hardness tester, universal tensile testing machine, impact tester, scanning electron microscope (SEM) and fatigue tester. By a series of experiments, the following results were obtained: The grain size of the coarse grain zone with Laser-MAG welded joint is 20μm, and that with MAG welded joint is about 32μm, both of the fine grain region are composed of fine lath martensite and granular bainite; the width of the heat affected region with Laser-MAG is lower than that with MAG. The strength and impact energy of welded joints with Laser-MAG is higher than that with MAG. The conditioned fatigue limit of welded joint with Laser-MAG is 280MPa; however, the conditioned fatigue limit of welded joint with MAG is 250MPa.

Novel pre-alloyed powder processing of modified alnico 8: Correlation of microstructure and magnetic properties

DOE PAGES

Anderson, I. E.; Kassen, A. G.; White, E. M. H.; ...

2015-04-13

Progress is reviewed on development of an improved near-final bulk magnet fabrication process for alnico 8, as a non-rare earth permanent magnet with promise for sufficient energy density and coercivity for electric drive motors. This study showed that alnico bulk magnets in near-final shape can be made by simple compression molding from spherical high purity gas atomized pre-alloyed powder. Dwell time at peak sintering temperature (1250°C) greatly affected grain size of the resulting magnet alloys. This microstructure transformation was demonstrated to be useful for gaining partially aligned magnetic properties and boosting energy product. Furthermore, while a route to increased coercivitymore » was not identified by these experiments, manufacturability of bulk alnico magnet alloys in near-final shapes was demonstrated, permitting further processing and alloy modification experiments that can target higher coercivity and better control of grain anisotropy during grain growth.« less

Microstructure of as atomized and annealed U-Mo7 particles: A SEM/EBSD study of grain growth

NASA Astrophysics Data System (ADS)

Iltis, X.; Zacharie-Aubrun, I.; Ryu, H. J.; Park, J. M.; Leenaers, A.; Yacout, A. M.; Keiser, D. D.; Vanni, F.; Stepnik, B.; Blay, T.; Tarisien, N.; Tanguy, C.; Palancher, H.

2017-11-01

Significant progresses in the performances under in-pile irradiation of particular U-Mo based fuels have been observed over the last fifteen years. One of the remaining issues has still to be tackled for use as a LEU fuel in the high power research reactors: the U-Mo recrystallization and its associated swelling have to be controlled or delayed. One way to mitigate this problem would be to optimize the initial microstructure of U-Mo atomized particle, by homogenizing Mo concentration and increasing grain size. This paper mainly focuses on U-Mo grain growth. Based on samples prepared in the framework of KOMO-5 and EMPIrE tests, a methodological work based on the use of EBSD is presented. In particular, surface preparation procedures are proposed for powders and rods, this last one being most likely readily applicable for plate analysis. As-atomized microstructures are analyzed in detail and subsequently compared to those obtained on particles annealed at 1000 °C under various conditions. It is found that 1 h annealing under vacuum is a good compromise of temperature and time to meet the development goals, provided that few impurity precipitates are present within U-Mo particles, since these can impact grain growth.

Microhardness and microstructure evolution of TiB2 reinforced Inconel 625/TiB2 composite produced by selective laser melting

NASA Astrophysics Data System (ADS)

Zhang, Baicheng; Bi, Guijun; Nai, Sharon; Sun, Chen-nan; Wei, Jun

2016-06-01

In this study, micron-size TiB2 particles were utilized to reinforce Inconel 625 produced by selective laser melting. Exceptional microhardness 600-700 HV0.3 of the composite was obtained. In further investigation, the microstructure and mechanical properties of Inconel 625/TiB2 composite can be significantly influenced by addition of TiB2 particles during SLM. It was found that the long directional columnar grains observed from SLM-processed Inconel 625 were totally changed to fine dendritic matrix due to the addition of TiB2 particles. Moreover, with laser energy density (LED) of 1200 J/m, a Ti, Mo rich interface around TiB2 particles with fine thickness can be observed by FESEM and EDS. The microstructure evolution can be determined by different laser energy density (LED): under 1200 J/m, γ phase in dendrite grains; under 600 J/m, γ phase in combination of dendritic and acicular grains; under 400 J/m, γ phase acicular grains. Under optimized LED 1200 J/m, the dynamic nanohardness (8.62 GPa) and elastic modulus (167 GPa) of SLM-processed Inconel 625/TiB2 composite are higher compared with those of SLM-processed Inconel 625 (3.97 GPa and 135 GPa, respectively).

Behavior and Microstructure in Cryomilled Aluminum alloy Containing Diamondoids Nanoparticles

NASA Astrophysics Data System (ADS)

Hanna, Walid Magdy

Aluminum (Al) alloys have been the materials of choice for both civil and military aircraft structure. Primary among these alloys are 6061 Al and 5083 Al, which have used for several structural applications including those in aerospace and automobile industry. It is desirable to enhance strength in Al alloys beyond that achieved via traditional techniques such as precipitation hardening. Recent developments have indicated strengthening via grain refinement is an effective approach since, according the Hall-Petch relation, as grain size decreases strength significantly increases. The innovate techniques of severe plastic deformation, cryomilling, are successful in reefing grain size. These techniques lead to a minimum grain size that is the result of a dynamic balance between the formation of dislocation structure and its recovery by thermal processes. According to Mohamed's model, each metal is characterized by a minimum grain size that is determined by materials parameters such as the stacking faulty energy and the activation energy for diffusion. In the present dissertation, 6061 Al and 5083 Al were synthesized using cryomilling. Microstructural characterization was extensively carried out to monitor grain size changes. A close examination of the morphology of the 6061 Al powder particles revealed that in the early milling stages, the majority of the particles changed from spheres to thin disk-shaped particles. This change was attributed to the high degree of plastic deformation generated by the impact energy during ball-powder-ball collisions. Both transmission electron microscopy (TEM) and X-ray diffraction (XRD) were used to monitor the change in grain size as a function of milling time. The results of both techniques demonstrated a close agreement with respect to two observations: (a) during cryomilling, the grain size of 6061 Al decreased with milling time, and (b) after 15 h of milling, the grain size approached a minimum value of about 22 nm, which is in the range reported for Al (18 nm--24 nm). Despite this agreement, there was a discrepancy: for grain sizes > 40 nm, the grain size measured by TEM was appreciably larger that inferred from XRD. It was suggested that this discrepancy was most likely related to the limitation for accurately measuring grain sizes > 100 nm by the technique of XRD. It was reported that the average grain size of the as-milled powders of 5083 Al alloy was about 20 nm, and that when the as-milled powders were exposed to elevated temperatures or consolidated via hot isostatic pressing and extruded, the average grain size increased to about 250 nm. Very recent results have indicated the success of maintaining the thermal stability of Al by adding diamantane during milling. 5083 Al powders were cryomilled with 0.5 wt. % diamantane for 8 hours producing mechanically alloyed powders with an average grain size of 17 nm. The grain size remained nanocrystalline (less than100 nm) for Al 5083 alloy with 0.5% diamantane, even after 48 h at the highest temperature of 773 K. The Effect of Diamantane on the thermal stability of cryomilled nanocrystalline 5083 Al alloy was investigated by heating the powder in an inert gas atmosphere at temperature range from 473K to 773K for time interval between 0.5 hr. to 48 hr. The average grain size was observed to be in nano scale range less than 100 nm. The thermal stability results were found to be consistent with the grain growth model based on drag forces exerted by dispersed particles against grain boundary migration (Burke model). As observed for other cryomilled Al alloys, two grain growth regimes were identified using this model: one at relatively low temperatures (473--623 K) where the activation energy is about 1.9 kJ/mole and another at higher temperatures where the activation energy is about 18 kJ/mole. The presence of the former region was explained in terms of stress relaxation facilitated by less stable processes such as recovery of dislocation segments or sub-boundary remnants while the latter region was attributed to grain boundary realignment annihilation of grain boundary remnants.

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.

Effect of Deformation Parameters on Microstructure and Properties During DIFT of X70HD Pipeline Steel

NASA Astrophysics Data System (ADS)

Wang, Jian; Zhu, Wei; Xiao, Hong; Zhang, Liang-liang; Qin, Hao; Yu, Yue

2018-02-01

Grain refinement is a critical approach to improve the strength of materials without damaging the toughness. The grains of deformation-induced ferrite are considerably smaller than those of proeutectoid ferrite. Grain refinement is crucial to the application of deformation-induced ferrite. The composition of ferrite and bainite or martensite is important in controlling the performance of X70HD pipeline steel, and cooling significantly influences the control of their ratio and grain size. By analyzing the static and dynamic phase-transition points using Gleeble-3800 thermal simulator, thermal simulations were performed through two-stage deformations in the austenite zone. Ferrite transformation rules were studied with thermal simulation tests under different deformation and cooling parameters based on the actual production of cumulative deformation. The influence of deformation parameters on the microstructure transformation was analyzed. Numerous fine-grain deformation-induced ferrites were obtained by regulating various parameters, including deformation temperature, strain rate, cooling rate, final cooling temperature and other parameters. Results of metallographic observation and microtensile testing revealed that the selection of appropriate parameters can refine the grains and improve the performance of the X70HD pipeline steel.

Relationship between microstructure and ductility of investment cast ASTM F-75 implant alloy.

PubMed

Gómez, M; Mancha, H; Salinas, A; Rodríguez, J L; Escobedo, J; Castro, M; Méndez, M

1997-02-01

Hip replacement implants fabricated using the ASTM F-75 alloy sometimes fail in a sudden catastrophic way. In general, fractures start at microstructural defects subjected to stress-corrosion under chemical attack by body fluids. In this paper the results of a study on the effect of casting parameters on the microstructure of ASTM F-75 are presented. The preheating mold temperature and the liquid temperature were varied between 900 and 1000 degrees C, and 1410 and 1470 degrees C, respectively. Optimum static strength and ductility were obtained when shrinkage microporosity and the volume fraction of M23C6 "eutectic" carbides precipitated at grain boundaries were minimized by increasing the preheating mold temperature to 1000 degrees C and by using intermediate pouring temperatures of 1455 degrees C. Under these casting conditions, however, the solidification rates are low, leading to large grain sizes, which, in turn, reduce the strength of the material under dynamic loading conditions. The volume fraction of the M23C6 "blocky" carbides appears to be independent of the casting conditions; however, their size and spatial distributions determine the strength of the as-cast alloys.

Studies on Microstructure and Thermoelectric Properties of p-Type Bi-Sb-Te Based Alloys by Gas Atomization and Hot Extrusion Processes

NASA Astrophysics Data System (ADS)

Park, Ki-Chan; Madavali, Babu; Kim, Eun-Bin; Koo, Kyung-Wan; Hong, Soon-Jik

2017-05-01

p-Type Bi2Te3 + 75% Sb2Te3 based thermoelectric materials were fabricated via gas atomization and the hot extrusion process. The gas atomized powder showed a clean surface with a spherical shape, and expanded in a wide particle size distribution (average particle size 50 μm). The phase of the fabricated extruded and R-extruded bars was identified using x-ray diffraction. The relative densities of both the extruded and R-extruded samples were measured by Archimedes principle with ˜98% relative density. The R-extruded bar exhibited finer grain microstructure than that of single extrusion process, which was attributed to a recrystallization mechanism during the fabrication. The R-extruded sample showed improved Vickers hardness compared to the extruded sample due to its fine grain microstructure. The electrical conductivity improved for the extruded sample whereas the Seebeck coefficient decreases due to its high carrier concentration. The peak power factor, ˜4.26 × 10-3 w/mK2 was obtained for the single extrusion sample, which is higher than the R-extrusion sample owing to its high electrical properties.

Microstructure characterization based on the type of deformed grains in cold-rolled, Cu-added, bake-hardenable steel

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

Kim, J.S.; Kim, S.I.; Choi, S.-H., E-mail: shihoon@sunchon.ac.kr

2014-06-01

The electron backscatter diffraction technique has been used to characterize the microstructure of deformed grains in cold-rolled, Cu-added, bake-hardenable steel. A new scheme based on the kind and number of average orientations, as determined from a unique grain map of the deformed grains, was developed in order to classify deformed grains by type. The α-fiber components, γ-fiber components and random orientations, those which could not be assigned to either γ-fiber or α-fiber components, were used to define the average orientation of unique grains within individual deformed grains. The microstructures of deformed grains in as-rolled specimens were analyzed based on themore » Taylor factor, stored energy, and misorientation. The relative levels and distributions of the Taylor factor, the stored energy and the misorientation were examined in terms of the types of deformed grains. - Highlights: • We characterized the microstructure of Cu-added BH steel using EBSD. • A new scheme was developed in order to classify deformed grains by type. • Stored energy and misorientation are strongly dependent on the type of deformed grains. • Microstructure was examined in terms of the types of deformed grains.« less

The effect of postprocessing on tensile property and microstructure evolution of friction stir welding aluminum alloy joint

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

Hu, Z.L., E-mail: zhilihuhit@163.com; State Key Laboratory of Advanced Welding and Joining, Harbin Institute of Technology, Harbin 150001; State Key Laboratory of Materials Processing and Die & Mould Technology, Huazhong University of Science and Technology

Friction stir welding is an efficient manufacturing method for joining aluminum alloy and can dramatically reduce grain size conferring excellent plastic deformation properties. Consequently, friction stir welding is used to manufacture tailor welded blanks to optimize weight or performance in the final component. In the study, the microstructural evolution and mechanical properties of friction stir welding joint during plastic forming and subsequent heat treatment were investigated. The microstructural characteristics of the friction stir welding joints were studied by Electron Backscattered Diffraction and Transmission Electron Microscopy. The mechanical properties were evaluated by tensile and microhardness tests. It is found that themore » tensile and yield strengths of friction stir welding joints are significantly improved after severe plastic deformation due to the grain refinement. Following heat treatment, the strength of the friction stir welding joints significantly decrease due to the obvious abnormal grain growth. Careful attention must be given to the processing route of any friction stir welding joint intended for plastic forming, especially the annealing between forming passes. Severe plastic deforming of the friction stir welding joint leads to a high level of stored energy/dislocation density, which causes the abnormal grain growth during subsequent heat treatment, and consequently reduce the mechanical properties of the friction stir welding joint. - Highlights: • Great changes are observed in the microstructure of FSW joint after postprocessing. • Postprocessing shows great effect on the microstructure stability of FSW joint. • The weld shows more significant decrease in strength than the BM due to the AGG. • Attention must be given to the processing route of FSW joint for plastic forming.« less

Low Temperature Superplasticity of Ti-6Al-4V Processed by Warm Multidirectional Forging (Preprint)

DTIC Science & Technology

2012-07-01

microstructure in the two-phase titanium alloy Ti- 6Al - 4V . A microstructure with a grain size of 135 nm was attained, enabling low-temperature...the / titanium alloy Ti- 6Al - 4V [3]. The great interest in microstructure refinement is associated with significantly reduced superplastic (SP...consisted of the / titanium alloy Ti- 6Al - 4V with a nominal composition (in weight pct.) of 6.3 Al, 4.1 V, 0.18 Fe, 0.03 Si, 0.02 Zr, 0.01 C, 0.18 O, 0.01 N

Patterning of nanocrystalline diamond films for diamond microstructures useful in MEMS and other devices

DOEpatents

Gruen, Dieter M [Downers Grove, IL; Busmann, Hans-Gerd [Bremen, DE; Meyer, Eva-Maria [Bremen, DE; Auciello, Orlando [Bolingbrook, IL; Krauss, Alan R [late of Naperville, IL; Krauss, Julie R [Naperville, IL

2004-11-02

MEMS structure and a method of fabricating them from ultrananocrystalline diamond films having average grain sizes of less than about 10 nm and feature resolution of less than about one micron . The MEMS structures are made by contacting carbon dimer species with an oxide substrate forming a carbide layer on the surface onto which ultrananocrystalline diamond having average grain sizes of less than about 10 nm is deposited. Thereafter, microfabrication process are used to form a structure of predetermined shape having a feature resolution of less than about one micron.

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.

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.

Microstructure evolution and texture development in a friction stir-processed AISI D2 tool steel

NASA Astrophysics Data System (ADS)

Yasavol, N.; Abdollah-zadeh, A.; Vieira, M. T.; Jafarian, H. R.

2014-02-01

Crystallographic texture developments during friction stir processing (FSP) of AISI D2 tool were studied with respect to grain sizes in different tool rotation rates. Comparison of the grain sizes in various rotation rates confirmed that grain refinement occurred progressively in higher rotation rates by severe plastic deformation. It was found that the predominant mechanism during FSP should be dynamic recovery (DRV) happened concurrently with continuous dynamic recrystallization (CDRX) caused by particle-stimulated nucleation (PSN). The developed shear texture relates to the ideal shear textures of D1 and D2 in bcc metals. The prevalence of highly dense arrangement of close-packed planes of bcc and the lowest Taylor factor showed the lowest compressive residual stress which is responsible for better mechanical properties compared with the grain-precipitate refinement.

Characterization of Laves phase in Crofer 22 H stainless steel.

PubMed

Hsiao, Zheng-Wen; Kuhn, Bernd; Chen, Delphic; Singheiser, Lorenz; Kuo, Jui-Chao; Lin, Dong-Yih

2015-07-01

This study investigated the effect of annealing temperature on the precipitation behavior of Crofer(®) 22 H at 600°C, 700°C, and 800°C. The grain size distribution, precipitate phase identification, and microstructure were analyzed using electron backscatter diffraction (EBSD) and energy dispersive X-ray spectroscopy (EDS). The morphology of Laves phase (Fe,Cr,Si)(2)(Nb,W) precipitates having the Cr(2)Nb structure changed from strip-like to needle-shaped as the annealing temperature was increased. The precipitates of the Laves phase also shifted from the grain boundaries to the grain interiors when the temperature was increased. However, the average grain size (150 μm) of the ferritic matrix did not significantly change at 600°C, 700°C, and 800°C for 10 h. Copyright © 2015 Elsevier Ltd. All rights reserved.

Continuum understanding of twin formation near grain boundaries of FCC metals with low stacking fault energy

NASA Astrophysics Data System (ADS)

Jung, Jaimyun; Yoon, Jae Ik; Kim, Jung Gi; Latypov, Marat I.; Kim, Jin You; Kim, Hyoung Seop

2017-12-01

Deformation twinning from grain boundaries is often observed in face-centered cubic metals with low stacking fault energy. One of the possible factors that contribute to twinning origination from grain boundaries is the intergranular interactions during deformation. Nonetheless, the influence of mechanical interaction among grains on twin evolution has not been fully understood. In spite of extensive experimental and modeling efforts on correlating microstructural features with their twinning behavior, a clear relation among the large aggregate of grains is still lacking. In this work, we characterize the micromechanics of grain-to-grain interactions that contribute to twin evolution by investigating the mechanical twins near grain boundaries using a full-field crystal plasticity simulation of a twinning-induced plasticity steel deformed in uniaxial tension at room temperature. Microstructures are first observed through electron backscatter diffraction technique to obtain data to reconstruct a statistically equivalent microstructure through synthetic microstructure building. Grain-to-grain micromechanical response is analyzed to assess the collective twinning behavior of the microstructural volume element under tensile deformation. Examination of the simulated results reveal that grain interactions are capable of changing the local mechanical behavior near grain boundaries by transferring strain across grain boundary or localizing strain near grain boundary.

Evaluation of Microstructure, Mechanical Properties and Corrosion Resistance of Friction Stir-Welded Aluminum and Magnesium Dissimilar Alloys

NASA Astrophysics Data System (ADS)

Verma, Jagesvar; Taiwade, Ravindra V.; Sapate, Sanjay G.; Patil, Awanikumar P.; Dhoble, Ashwinkumar S.

2017-10-01

Microstructure, mechanical properties and corrosion resistance of dissimilar friction stir-welded aluminum and magnesium alloys were investigated by applying three different rotational speeds at two different travel speeds. Sound joints were obtained in all the conditions. The microstructure was examined by an optical and scanning electron microscope, whereas localized chemical information was studied by energy-dispersive spectroscopy. Stir zone microstructure showed mixed bands of Al and Mg with coarse and fine equiaxed grains. Grain size of stir zone reduced compared to base metals, indicated by dynamic recrystallization. More Al patches were observed in the stir zone as rotational speed increased. X-ray diffraction showed the presence of intermetallics in the stir zone. Higher tensile strength and hardness were obtained at a high rotational speed corresponding to low travel speed. Tensile fractured surface indicated brittle nature of joints. Dissimilar friction stir weld joints showed different behaviors in different corrosive environments, and better corrosion resistance was observed at a high rotational speed corresponding to low travel speed (FW3) in a sulfuric and chloride environments. Increasing travel speed did not significantly affect on microstructure, mechanical properties and corrosion resistance as much as the rotational speed.

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.

Effects of Annular Electromagnetic Stirring Coupled with Intercooling on Grain Refinement and Homogeneity During Direct Chill Casting of Large-Sized 7005 Alloy Billet

NASA Astrophysics Data System (ADS)

Luo, Yajun; Zhang, Zhifeng; Li, Bao; Gao, Mingwei; Qiu, Yang; He, Min

2017-12-01

To obtain a large-sized, high-quality aluminum alloy billet, an advanced uniform direct chill (UDC) casting method was developed by combining annular electromagnetic stirring (A-EMS) with intercooling in the sump. The 7005 alloy was chosen to investigate the effect of UDC on grain refinement and homogeneity during normal direct chill (NDC) casting. It was concluded that the microstructure consisting of both primary α-Al phase and secondary phases becomes finer and more homogeneous for the billets prepared with UDC casting compared to those prepared with NDC casting, and the forced cooling from both the inner and outer melt under A-EMS has a measurable effect on grain refinement and homogeneity.

Effect of Thermomechanical Processing on Microstructure, Texture Evolution, and Mechanical Properties of Al-Mg-Si-Cu Alloys with Different Zn Contents

NASA Astrophysics Data System (ADS)

Wang, X. F.; Guo, M. X.; Chen, Y.; Zhu, J.; Zhang, J. S.; Zhuang, L. Z.

2017-07-01

The effect of thermomechanical processing on microstructure, texture evolution, and mechanical properties of Al-Mg-Si-Cu alloys with different Zn contents was studied by mechanical properties, microstructure, and texture characterization in the present study. The results show that thermomechanical processing has a significant influence on the evolution of microstructure and texture and on the final mechanical properties, independently of Zn contents. Compared with the T4P-treated (first preaged at 353 K (80 °C) for 12 hours and then naturally aged for 14 days) sheets with high final cold rolling reduction, the T4P-treated sheets with low final cold rolling reduction possess almost identical strength and elongation and higher average r values. Compared with the intermediate annealed sheets with high final cold rolling reduction, the intermediate annealed sheets with low final cold rolling reduction contain a higher number of particles with a smaller size. After solution treatment, in contrast to the sheets with high final cold rolling reduction, the sheets with low final cold rolling reduction possess finer grain structure and tend to form a weaker recrystallization texture. The recrystallization texture may be affected by particle distribution, grain size, and final cold rolling texture. Finally, the visco-plastic self-consistent (VPSC) model was used to predict r values.

Microstructure characterization of LAE442 magnesium alloy processed by extrusion and ECAP

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

Minárik, Peter; Král, Robert; Pešička, Josef

2016-02-15

The magnesium alloy LAE442 was processed by extrusion and equal channel angular pressing (ECAP) to achieve ultrafine grained microstructure. Detailed characterization of the microstructure was performed by scanning electron microscope, electron back scattered diffraction (EBSD) and transmission electron microscope. The initial, as-cast, microstructure consisted of large grains of ~ 1 mm. The grain refinement due to the processing by severe plastic deformation led to a decrease of the average grain size to ~ 1.7 μm after the final step of ECAP. A detailed characterization of secondary phases showed the precipitation of Al{sub 11}RE{sub 3}, Al{sub 2}Ca and Al{sub 10}RE{sub 2}Mn{submore » 7} intermetallic phases. X-ray diffraction measurements proved that Li is dissolved within the magnesium matrix in the as-cast condition. Newly formed Al{sub 3}Li phase was observed after ECAP. The texture formation due to the extrusion and ECAP was different from that in the other magnesium alloys due to the activation of non-basal slip systems as a result of the decrease of the c/a ratio. - Highlights: • Combined extrusion and equal channel angular pressing results in significant grain refinement by factor 1000 approximately. • Al{sub 11}RE{sub 3}, Al{sub 2}Ca and Al{sub 10}RE{sub 2}Mn{sub 7} secondary phases are present in the as-cast material while Li was dissolved in the Mg matrix. • Extrusion and ECAP have no effect on the composition of the secondary phases but they influence strongly their distribution. • Texture evolution is affected by decrease of c/a ratio due to the presence of Li and resulting activation of non-basal slip.« less

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.

Microstructure, magnetic and magnetocaloric properties in Ni42.9Co6.9Mn38.3Sn11.9 alloy ribbons

NASA Astrophysics Data System (ADS)

Ma, S. C.; Ge, Q.; Yang, S.; Liu, K.; Han, X. Q.; Yu, K.; Song, Y.; Zhang, Z. S.; Jiang, Q. Z.; Chen, C. C.; Liu, R. H.; Zhong, Z. C.

2018-05-01

The microstructure, magnetic and magnetocaloric properties are investigated in the melt-spun and annealed Ni42.9Co6.9Mn38.3Sn11.9 ribbons. The columnar grains grow perpendicular to ribbon surfaces. After annealing, the grain size increases greatly. Meanwhile, the parent phase is suppressed and therefore L10 martensite predominates, indicating obvious shift of martensitic transformation to high temperature. More interestingly, the martensite variants are distinctly observed on the fractured cross-section of annealed ribbons, not just on the free surface in general. The significant enhancement of magnetic entropy change and effective refrigerant capacities with relatively smaller thermal hysteresis make annealed ribbons potential candidate in magnetic refrigeration around room temperature.

Investigation on temporal evolution of the grain refinement in copper under high strain rate loading via in-situ synchrotron measurement and predictive modeling

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

Shah, Pooja Nitin; Shin, Yung C.; Sun, Tao

Synchrotron X-rays are integrated with a modified Kolsky tension bar to conduct in situ tracking of the grain refinement mechanism operating during the dynamic deformation of metals. Copper with an initial average grain size of 36 μm is refined to 6.3 μm when loaded at a constant high strain rate of 1200 s -1. The synchrotron measurements revealed the temporal evolution of the grain refinement mechanism in terms of the initiation and rate of refinement throughout the loading test. A multiscale coupled probabilistic cellular automata based recrystallization model has been developed to predict the microstructural evolution occurring during dynamic deformationmore » processes. The model accurately predicts the initiation of the grain refinement mechanism with a predicted final average grain size of 2.4 μm. As a result, the model also accurately predicts the temporal evolution in terms of the initiation and extent of refinement when compared with the experimental results.« less

Investigation on temporal evolution of the grain refinement in copper under high strain rate loading via in-situ synchrotron measurement and predictive modeling

DOE PAGES

Shah, Pooja Nitin; Shin, Yung C.; Sun, Tao

2017-10-03

Synchrotron X-rays are integrated with a modified Kolsky tension bar to conduct in situ tracking of the grain refinement mechanism operating during the dynamic deformation of metals. Copper with an initial average grain size of 36 μm is refined to 6.3 μm when loaded at a constant high strain rate of 1200 s -1. The synchrotron measurements revealed the temporal evolution of the grain refinement mechanism in terms of the initiation and rate of refinement throughout the loading test. A multiscale coupled probabilistic cellular automata based recrystallization model has been developed to predict the microstructural evolution occurring during dynamic deformationmore » processes. The model accurately predicts the initiation of the grain refinement mechanism with a predicted final average grain size of 2.4 μm. As a result, the model also accurately predicts the temporal evolution in terms of the initiation and extent of refinement when compared with the experimental results.« less

The Influence of Lath, Block and Prior Austenite Grain (PAG) Size on the Tensile, Creep and Fatigue Properties of Novel Maraging Steel

PubMed Central

McAdam, Steven; Hill, Paul; Rawson, Martin; Perkins, Karen

2017-01-01

The influence of martensitic microstructure and prior austenite grain (PAG) size on the mechanical properties of novel maraging steel was studied. This was achieved by looking at two different martensitic structures with PAG sizes of approximately 40 µm and 80 µm, produced by hot rolling to different reductions. Two ageing heat-treatments were considered: both heat-treatments consisted of austenisation at 960 °C, then aging at 560 °C for 5 h, but while one was rapidly cooled the other was slow cooled and then extended aged at 480 °C for 64 h. It is shown that for the shorter ageing treatment the smaller PAG size resulted in significant improvements in strength (increase of more than 150 MPa), ductility (four times increase), creep life (almost four times increase in creep life) and fatigue life (almost doubled). Whereas, the extended aged sample showed similar changes in the fatigue life, elongation and hardness it displayed yet showed no difference in tensile strength and creep. These results display the complexity of microstructural contributions to mechanical properties in maraging steels. PMID:28773086

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.