From Solidification Processing to Microstructure to Mechanical Properties: A Multi-scale X-ray Study of an Al-Cu Alloy Sample

DOE PAGES

Tourret, D.; Mertens, J. C. E.; Lieberman, E.; ...

2017-09-13

We follow an Al-12 at. pct Cu alloy sample from the liquid state to mechanical failure, using in situ X-ray radiography during directional solidification and tensile testing, as well as three-dimensional computed tomography of the microstructure before and after mechanical testing. The solidification processing stage is simulated with a multi-scale dendritic needle network model, and the micromechanical behavior of the solidified microstructure is simulated using voxelized tomography data and an elasto-viscoplastic fast Fourier transform model. This study demonstrates the feasibility of direct in situ monitoring of a metal alloy microstructure from the liquid processing stage up to its mechanical failure,more » supported by quantitative simulations of microstructure formation and its mechanical behavior.« less

From Solidification Processing to Microstructure to Mechanical Properties: A Multi-scale X-ray Study of an Al-Cu Alloy Sample

NASA Astrophysics Data System (ADS)

Tourret, D.; Mertens, J. C. E.; Lieberman, E.; Imhoff, S. D.; Gibbs, J. W.; Henderson, K.; Fezzaa, K.; Deriy, A. L.; Sun, T.; Lebensohn, R. A.; Patterson, B. M.; Clarke, A. J.

2017-11-01

We follow an Al-12 at. pct Cu alloy sample from the liquid state to mechanical failure, using in situ X-ray radiography during directional solidification and tensile testing, as well as three-dimensional computed tomography of the microstructure before and after mechanical testing. The solidification processing stage is simulated with a multi-scale dendritic needle network model, and the micromechanical behavior of the solidified microstructure is simulated using voxelized tomography data and an elasto-viscoplastic fast Fourier transform model. This study demonstrates the feasibility of direct in situ monitoring of a metal alloy microstructure from the liquid processing stage up to its mechanical failure, supported by quantitative simulations of microstructure formation and its mechanical behavior.

Influence of Sintering Temperature on the Microstructure and Mechanical Properties of In Situ Reinforced Titanium Composites by Inductive Hot Pressing

PubMed Central

Arévalo, Cristina; Montealegre-Meléndez, Isabel; Ariza, Enrique; Kitzmantel, Michael; Rubio-Escudero, Cristina; Neubauer, Erich

2016-01-01

This research is focused on the influence of processing temperature on titanium matrix composites reinforced through Ti, Al, and B4C reactions. In order to investigate the effect of Ti-Al based intermetallic compounds on the properties of the composites, aluminum powder was incorporated into the starting materials. In this way, in situ TixAly were expected to form as well as TiB and TiC. The specimens were fabricated by the powder metallurgy technique known as inductive hot pressing (iHP), using a temperature range between 900 °C and 1400 °C, at 40 MPa for 5 min. Raising the inductive hot pressing temperature may affect the microstructure and properties of the composites. Consequently, the variations of the reinforcing phases were investigated. X-ray diffraction, microstructural analysis, and mechanical properties (Young’s modulus and hardness) of the specimens were carried out to evaluate and determine the significant influence of the processing temperature on the behavior of the composites. PMID:28774039

Effect of Thermal and Chemical Treatment on the Microstructural, Mechanical and Machining Performance of W319 Al-Si-Cu Cast Alloy Engine Blocks and Directionally Solidified Machinability Test Blocks

NASA Astrophysics Data System (ADS)

Szablewski, Daniel

The research presented in this work is focused on making a link between casting microstructural, mechanical and machining properties for 319 Al-Si sand cast components. In order to achieve this, a unique Machinability Test Block (MTB) is designed to simulate the Nemak V6 Al-Si engine block solidification behavior. This MTB is then utilized to cast structures with in-situ nano-alumina particle master alloy additions that are Mg based, as well as independent in-situ Mg additions, and Sr additions to the MTB. The Universal Metallurgical Simulator and Analyzer (UMSA) Technology Platform is utilized for characterization of each cast structure at different Secondary Dendrite Arm Spacing (SDAS) levels. The rapid quench method and Jominy testing is used to assess the capability of the nano-alumina master alloy to modify the microstructure at different SDAS levels. Mechanical property assessment of the MTB is done at different SDAS levels on cast structures with master alloy additions described above. Weibull and Quality Index statistical analysis tools are then utilized to assess the mechanical properties. The MTB is also used to study single pass high speed face milling and bi-metallic cutting operations where the Al-Si hypoeutectic structure is combined with hypereutectoid Al-Si liners and cast iron cylinder liners. These studies are utilized to aid the implementation of Al-Si liners into the Nemak V6 engine block and bi-metallic cutting of the head decks. Machining behavior is also quantified for the investigated microstructures, and the Silicon Modification Level (SiML) is utilized for microstructural analysis as it relates to the machining behavior.

Role of Microstructure on the Performance of UHTCs

NASA Technical Reports Server (NTRS)

Johnson, Sylvia M.; Gasch, Matthew J.; Lawson, John W.; Gusman, Michael I.; Stackpoole, Mairead

2010-01-01

We have investigated a number of methods to control microstructure. We have routes to form: a) in situ "composites" b) Very fine microstructures. Arcjet testing and other characterization of monolithic materials. Control oxidation through microstructure and composition. Beginning to incorporate these materials as matrices for composites. Modeling effort to facilitate material design and characterization.

Microstructures and Properties of Plasma Sprayed Ni Based Coatings Reinforced by TiN/C1-xNxTi Generated from In-Situ Solid-Gas Reaction.

PubMed

Wang, Wenquan; Li, Wenmo; Xu, Hongyong

2017-07-11

The strengthening hard phases TiN/C 1- x N x Ti were generated by in-situ solid-gas reaction in Ni-based composite coatings prepared using a plasma spray welding process to reinforce the wear resistance of the coatings. The microstructures and properties of the coatings were investigated. The results showed that the coatings mainly consisted of phases such as TiN, C 1- x N x Ti, TiC, etc. A small amount of CrB, M₇C₃, and M 23 C₆ were also detected in the coatings by micro-analysis method. Compared with the originally pure NiCrBSi coatings, the hardness of the NiCrBSi coatings reinforced by in-situ solid-gas reaction was 900 HV 0.5 , increased by more than 35%. Consequently, the wear resistance of the reinforced coatings was greatly improved due to the finely and uniformly dispersed hard phases mentioned above. The weight losses after wear test for the two kinds of coatings were 15 mg and 8 mg, respectively.

Modelling of deformation and recrystallisation microstructures in rocks and ice

NASA Astrophysics Data System (ADS)

Bons, Paul D.; Evans, Lynn A.; Gomez-Rivas, Enrique; Griera, Albert; Jessell, Mark W.; Lebensohn, Ricardo; Llorens, Maria-Gema; Peternell, Mark; Piazolo, Sandra; Weikusat, Ilka; Wilson, Chris J. L.

2015-04-01

Microstructures both record the deformation history of a rock and strongly control its mechanical properties. As microstructures in natural rocks only show the final "post-mortem" state, geologists have attempted to simulate the development of microstructures with experiments and later numerical models. Especially in-situ experiments have given enormous insight, as time-lapse movies could reveal the full history of a microstructure. Numerical modelling is an alternative approach to simulate and follow the change in microstructure with time, unconstrained by experimental limitations. Numerical models have been applied to a range of microstructural processes, such as grain growth, dynamic recrystallisation, porphyroblast rotation, vein growth, formation of mylonitic fabrics, etc. The numerical platform "Elle" (www.elle.ws) in particular has brought progress in the simulation of microstructural development as it is specifically designed to include the competition between simultaneously operating processes. Three developments significantly improve our capability to simulate microstructural evolution: (1) model input from the mapping of crystallographic orientation with EBSD or the automatic fabric analyser, (2) measurement of grain size and crystallographic preferred orientation evolution using neutron diffraction experiments and (3) the implementation of the full-field Fast Fourier Transform (FFT) solver for modelling anisotropic crystal-plastic deformation. The latter enables the detailed modelling of stress and strain as a function of local crystallographic orientation, which has a strong effect on strain localisation such as, for example, the formation of shear bands. These models can now be compared with the temporal evolution of crystallographic orientation distributions in in-situ experiments. In the last decade, the possibility to combine experiments with numerical simulations has allowed not only verification and refinement of the numerical simulation technique but also increased significantly the ability to predict and/or interpret natural microstructures. This contribution will present the most recent developments in in-situ and numerical modelling of deformation and recrystallisation microstructures in rocks and in ice.

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses.

PubMed

Miglierini, Marcel B; Procházka, Vít; Vrba, Vlastimil; Švec, Peter; Janičkovič, Dušan; Matúš, Peter

2018-06-07

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic glasses (MGs). Despite their amorphous nature, the identification of hyperfine interactions unveils faint structural modifications. For this purpose, we have employed two techniques that utilize nuclear resonance among nuclear levels of a stable 57 Fe isotope, namely Mössbauer spectrometry and nuclear forward scattering (NFS) of synchrotron radiation. The effects of heat treatment upon (Fe2.85Co1)77Mo8Cu1B14 MG are discussed using the results of ex situ and in situ experiments, respectively. As both methods are sensitive to hyperfine interactions, information on structural arrangement as well as on magnetic microstructure is readily available. Mössbauer spectrometry performed ex situ describes how the structural arrangement and magnetic microstructure appears at room temperature after the annealing under certain conditions (temperature, time), and thus this technique inspects steady states. On the other hand, NFS data are recorded in situ during dynamically changing temperature and NFS examines transient states. The use of both techniques provides complementary information. In general, they can be applied to any suitable system in which it is important to know its steady state but also transient states.

Effect of Layer Thickness in Selective Laser Melting on Microstructure of Al/5 wt.%Fe2O3 Powder Consolidated Parts

PubMed Central

Hao, Liang

2014-01-01

In situ reaction was activated in the powder mixture of Al/5 wt.%Fe2O3 by using selective laser melting (SLM) to directly fabricate aluminium metal matrix composite parts. The microstructural characteristics of these in situ consolidated parts through SLM were investigated under the influence of thick powder bed, 75 μm layer thickness, and 50 μm layer thickness in various laser powers and scanning speeds. It was found that the layer thickness has a strong influence on microstructural outcome, mainly attributed to its impact on oxygen content of the matrix. Various microstructural features (such as granular, coralline-like, and particulate appearance) were observed depending on the layer thickness, laser power, and scanning speed. This was associated with various material combinations such as pure Al, Al-Fe intermetallics, and Al(-Fe) oxide phases formed after in situ reaction and laser rapid solidification. Uniformly distributed very fine particles could be consolidated in net-shape Al composite parts by using lower layer thickness, higher laser power, and lower scanning speed. The findings contribute to the new development of advanced net-shape manufacture of Al composites by combining SLM and in situ reaction process. PMID:24526879

Comparison of Commonly-Used Microwave Radiative Transfer Models for Snow Remote Sensing

NASA Technical Reports Server (NTRS)

Royer, Alain; Roy, Alexandre; Montpetit, Benoit; Saint-Jean-Rondeau, Olivier; Picard, Ghislain; Brucker, Ludovic; Langlois, Alexandre

2017-01-01

This paper reviews four commonly-used microwave radiative transfer models that take different electromagnetic approaches to simulate snow brightness temperature (T(sub B)): the Dense Media Radiative Transfer - Multi-Layer model (DMRT-ML), the Dense Media Radiative Transfer - Quasi-Crystalline Approximation Mie scattering of Sticky spheres (DMRT-QMS), the Helsinki University of Technology n-Layers model (HUT-nlayers) and the Microwave Emission Model of Layered Snowpacks (MEMLS). Using the same extensively measured physical snowpack properties, we compared the simulated T(sub B) at 11, 19 and 37 GHz from these four models. The analysis focuses on the impact of using different types of measured snow microstructure metrics in the simulations. In addition to density, snow microstructure is defined for each snow layer by grain optical diameter (Do) and stickiness for DMRT-ML and DMRT-QMS, mean grain geometrical maximum extent (D(sub max)) for HUT n-layers and the exponential correlation length for MEMLS. These metrics were derived from either in-situ measurements of snow specific surface area (SSA) or macrophotos of grain sizes (D(sub max)), assuming non-sticky spheres for the DMRT models. Simulated T(sub B) sensitivity analysis using the same inputs shows relatively consistent T(sub B) behavior as a function of Do and density variations for the vertical polarization (maximum deviation of 18 K and 27 K, respectively), while some divergences appear in simulated variations for the polarization ratio (PR). Comparisons with ground based radiometric measurements show that the simulations based on snow SSA measurements have to be scaled with a model-specific factor of Do in order to minimize the root mean square error (RMSE) between measured and simulated T(sub B). Results using in-situ grain size measurements (SSA or D(sub max), depending on the model) give a mean T(sub B) RMSE (19 and 37 GHz) of the order of 16-26 K, which is similar for all models when the snow microstructure metrics are scaled. However, the MEMLS model converges to better results when driven by the correlation length estimated from in-situ SSA measurements rather than D(sub max) measurements. On a practical level, this paper shows that the SSA parameter, a snow property that is easy to retrieve in-situ, appears to be the most relevant parameter for characterizing snow microstructure, despite the need for a scaling factor.

A review of techniques for visualising soft tissue microstructure deformation and quantifying strain Ex Vivo.

PubMed

Disney, C M; Lee, P D; Hoyland, J A; Sherratt, M J; Bay, B K

2018-04-14

Many biological tissues have a complex hierarchical structure allowing them to function under demanding physiological loading conditions. Structural changes caused by ageing or disease can lead to loss of mechanical function. Therefore, it is necessary to characterise tissue structure to understand normal tissue function and the progression of disease. Ideally intact native tissues should be imaged in 3D and under physiological loading conditions. The current published in situ imaging methodologies demonstrate a compromise between imaging limitations and maintaining the samples native mechanical function. This review gives an overview of in situ imaging techniques used to visualise microstructural deformation of soft tissue, including three case studies of different tissues (tendon, intervertebral disc and artery). Some of the imaging techniques restricted analysis to observational mechanics or discrete strain measurement from invasive markers. Full-field local surface strain measurement has been achieved using digital image correlation. Volumetric strain fields have successfully been quantified from in situ X-ray microtomography (micro-CT) studies of bone using digital volume correlation but not in soft tissue due to low X-ray transmission contrast. With the latest developments in micro-CT showing in-line phase contrast capability to resolve native soft tissue microstructure, there is potential for future soft tissue mechanics research where 3D local strain can be quantified. These methods will provide information on the local 3D micromechanical environment experienced by cells in healthy, aged and diseased tissues. It is hoped that future applications of in situ imaging techniques will impact positively on the design and testing of potential tissue replacements or regenerative therapies. © 2018 The Authors Journal of Microscopy © 2018 Royal Microscopical Society.

Application of X-ray phase contrast micro-tomography to the identification of traditional Chinese medicines

NASA Astrophysics Data System (ADS)

Ye, L. L.; Xue, Y. L.; Ni, L. H.; Tan, H.; Wang, Y. D.; Xiao, T. Q.

2013-07-01

Nondestructive and in situ investigation to the characteristic microstructures are important to the identification of traditional Chinese medicines (TCMs), especially for precious specimens and samples with oil contains. X-ray phase contrast micro-tomography (XPCMT) could be a practical solution for this kind of investigation. Fructus Foeniculi, a fruit kind of TCMs, is selected as the test sample. Experimental results show that the characteristic microstructures of Fructus Foeniculi, including vittae, vascular bundles, embryo, endosperm and the mesocarp reticulate cells around the vittae can be clearly distinguished and the integrated dissepiments microstructure in the vittae was observed successfully. Especially, for the first time, with virtual slice technique, it can investigate the liquid contains inside the TCMs. The results show that the vittae filled with volatile oil in the oil chamber were observed with this nondestructive and in situ 3-dimensional imaging technique. Furthermore, taking the advantage of micro-computed tomography, we can obtain the characteristic microstructures' quantitative information of the volume in liquid state. The volume of the oil chambers and the volatile oil, which are contained inside the vittae, was quantitatively analyzed. Accordingly, it can calculate the volume ratio of the volatile oil easily and accurately. As a result, we could conclude that XPCMT could be a useful tool for the nondestructive identification and quantitative analysis to TCMs.

Microstructural and micromechanical characterization of IN718 theta shaped specimens built with electron beam melting

DOE PAGES

Cakmak, Ercan; Kirka, Michael M.; Watkins, Thomas R.; ...

2016-02-23

Theta-shaped specimens were additively manufactured out of Inconel 718 powders using an electron beam melting technique, as a model complex load bearing structure. We employed two different build strategies; producing two sets of specimens. Microstructural and micro-mechanical characterizations were performed using electron back-scatter, synchrotron x-ray and in-situ neutron diffraction techniques. In particular, the cross-members of the specimens were the focus of the synchrotron x-ray and in-situ neutron diffraction measurements. The build strategies employed resulted in the formation of distinct microstructures and crystallographic textures, signifying the importance of build-parameter manipulation for microstructural optimization. Large strain anisotropy of the different lattice planesmore » was observed during in-situ loading. Texture was concluded to have a distinct effect upon both the axial and transverse strain responses of the cross-members. In particular, the (200), (220) and (420) transverse lattice strains all showed unexpected overlapping trends in both builds. This was related to the strong {200} textures along the build/loading direction, providing agreement between the experimental and calculated results.« less

In Situ Synchrotron X-ray Study of Ultrasound Cavitation and Its Effect on Solidification Microstructures

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

Mi, Jiawei; Tan, Dongyue; Lee, Tung Lik

2014-12-11

Considerable progress has been made in studying the mechanism and effectiveness of using ultrasound waves to manipulate the solidification microstructures of metallic alloys. However, uncertainties remain in both the underlying physics of how microstructures evolve under ultrasonic waves, and the best technological approach to control the final microstructures and properties. We used the ultrafast synchrotron X-ray phase contrast imaging facility housed at the Advanced Photon Source, Argonne National Laboratory, US to study in situ the highly transient and dynamic interactions between the liquid metal and ultrasonic waves/bubbles. The dynamics of ultrasonic bubbles in liquid metal and their interactions with themore » solidifying phases in a transparent alloy were captured in situ. The experiments were complemented by the simulations of the acoustic pressure field, the pulsing of the bubbles, and the associated forces acting onto the solidifying dendrites. The study provides more quantitative understanding on how ultrasonic waves/bubbles influence the growth of dendritic grains and promote the grain multiplication effect for grain refinement.« less

Synchrotron X-ray micro-tomography at the Advanced Light Source: Developments in high-temperature in-situ mechanical testing

NASA Astrophysics Data System (ADS)

Barnard, Harold S.; MacDowell, A. A.; Parkinson, D. Y.; Mandal, P.; Czabaj, M.; Gao, Y.; Maillet, E.; Blank, B.; Larson, N. M.; Ritchie, R. O.; Gludovatz, B.; Acevedo, C.; Liu, D.

2017-06-01

At the Advanced Light Source (ALS), Beamline 8.3.2 performs hard X-ray micro-tomography under conditions of high temperature, pressure, mechanical loading, and other realistic conditions using environmental test cells. With scan times of 10s-100s of seconds, the microstructural evolution of materials can be directly observed over multiple time steps spanning prescribed changes in the sample environment. This capability enables in-situ quasi-static mechanical testing of materials. We present an overview of our in-situ mechanical testing capabilities and recent hardware developments that enable flexural testing at high temperature and in combination with acoustic emission analysis.

Friction stir processing of an aluminum-magnesium alloy with pre-placing elemental titanium powder: In-situ formation of an Al{sub 3}Ti-reinforced nanocomposite and materials characterization

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

Khodabakhshi, F., E-mail: farzadkhodabakhshi83@gmail.com; Simchi, A.; Institute for Nanoscience and Nanotechnology, Sharif University of Technology, P.O. Box 11365-9466, Azadi Avenue, 14588 Tehran

A fine-grained Al–Mg/Al{sub 3}Ti nanocomposite was fabricated by friction stir processing (FSP) of an aluminum-magnesium (AA5052) alloy with pre-placed titanium powder in the stirred zone. Microstructural evolutions and formation of intermetallic phases were analyzed by optical and electron microscopic techniques across the thickness section of the processed sheets. The microstructure of the nanocomposite consisted of a fine-grained aluminum matrix (1.5 µm), un-reacted titanium particles (<40 µm) and reinforcement particles of Al{sub 3}Ti (<100 nm) and Mg{sub 2}Si (<100 nm). Detailed microstructural analysis indicated solid-state interfacial reactions between the aluminum matrix and micro-sized titanium particles to form Al{sub 3}Ti intermetallic phase.more » The hard inclusions were then fractured and re-distributed in the metal matrix by the severe thermo-mechanical conditions imposed by FSP. Evaluation of mechanical properties by hardness measurement and uniaxial tensile test determined significant enhancement in the mechanical strength (by 2.5 order of magnetite) with a high ductility (~22%). Based on a dislocation-based model analysis, it was suggested that the strength enhancement was governed by grain refinement and the presence of hard inclusions (4 vol%) in the metal matrix. Fractographic studies also showed a ductile-brittle fracture mode for the nanocomposite compared with fully ductile rupture of the annealed alloy as well as the FSPed specimen without pre-placing titanium particles. - Highlights: • FSP was employed to fabricate in situ nanocomposite. • The AA5052 Al alloy with pre-placed micro-sized Ti particles were utilized. • The structural analysis was revealed that the in situ formation of Al{sub 3}Ti nanophase. • The SZ grain structure was refined by PSN and ZHP mechanisms during DRX. • Hardness and tensile strength were improved up to ~2.5 times with a good ductility.« less

Characterizing Suspension Plasma Spray Coating Formation Dynamics through Curvature Measurements

NASA Astrophysics Data System (ADS)

Chidambaram Seshadri, Ramachandran; Dwivedi, Gopal; Viswanathan, Vaishak; Sampath, Sanjay

2016-12-01

Suspension plasma spraying (SPS) enables the production of variety of microstructures with unique mechanical and thermal properties. In SPS, a liquid carrier (ethanol/water) is used to transport the sub-micrometric feedstock into the plasma jet. Considering complex deposition dynamics of SPS technique, there is a need to better understand the relationships among spray conditions, ensuing particle behavior, deposition stress evolution and resultant properties. In this study, submicron yttria-stabilized zirconia particles suspended in ethanol were sprayed using a cascaded arc plasma torch. The stresses generated during the deposition of the layers (termed evolving stress) were monitored via the change in curvature of the substrate measured using an in situ measurement apparatus. Depending on the deposition conditions, coating microstructures ranged from feathery porous to dense/cracked deposits. The evolving stresses and modulus were correlated with the observed microstructures and visualized via process maps. Post-deposition bi-layer curvature measurement via low temperature thermal cycling was carried out to quantify the thermo-elastic response of different coatings. Lastly, preliminary data on furnace cycle durability of different coating microstructures were evaluated. This integrated study involving in situ diagnostics and ex situ characterization along with process maps provides a framework to describe coating formation mechanisms, process parametrics and microstructure description.

Optimized Setup and Protocol for Magnetic Domain Imaging with In Situ Hysteresis Measurement.

PubMed

Liu, Jun; Wilson, John; Davis, Claire; Peyton, Anthony

2017-11-07

This paper elaborates the sample preparation protocols required to obtain optimal domain patterns using the Bitter method, focusing on the extra steps compared to standard metallographic sample preparation procedures. The paper proposes a novel bespoke rig for dynamic domain imaging with in situ BH (magnetic hysteresis) measurements and elaborates the protocols for the sensor preparation and the use of the rig to ensure accurate BH measurement. The protocols for static and ordinary dynamic domain imaging (without in situ BH measurements) are also presented. The reported method takes advantage of the convenience and high sensitivity of the traditional Bitter method and enables in situ BH measurement without interrupting or interfering with the domain wall movement processes. This facilitates establishing a direct and quantitative link between the domain wall movement processes-microstructural feature interactions in ferritic steels with their BH loops. This method is anticipated to become a useful tool for the fundamental study of microstructure-magnetic property relationships in steels and to help interpret the electromagnetic sensor signals for non-destructive evaluation of steel microstructures.

In situ TEM of radiation effects in complex ceramics.

PubMed

Lian, Jie; Wang, L M; Sun, Kai; Ewing, Rodney C

2009-03-01

In situ transmission electron microscopy (TEM) has been extensively applied to study radiation effects in a wide variety of materials, such as metals, ceramics and semiconductors and is an indispensable tool in obtaining a fundamental understanding of energetic beam-matter interactions, damage events, and materials' behavior under intense radiation environments. In this article, in situ TEM observations of radiation effects in complex ceramics (e.g., oxides, silicates, and phosphates) subjected to energetic ion and electron irradiations have been summarized with a focus on irradiation-induced microstructural evolution, changes in microchemistry, and the formation of nanostructures. New results for in situ TEM observation of radiation effects in pyrochlore, A(2)B(2)O(7), and zircon, ZrSiO(4), subjected to multiple beam irradiations are presented, and the effects of simultaneous irradiations of alpha-decay and beta-decay on the microstructural evolution of potential nuclear waste forms are discussed. Furthermore, in situ TEM results of radiation effects in a sodium borosilicate glass subjected to electron-beam exposure are introduced to highlight the important applications of advanced analytical TEM techniques, including Z-contrast imaging, energy filtered TEM (EFTEM), and electron energy loss spectroscopy (EELS), in studying radiation effects in materials microstructural evolution and microchemical changes. By combining ex situ TEM and advanced analytical TEM techniques with in situ TEM observations under energetic beam irradiations, one can obtain invaluable information on the phase stability and response behaviors of materials under a wide range of irradiation conditions. (c) 2009 Wiley-Liss, Inc.

Crystallization dynamics in glass-forming systems

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

Cullinan, Timothy Edward

Crystallization under far-from-equilibrium conditions is investigated for two different scenarios: crystallization of the metallic glass alloy Cu 50Zr 50 and solidification of a transparent organic compound, o-terphenyl. For Cu 50Zr 50, crystallization kinetics are quanti ed through a new procedure that directly fits thermal analysis data to the commonly utilized JMAK model. The phase evolution during crystallization is quantified through in-situ measurements (HEXRD, DSC) and ex-situ microstructural analysis (TEM, HRTEM). The influence of chemical partitioning, diffusion, and crystallographic orientation on this sequence are examined. For o-terphenyl, the relationship between crystal growth velocity and interface undercooling is systematically studied via directionalmore » solidification.« less

Prospects of In-Situ α-Al2O3 as an Inoculant in Aluminum: A Feasibility Study

NASA Astrophysics Data System (ADS)

Sreekumar, V. M.; Hari Babu, N.; Eskin, D. G.

2017-09-01

In-situ α-Al2O3 was successfully synthesized and dispersed in Al alloy using B2O3 and ultrasonication-aided liquid mixing technique. Microstructure analysis identified α-Al2O3 as the most common phase in the composite master alloy, whereas AlB12 was frequently observed and AlB2 was rarely found in the alloy. Grain refinement analysis of selected Al alloys registered a transition of columnar to equiaxial grains of α-Al with the inoculation of the master alloy and ultrasonication treatment. Similarly, an improvement in the mechanical properties of A357 alloy was observed with the combination of inoculation and ultrasonication treatment.

Mechanical properties enhancement and microstructure study of Al-Si-TiB2 in situ composites

NASA Astrophysics Data System (ADS)

Sahoo, S. K.; Majhi, J.; Pattnaik, A. B.; Sahoo, J. K.; Das, Swagat

2018-03-01

Al–Si alloy-based composite is one of the most promising MMC materials owing to its outstanding mechanical properties, wear and corrosion resistance, low cost and ability to be synthesized via conventional casting routes. Challenges in achieving clean interface between reinforced particles and matrix alloy have been overcome by means of in-situ techniques of fabrication. Present investigation is concerned with synthesizing Al-Si-TiB2 in-situ composites through stir casting route using K2TiF6 and KBF4 halide salts for exothermic salt metal reaction. X-Ray diffraction analysis revealed the existence of TiB2 in the prepared samples. Effect of TiB2in-situ particles in the Al-Si base alloy has been investigated from the results obtained from optical microscopy as well as SEM study and wear analysis with a pin on disc wear testing apparatus. Improved hardness and wear properties were observed with addition of TiB2.

A Structural Study of Escherichia coli Cells Using an In Situ Liquid Chamber TEM Technology.

PubMed

Wang, Yibing; Chen, Xin; Cao, Hongliang; Deng, Chao; Cao, Xiaodan; Wang, Ping

2015-01-01

Studying cell microstructures and their behaviors under living conditions has been a challenging subject in microbiology. In this work, in situ liquid chamber TEM was used to study structures of Escherichia coli cells in aqueous solutions at a nanometer-scale resolution. Most of the cells remained intact under electron beam irradiation, and nanoscale structures were observed during the TEM imaging. The analysis revealed structures of pili surrounding the E. coli cells; the movements of the pili in the liquid were also observed during the in situ tests. This technology also allowed the observation of features of the nucleoid in the E. coli cells. Overall, in situ TEM can be applied as a valuable tool to study real-time microscopic structures and processes in microbial cells residing in native aqueous solutions.

Artifacts introduced by ion milling in Al-Li-Cu alloys.

PubMed

Singh, A K; Imam, M A; Sadananda, K

1988-04-01

Ion milling is commonly used to prepare specimens for observation under transmission electron microscope (TEM). This technique sometimes introduces artifacts in specimens contributing to misleading interpretation of TEM results as observed in the present investigation of Al-Li-Cu alloys. This type of alloy, in general, contains several kinds of precipitates, namely delta', T1, and theta'. It is found that ion milling even for a short time produces drastic changes in the precipitate characteristics as compared to standard electropolishing methods of specimen preparation for TEM. Careful analysis of selected area diffraction patterns and micrographs shows that after ion milling delta' precipitates are very irregular, whereas other precipitates coarsen and they are surrounded by misfit dislocations. In situ hot-stage TEM experiments were performed to relate the microstructure to that observed in the ion-milled specimen. Results and causes of ion milling effects on the microstructure are discussed in relation to standard electropolishing techniques and in situ hot-stage experiment.

ELLIPSOMETRIC STUDY OF a-Si:H NUCLEATION, GROWTH, AND INTERFACES

NASA Astrophysics Data System (ADS)

Collins, R. W.

Recent in situ and spectroscopic ellipsometry investigations of hydrogenated amorphous silicon (a-Si:H) nucleation behavior, microstructural evolution, and interface formation are reviewed. An outline of the commonly applied experimental techniques and data analysis is also presented. In situ ellipsometry reveals a nuclei formation and convergence sequence in the first 50Å of a-Si:H growth by rf plasma deposition from silane on c-Si and metal substrates. This sequence provides evidence of favorable growth chemistry that results in material with a low density of structural defects. The influence of deposition parameters and processes on the nucleation and subsequent microstructural evolution of a-Si:H is covered in detail. Among the other topics discussed include: nucleation of microcrystalline Si, evolution of surface roughness on a-Si:H, inert and reactive gas plasma modification of a-Si:H, and formation of a-Si:H heterostructures with SiO2, wide band gap alloys, and Bdoped a-Si:H.

Investigation of Hydrogen Embrittlement Susceptibility of X80 Weld Joints by Thermal Simulation

NASA Astrophysics Data System (ADS)

Peng, Huangtao; An, Teng; Zheng, Shuqi; Luo, Bingwei; Wang, Siyu; Zhang, Shuai

2018-05-01

The objective of this study was to investigate the hydrogen embrittlement (HE) susceptibility and influence mechanism of X80 weld joints. Slow strain rate testing (SSRT) under in situ H-charging, combined with microstructure and fracture analysis, was performed on the base metal (BM), weld metal (WM), thermally simulated fine-grained heat-affected zone (FGHAZ) and coarse-grained heat-affected zone (CGHAZ). Results showed that the WM and simulated HAZ had a greater degree of high local strain distribution than the BM; compared to the CGHAZ, the FGHAZ had lower microhardness and more uniformly distributed stress. SSRT results showed that the weld joint was highly sensitive to HE; the HE index decreased in the following sequence: FGHAZ, WM, CGHAZ and BM. The effect of the microstructure on HE was mainly reflected in microstructure, local stress distribution and microhardness.

Transmission Electron Microscopy of Non-Etched Presolar Silicon Carbide

NASA Technical Reports Server (NTRS)

Stroud, Rhonda M.; Nittler, Larry R.; Alexander, Conel M. O'D.; Bernatowicz, Thomas J.; Messenger, Scott R.

2003-01-01

Our solar system formed from nuclei produced in earlier generations of stars. Mixing in the proto-solar nebula isotopically homogenized most of this material, but some grains, called presolar grains, retain their original isotopic composition. The isotopic properties of presolar SiC grains indicate that most of the grains formed in the outflows of carbon-rich Asymptotic Giant Branch (AGB) stars. The microstructure of these presolar grains reflects the conditions of the dust formation and subsequent alteration. Early microstructural studies of SiC grains obtained by acid dissolution from meteorites show that most isotopically anomalous SiC grains have the face-centered cubic b- SiC structure. However, Daulton et al. have shown that a small fraction of sub-micron presolar SiC grains are of the hexagonal 2H polytype (a-SiC). Although the harsh chemical treatments of these grains does not alter their crystal structure, significant alteration of the surface morphology of the grains due to the acid treatments has been observed. In addition, the acid treatments may preferentially remove cracked or fissured grains, and possible sub-grains, such as graphite. By studying SiC grains isolated by physical separation and found in situ, we attempt to obtain a more complete analysis of presolar SiC microstructures, including the surface morphology, in order to address the formation and processing history of the grains. In our prior work, we reported on one in situ SiC grain (hereafter CBIS1). Here we present results from two additional grains, one in situ, and one prepared as a physical separate.

In Situ GIWAXS Analysis of Solvent and Additive Effects on PTB7 Thin Film Microstructure Evolution during Spin Coating

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

Manley, Eric F.; Strzalka, Joseph; Fauvell, Thomas J.

The influence of solvent and processing additives on the pathways and rates of crystalline morphology formation for spin-coated semiconducting PTB7 (poly[[4,8-bis[(2- ethylhexyl)oxy]benzo[1,2-b:4,5-b']dithiophene-2,6-diyl][3-fluoro-2-[(2-ethylhexyl)- carbonyl]-thieno[3,4-b]thiophenediyl

In Situ GIWAXS Analysis of Solvent and Additive Effects on PTB7 Thin Film Microstructure Evolution during Spin Coating

DOE PAGES

Manley, Eric F.; Strzalka, Joseph; Fauvell, Thomas J.; ...

2017-10-09

The influence of solvent and processing additives on the pathways and rates of crystalline morphology formation for spin-coated semiconducting PTB7 (poly[[4,8-bis[(2- ethylhexyl)oxy]benzo[1,2-b:4,5-b']dithiophene-2,6-diyl][3-fluoro-2-[(2-ethylhexyl)- carbonyl]-thieno[3,4-b]thiophenediyl

Effect of thermomechanical processing on the microstructure and retained austenite stability during in situ tensile testing using synchrotron x-ray diffraction of NbMoAI TRIP steel.

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

Pereloma, E.; Zhang, L.; Liss, K.-D.

2011-06-01

In this work we compare and contrast the stability of retained austenite during tensile testing of Nb-Mo-Al transformation-induced plasticity steel subjected to different thermomechanical processing schedules. The obtained microstructures were characterised using optical metallography, transmission electron microscopy and X-ray diffraction. The transformation of retained austenite to martensite under tensile loading was observed by in-situ high energy X-ray diffraction at 1ID / APS. It has been shown that the variations in the microstructure of the steel, such as volume fractions of present phases, their morphology and dimensions, play a critical role in the strain-induced transition of retained austenite to martensite.

Microstructure-failure mode correlations in braided composites

NASA Technical Reports Server (NTRS)

Filatovs, G. J.; Sadler, Robert L.; El-Shiekh, Aly

1992-01-01

Explication of the fracture processes of braided composites is needed for modeling their behavior. Described is a systematic exploration of the relationship between microstructure, loading mode, and micro-failure mechanisms in carbon/epoxy braided composites. The study involved compression and fracture toughness tests and optical and scanning electron fractography, including dynamic in-situ testing. Principal failure mechanisms of low sliding, buckling, and unstable crack growth are correlated to microstructural parameters and loading modes; these are used for defining those microstructural conditions which are strength limiting.

Multiscale Modeling and Process Optimization for Engineered Microstructural Complexity

DTIC Science & Technology

2007-10-26

Ferroelectric Ceramics , Materials Science Forum, 404-407, 413-418 2002. 42. R. T. Brewer, H. A. Atwater Rapid biaxial texture development during...Multiscale Study of Internal Stress and Texture in Electroceramics, 106th Annual Meeting of the American Ceramic Society, Indianapolis, Indiana, 20...Rogan, Texture and Strain Analysis of PZT by In-Situ Neutron Diffraction, MRS Spring Meeting, San Francisco, CA; April 2002. 43. E. Ustundag

Backtracking Depth-Resolved Microstructures for Crystal Plasticity Identification—Part 1: Backtracking Microstructures

NASA Astrophysics Data System (ADS)

Shi, Qiwei; Latourte, Félix; Hild, François; Roux, Stéphane

2017-12-01

In situ mechanical tests performed on polycrystalline materials in a scanning electron microscope suffer from the lack of information on depth-resolved three-dimensional microstructures. The latter ones can be accessed with focused ion beam technology only postmortem, because it is destructive. The present study considers the challenge of backtracking this deformed microstructure to the reference state. This theoretical question is tackled on a numerical (synthetic) test case. A two-dimensional microstructure with one dimension along the depth is considered, and deformed using a crystal plasticity law. The proposed numerical strategy is shown to retrieve accurately the reference state.

Corrosion and Corrosion-Fatigue Behavior of 7075 Aluminum Alloys Studied by In Situ X-Ray Tomography

NASA Astrophysics Data System (ADS)

Stannard, Tyler

7XXX Aluminum alloys have high strength to weight ratio and low cost. They are used in many critical structural applications including automotive and aerospace components. These applications frequently subject the alloys to static and cyclic loading in service. Additionally, the alloys are often subjected to aggressive corrosive environments such as saltwater spray. These chemical and mechanical exposures have been known to cause premature failure in critical applications. Hence, the microstructural behavior of the alloys under combined chemical attack and mechanical loading must be characterized further. Most studies to date have analyzed the microstructure of the 7XXX alloys using two dimensional (2D) techniques. While 2D studies yield valuable insights about the properties of the alloys, they do not provide sufficiently accurate results because the microstructure is three dimensional and hence its response to external stimuli is also three dimensional (3D). Relevant features of the alloys include the grains, subgrains, intermetallic inclusion particles, and intermetallic precipitate particles. The effects of microstructural features on corrosion pitting and corrosion fatigue of aluminum alloys has primarily been studied using 2D techniques such as scanning electron microscopy (SEM) surface analysis along with post-mortem SEM fracture surface analysis to estimate the corrosion pit size and fatigue crack initiation site. These studies often limited the corrosion-fatigue testing to samples in air or specialized solutions, because samples tested in NaCl solution typically have fracture surfaces covered in corrosion product. Recent technological advancements allow observation of the microstructure, corrosion and crack behavior of aluminum alloys in solution in three dimensions over time (4D). In situ synchrotron X-Ray microtomography was used to analyze the corrosion and cracking behavior of the alloy in four dimensions to elucidate crack initiation at corrosion pits for samples of multiple aging conditions and impurity concentrations. Additionally, chemical reactions between the 3.5 wt% NaCl solution and the crack surfaces were quantified by observing the evolution of hydrogen bubbles from the crack. The effects of the impurity particles and age-hardening particles on the corrosion and fatigue properties were examined in 4D.

In-situ 3D visualization of composite microstructure during polymer-to-ceramic conversion

DOE PAGES

Larson, Natalie M.; Zok, Frank W.

2017-10-31

One route for producing fiber-reinforced ceramic-matrix composites entails repeated impregnation and pyrolysis of a preceramic polymer in a fiber preform. The process relies crucially on the development of networks of contiguous cracks during pyrolysis, thereby allowing further impregnation to attain nearly-full densification. The present study employs in-situ x-ray computed tomography (XCT) to reveal in three dimensions the evolution of matrix structure during pyrolysis of a SiC-based preceramic polymer to 1200 °C. Observations are used to guide the development of a taxonomy of crack geometries and crack structures and to identify the temporal sequence of their formation. A quantitative analysis ismore » employed to characterize effects of local microstructural dimensions on the conditions required to form cracks of various types. Complementary measurements of gas evolution and mass loss of the preceramic polymer during pyrolysis as well as changes in mass density and Young's modulus provide context for the physical changes revealed by XCT. Furthermore, the findings provide a foundation for future development of physics-based models to guide composite fabrication processes.« less

Assessment of Shape Memory Alloys - From Atoms To Actuators - Via In Situ Neutron Diffraction

NASA Technical Reports Server (NTRS)

Benafan, Othmane

2014-01-01

As shape memory alloys (SMAs) become an established actuator technology, it is important to identify the fundamental mechanisms responsible for their performance by understanding microstructure performance relationships from processing to final form. Yet, microstructural examination of SMAs at stress and temperature is often a challenge since structural changes occur with stress and temperature and microstructures cannot be preserved through quenching or after stress removal, as would be the case for conventional materials. One solution to this dilemma is in situ neutron diffraction, which has been applied to the investigation of SMAs and has offered a unique approach to reveal the fundamental micromechanics and microstructural aspects of bulk SMAs in a non-destructive setting. Through this technique, it is possible to directly correlate the micromechanical responses (e.g., internal residual stresses, lattice strains), microstructural evolutions (e.g., texture, defects) and phase transformation properties (e.g., phase fractions, kinetics) to the macroscopic actuator behavior. In this work, in situ neutron diffraction was systematically employed to evaluate the deformation and transformation behavior of SMAs under typical actuator conditions. Austenite and martensite phases, yield behavior, variant selection and transformation temperatures were characterized for a polycrystalline NiTi (49.9 at. Ni). As the alloy transforms under thermomechanical loading, the measured textures and lattice plane-level variations were directly related to the cyclic actuation-strain characteristics and the dimensional instability (strain ratcheting) commonly observed in this alloy. The effect of training on the shape memory characteristics of the alloy and the development of two-way shape memory effect (TWSME) were also assessed. The final conversion from a material to a useful actuator, typically termed shape setting, was also investigated in situ during constrained heatingcooling and subsequent shape recovery experiments. Neutron diffraction techniques are also being applied to the investigation of novel high temperature SMAs with the objective of designing alloys with better stability, higher transition temperatures and ultimately superior durability.

Spatially controlled, in situ synthesis of polymers

DOEpatents

Caneba, Gerard T.; Tirumala, Vijaya Raghavan; Mancini, Derrick C.; Wang, Hsien-Hau

2005-03-22

An in situ polymer microstructure formation method. The monomer mixture is polymerized in a solvent/precipitant through exposure to ionizing radiation in the absence any chemical mediators. If an exposure mask is employed to block out certain regions of the radiation cross section, then a patterned microstructure is formed. The polymerization mechanism is based on the so-called free-radical retrograde-precipitation polymerization process, in which polymerization occurs while the system is phase separating above the lower critical solution temperature. This method was extended to produce a crosslinked line grid-pattern of poly (N-isopropylacrylamide), which has been known to have thermoreversible properties.

Effects of the TiC Nanoparticle on Microstructures and Tensile Properties of Selective Laser Melted IN718/TiC Nanocomposites

NASA Astrophysics Data System (ADS)

Yao, Xiling; Moon, Seung Ki; Lee, Bing Yang; Bi, Guijun

2018-03-01

The purpose of this paper is to investigate the effects of TiC nanoparticle content on microstructures and tensile properties of the IN718/TiC nanocomposites fabricated by selective laser melting (SLM). 0.5wt%, 1.0wt%, and 2.0wt% of TiC nanoparticles are added to the IN718 powders. The bulk-form IN718/TiC nanocomposites with different TiC contents are fabricated in-situ by SLM using the same process settings. The evolution of microstructures and tensile properties as the effect of changing the TiC content is studied using the optical microscopy, scanning electron microscopy, X-ray diffraction analysis, and tensile testing. The increase of TiC content refines the microstructure, promotes the formation of the cellular morphology, and reduces the size and continuity of Laves precipitates. Increasing the TiC content improves the yield strength and ultimate tensile strength but decreases the ductility. The grain refinement, dislocation bowing, dislocation punching, and the reduction in Laves precipitate contribute to the strengthening effect in the IN718/TiC nanocomposites.

Macroscopic and Microstructural Aspects of the Transformation Behavior in a Polycrystalline NiTi Shape Memory Alloy

NASA Technical Reports Server (NTRS)

Benafan, Othmane; Noebe, Ronald D.; Padula, Santo A., II; Lerch, Bradley A.; Bigelow, Glen S.; Gaydosh, Darrell J.; Garg, Anita; An, Ke; Vaidyanathan, Raj

2013-01-01

The mechanical and microstructural behavior of a polycrystalline Ni(49.9)Ti(50.1) (at.%) shape memory alloy was investigated as a function of temperature around the transformation regime. The bulk macroscopic responses, measured using ex situ tensile deformation and impulse excitation tests, were compared to the microstructural evolution captured using in situ neutron diffraction. The onset stress for inelastic deformation and dynamic Young's modulus were found to decrease with temperature, in the martensite regime, reaching a significant minimum at approximately 80 C followed by an increase in both properties, attributed to the martensite to austenite transformation. The initial decrease in material compliance during heating affected the ease with which martensite reorientation and detwinning could occur, ultimately impacting the stress for inelastic deformation prior to the start of the reverse transformation.

In situ optical microscopy of the martensitic phase transformation of lithium

NASA Astrophysics Data System (ADS)

Krystian, M.; Pichl, W.

2000-12-01

The phase transformation of lithium was investigated by in situ optical microscopy in a helium cryostat. The martensite microstructure is composed of irregular segments which grow in rapid bursts from many nuclei to a final size of 10 to 20 μm and then are immobilized. A major part of the segments is arranged in groups of parallel lamellas. A theoretical consideration of lattice compatibility predicts the existence of an almost perfectly coherent habit-plane interface between bcc and 9R in lithium. Therefore, the irregular microstructure is interpreted by the presence of the disordered polytype phase. Comparison with an earlier investigation in comparably impure lithium indicates a strong influence of impurities on the transformation mechanism. The connections between the low-temperature phase diagram, the geometrical compatibility condition, and the martensite microstructure are discussed.

Nanoscale size effect in in situ titanium based composites with cell viability and cytocompatibility studies.

PubMed

Miklaszewski, Andrzej; Jurczyk, Mieczysława U; Kaczmarek, Mariusz; Paszel-Jaworska, Anna; Romaniuk, Aleksandra; Lipińska, Natalia; Żurawski, Jakub; Urbaniak, Paulina; Jurczyk, Mieczyslaw

2017-04-01

Novel in situ Metal Matrix Nanocomposite (MMNC) materials based on titanium and boron, revealed their new properties in the nanoscale range. In situ nanocomposites, obtained through mechanical alloying and traditional powder metallurgy compaction and sintering, show obvious differences to their microstructural analogue. A unique microstructure connected with good mechanical properties reliant on the processing conditions favour the nanoscale range of results of the Ti-TiB in situ MMNC example. The data summarised in this work, support and extend the knowledge boundaries of the nanoscale size effect that influence not only the mechanical properties but also the studies on the cell viability and cytocompatibility. Prepared in the same bulk, in situ MMNC, based on titanium and boron, could be considered as a possible candidate for dental implants and other medical applications. The observed relations and research conclusions are transferable to the in situ MMNC material group. Aside from all the discussed relations, the increasing share of these composites in the ever-growing material markets, heavily depends on the attractiveness and a possible wider application of these composites as well as their operational simplicity presented in this work. Copyright © 2016 Elsevier B.V. All rights reserved.

The effects of crosslinkers on physical, mechanical, and cytotoxic properties of gelatin sponge prepared via in-situ gas foaming method as a tissue engineering scaffold.

PubMed

Poursamar, S Ali; Lehner, Alexander N; Azami, Mahmoud; Ebrahimi-Barough, Somayeh; Samadikuchaksaraei, Ali; Antunes, A P M

2016-06-01

In this study porous gelatin scaffolds were prepared using in-situ gas foaming, and four crosslinking agents were used to determine a biocompatible and effective crosslinker that is suitable for such a method. Crosslinkers used in this study included: hexamethylene diisocyanate (HMDI), poly(ethylene glycol) diglycidyl ether (epoxy), glutaraldehyde (GTA), and genipin. The prepared porous structures were analyzed using Fourier Transform Infrared Spectroscopy (FT-IR), thermal and mechanical analysis as well as water absorption analysis. The microstructures of the prepared samples were analyzed using Scanning Electron Microscopy (SEM). The effects of the crosslinking agents were studied on the cytotoxicity of the porous structure indirectly using MTT analysis. The affinity of L929 mouse fibroblast cells for attachment on the scaffold surfaces was investigated by direct cell seeding and DAPI-staining technique. It was shown that while all of the studied crosslinking agents were capable of stabilizing prepared gelatin scaffolds, there are noticeable differences among physical and mechanical properties of samples based on the crosslinker type. Epoxy-crosslinked scaffolds showed a higher capacity for water absorption and more uniform microstructures than the rest of crosslinked samples, whereas genipin and GTA-crosslinked scaffolds demonstrated higher mechanical strength. Cytotoxicity analysis showed the superior biocompatibility of the naturally occurring genipin in comparison with other synthetic crosslinking agents, in particular relative to GTA-crosslinked samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis and characterization of bulk metallic glasses prepared by laser direct deposition

NASA Astrophysics Data System (ADS)

Ye, Xiaoyang

Fe-based and Zr-based metallic glasses have attracted extensive interest for structural applications due to their excellent glass forming ability, superior mechanical properties, unique thermal and corrosion properties. In this study, the feasibility of synthesizing metallic glasses with good ductility by laser direct deposition is explored. Both in-situ synthesis with elemental powder mixture and ex-situ synthesis with prealloyed powder are discussed. Microstructure and properties of laser direct deposited metallic glass composites are analyzed. Synthesis of Fe-Cr-Mo-W-Mn-C-Si-B metallic glass composite with a large fraction of amorphous phase was accomplished using laser direct deposition. X-ray diffraction (XRD) and transmission electron microscopy investigations revealed the existence of amorphous structure. Microstructure analyses by optical microscopy and scanning electron microscopy (SEM) indicated the periodically repeated microstructures of amorphous and crystalline phases. Partially crystallized structure brought by laser reheating and remelting during subsequent laser scans aggregated in the overlapping area between each scan. XRD analysis showed that the crystalline particle embedded in the amorphous matrix was Cr 1.07Fe18.93 phase. No significant microstructural differences were found from the first to the last layer. Microhardness of the amorphous phase (HV0.2 1591) showed a much higher value than that of the crystalline phase (HV0.2 947). Macrohardness of the top layer had a value close to the microhardness of the amorphous region. Wear resistance property of deposited layers showed a significant improvement with the increased fraction of amorphous phase. Zr65Al10Ni10Cu15 amorphous composites with a large fraction of amorphous phase were in-situ synthesized by laser direct deposition. X-ray diffraction confirmed the existence of both amorphous and crystalline phases. Laser parameters were optimized in order to increase the fraction of amorphous phase. The microstructure analysis by scanning electron microscopy revealed the deposited structure was composed of periodically repeated amorphous and crystalline phases. Overlapping regions with nanoparticles aggregated were crystallized by laser reheating and remelting processes during subsequent laser scans. Vickers microhardness of the amorphous region showed around 35% higher than that of crystalline region. Average hardness obtained by a Rockwell macrohardness tester was very close to the microhardness of the amorphous region. The compression test showed that the fracture strain of Zr65Al10Ni10Cu15 amorphous composites was enhanced from less than 2% to as high as 5.7%, compared with fully amorphous metallic glass. Differential scanning calorimetry test results further revealed the amorphous structure and glass transition temperature Tg was observed to be around 655K. In 3 mol/L NaCl solution, laser direct deposited amorphous composites exhibited distinctly improved corrosion resistance, compared with fully-crystallized samples.

Fatigue Damage Assessment Leveraging Nondestructive Evaluation Data

NASA Astrophysics Data System (ADS)

Mazur, K.; Wisner, B.; Kontsos, A.

2018-05-01

Fatigue in materials depends on several microstructural parameters. The length and time scales involved in such processes have been investigated by characterization methods that target microstructural effects or that rely on specimen-level observations. Combinations of in situ and ex situ techniques are also used to correlate microstructural changes to bulk properties. We present herein an effort to directly link local changes with specimen-level fatigue damage assessment. To achieve this goal, grain-scale observations in an aluminum alloy are linked with deformation measurements made by digital image correlation and with acoustic emission monitoring obtained from inside the scanning electron microscope. Damage assessment is attempted using a data-processing framework that involves noise removal, data reduction, and classification. The results demonstrate that nondestructive evaluation combined with small-scale testing can provide a means for fatigue damage assessment applicable to a broad range of materials and testing conditions.

Computational Simulation of Thermal and Spattering Phenomena and Microstructure in Selective Laser Melting of Inconel 625

NASA Astrophysics Data System (ADS)

Özel, Tuğrul; Arısoy, Yiğit M.; Criales, Luis E.

Computational modelling of Laser Powder Bed Fusion (L-PBF) processes such as Selective laser Melting (SLM) can reveal information that is hard to obtain or unobtainable by in-situ experimental measurements. A 3D thermal field that is not visible by the thermal camera can be obtained by solving the 3D heat transfer problem. Furthermore, microstructural modelling can be used to predict the quality and mechanical properties of the product. In this paper, a nonlinear 3D Finite Element Method based computational code is developed to simulate the SLM process with different process parameters such as laser power and scan velocity. The code is further improved by utilizing an in-situ thermal camera recording to predict spattering which is in turn included as a stochastic heat loss. Then, thermal gradients extracted from the simulations applied to predict growth directions in the resulting microstructure.

Multiscale Modeling and Process Optimization for Engineered Microstructural Complexity

DTIC Science & Technology

2007-10-26

R. C. Rogan, E. Üstündag, M. R. Daymond and V. Knoblauch Ferroelastic Behavior of PZT -Based Ferroelectric Ceramics , Materials Science Forum, 404...Bhattacharya, Materials Science Seminar, University of Southern California, 2003. 42. R.C. Rogan, Texture and Strain Analysis of PZT by In-Situ...Annual Meeting of the American Ceramic Society, St. Louis, MO; May 2002. 44. R. Rogan, Ferroelastic Behavior of PZT -Based Ferroelectric Ceramics , 6th

Catalytic graphitization behavior of phenolic resins by addition of in situ formed nano-Fe particles

NASA Astrophysics Data System (ADS)

Rastegar, H.; Bavand-vandchali, M.; Nemati, A.; Golestani-Fard, F.

2018-07-01

This work presents the catalytic graphitization process of phenolic resins (PR's) by addition of in situ nano-Fe particles as catalyst. Pyrolysis treatments of prepared compositions including various contents of nano-Fe particles were carried out at 600-1200 °C for 3 h under reducing atmosphere and graphitization process were evaluated by different techniques such as X-Ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM), High Resolution Transmission Electron Microscopy (HRTEM), Simultaneous Thermal Analysis (STA) and Raman spectroscopy that mainly performed to identify the phase and microstructural analysis, oxidation resistance and extend of graphitized carbon formation. Results indicate that, in situ graphitic carbon development were already observed after firing the samples at 800 °C for 3 h under reducing atmosphere, increasing temperature and amount of nano-Fe led to a more effective graphitization level. In addition, the different nano crystalline carbon shapes such as onion and bamboo like and carbon nanotubes (CNTs) were in situ identified during graphitization process of nano-Fe containing samples. It was suggested that formation of these different nano carbon structures related to nano-Fe catalyst behavior and the carbon shell growth.

Metastable tantalum oxide formation during the devitrification of amorphous tantalum thin films

DOE PAGES

Donaldson, Olivia K.; Hattar, Khalid; Trelewicz, Jason R.

2016-07-04

Microstructural evolution during the devitrification of amorphous tantalum thin films synthesized via pulsed laser deposition was investigated using in situ transmission electron microscopy (TEM) combined with ex situ isothermal annealing, bright-field imaging, and electron-diffraction analysis. The phases formed during crystallization and their stability were characterized as a function of the chamber pressure during deposition, devitrification temperature, and annealing time. A range of metastable nanocrystalline tantalum oxides were identified following devitrification including multiple orthorhombic oxide phases, which often were present with, or evolved to, the tetragonal TaO 2 phase. While the appearance of these phases indicated the films were evolving tomore » the stable form of tantalum oxide—monoclinic tantalum pentoxide—it was likely not achieved for the conditions considered due to an insufficient amount of oxygen present in the films following deposition. Nevertheless, the collective in situ and ex situ TEM analysis applied to thin film samples enabled the isolation of a number of metastable tantalum oxides. As a result, new insights were gained into the transformation sequence and stability of these nanocrystalline phases, which presents opportunities for the development of advanced tantalum oxide-based dielectric materials for novel memristor designs.« less

Homogenization kinetics of a nickel-based superalloy produced by powder bed fusion laser sintering

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

Zhang, Fan; Levine, Lyle E.; Allen, Andrew J.

2017-04-01

Additively manufactured (AM) metal components often exhibit fine dendritic microstructures and elemental segregation due to the initial rapid solidification and subsequent melting and cooling during the build process, which without homogenization would adversely affect materials performance. In this letter, we report in situ observation of the homogenization kinetics of an AM nickel-based superalloy using synchrotron small angle X-ray scattering. The identified kinetic time scale is in good agreement with thermodynamic diffusion simulation predictions using microstructural dimensions acquired by ex situ scanning electron microscopy. These findings could serve as a recipe for predicting, observing, and validating homogenization treatments in AM materials.

Homogenization Kinetics of a Nickel-based Superalloy Produced by Powder Bed Fusion Laser Sintering.

PubMed

Zhang, Fan; Levine, Lyle E; Allen, Andrew J; Campbell, Carelyn E; Lass, Eric A; Cheruvathur, Sudha; Stoudt, Mark R; Williams, Maureen E; Idell, Yaakov

2017-04-01

Additively manufactured (AM) metal components often exhibit fine dendritic microstructures and elemental segregation due to the initial rapid solidification and subsequent melting and cooling during the build process, which without homogenization would adversely affect materials performance. In this letter, we report in situ observation of the homogenization kinetics of an AM nickel-based superalloy using synchrotron small angle X-ray scattering. The identified kinetic time scale is in good agreement with thermodynamic diffusion simulation predictions using microstructural dimensions acquired by ex situ scanning electron microscopy. These findings could serve as a recipe for predicting, observing, and validating homogenization treatments in AM materials.

In Situ Study of Microstructure Evolution in Solidification of Hypereutectic Al-Si Alloys with Application of Thermal Analysis and Neutron Diffraction

NASA Astrophysics Data System (ADS)

Sediako, Dimitry G.; Kasprzak, Wojciech

2015-09-01

Understanding of the kinetics of solid-phase evolution in solidification of hypereutectic aluminum alloys is a key to control their as-cast microstructure and resultant mechanical properties, and in turn, to enhance the service characteristics of actual components. This study was performed to evaluate the solidification kinetics for three P-modified hypereutectic Al-19 pct Si alloys: namely, Al-Si binary alloy and with the subsequent addition of 2.8 pct Cu and 2.8 pct Cu + 0.7 pct Mg. Metallurgical evaluation included thermodynamic calculations of the solidification process using the FactSage™ 6.2 software package, as well as experimental thermal analysis, and in situ neutron diffraction. The study revealed kinetics of solid α-Al, solid Si, Al2Cu, and Mg2Si evolution, as well as the individual effects of Cu and Mg alloying additions on the solidification path of the Al-Si system. Various techniques applied in this study resulted in some discrepancies in the results. For example, the FactSage computations, in general, resulted in 281 K to 286 K (8 °C to 13 °C) higher Al-Si eutectic temperatures than the ones recorded in the thermal analysis, which are also ~278 K (~5 °C) higher than those observed in the in situ neutron diffraction. None of the techniques can provide a definite value for the solidus temperature, as this is affected by the chosen calculation path [283 K to 303 K (10 °C to 30 °C) higher for equilibrium solidification vs non-equilibrium] for the FactSage analysis; and further complicated by evolution of secondary Al-Cu and Mg-Si phases that commenced at the end of solidification. An explanation of the discrepancies observed and complications associated with every technique applied is offered in the paper.

The nanostructure and microstructure of SiC surface layers deposited by MWCVD and ECRCVD

NASA Astrophysics Data System (ADS)

Dul, K.; Jonas, S.; Handke, B.

2017-12-01

Scanning electron microscopy (SEM) and Atomic force microscopy (AFM) have been used to investigate ex-situ the surface topography of SiC layers deposited on Si(100) by Microwave Chemical Vapour Deposition (MWCVD) -S1,S2 layers and Electron Cyclotron Resonance Chemical Vapor Deposition (ECRCVD) - layers S3,S4, using silane, methane, and hydrogen. The effects of sample temperature and gas flow on the nanostructure and microstructure have been investigated. The nanostructure was described by three-dimensional surface roughness analysis based on digital image processing, which gives a tool to quantify different aspects of surface features. A total of 13 different numerical parameters used to describe the surface topography were used. The scanning electron image (SEM) of the microstructure of layers S1, S2, and S4 was similar, however, layer S3 was completely different; appearing like grains. Nonetheless, it can be seen that no grain boundary structure is present in the AFM images.

Analysis of high temperature deformation mechanism in ODS EUROFER97 alloy

NASA Astrophysics Data System (ADS)

Ramar, A.; Spätig, P.; Schäublin, R.

2008-12-01

Oxide dispersion in tempered martensitic EUROFER97 steel is an efficient approach to improve its strength. The oxide dispersion strengthened (ODS) EUROFER97 steel shows a good strength up to 600 °C, but degrades rapidly beyond that temperature. To understand the origin in the microstructure of this drop in strength in situ heating experiment in TEM was performed from room temperature to 1000 °C. Upon heating neither microstructure changes nor dislocation movement are observed up to 600 °C. Movement of dislocations are observed above 680 °C. Phase transformation to austenite starts at 840 °C. Yttria particles remain stable up to 1000 °C. Changes in mechanical properties thus do not relate to changes in yttria dispersion. It is attempted to relate these observations to the thermal activation parameters measured by the technique of conventional strain rate experiment, which allow to identify at a mesoscopic scale the microstructural mechanisms responsible for the degradation of ODS steel at high temperatures.

Three dimensional characterization of nickel coarsening in solid oxide cells via ex-situ ptychographic nano-tomography

NASA Astrophysics Data System (ADS)

De Angelis, Salvatore; Jørgensen, Peter Stanley; Tsai, Esther Hsiao Rho; Holler, Mirko; Kreka, Kosova; Bowen, Jacob R.

2018-04-01

Nickel coarsening is considered a significant cause of solid oxide cell (SOC) performance degradation. Therefore, understanding the morphological changes in the nickel-yttria stabilized zirconia (Ni-YSZ) fuel electrode is crucial for the wide spread usage of SOC technology. This paper reports a study of the initial 3D microstructure evolution of a SOC analyzed in the pristine state and after 3 and 8 h of annealing at 850 °C, in dry hydrogen. The analysis of the evolution of the same location of the electrode shows a substantial change of the nickel and pore network during the first 3 h of treatment, while only negligible changes are observed after 8 h. The nickel coarsening results in loss of connectivity in the nickel network, reduced nickel specific surface area and decreased total triple phase boundary density. For the condition of this experiment, nickel coarsening is shown to be predominantly curvature driven, and changes in the electrode microstructure parameters are discussed in terms of local microstructural evolution.

Selective Internal Oxidation and Severe Plastic Deformation of Multiphase Fe-Y Alloys

NASA Astrophysics Data System (ADS)

Kachur, Stephen J.

Oxide dispersion strengthened (ODS) alloys are known for their desirable mechanical properties and unique microstructures. These alloys are characterized by an even dispersion of oxide phase throughout a metallic matrix, and exhibit high strength and enhanced creep properties at elevated temperatures. This makes them ideal candidate materials for use in many structural applications, such as coal-fired power plants or in next generation nuclear reactors. Currently most often produced by mechanical alloying, a powder metallurgy based process that utilizes high energy ball milling, these alloys are difficult and costly to produce. One proposed method for forming ODS alloys without high-energy ball milling is to internally oxidize a bulk alloy before subjecting it to severe plastic deformation to induce an even oxide distribution. This work examines such a processing scheme with a focus on the internal oxidation behavior. Internal oxidation has been shown to occur orders of magnitude faster than expected in multi-phase alloys where a highly reactive oxidizable solute has negligible solubility and diffusivity in other, more-noble, phases. Commonly referred to as in situ oxidation, this accelerated oxidation process has potential for use in a processing scheme for ODS alloys. While in situ oxidation has been observed in many different alloy systems, a comprehensive study of alloy composition and microstructure has not been performed to describe the unusual oxidation rates. This work used Fe-Y binary alloys as model system to study effects of composition and microstructure. These alloys have been shown to exhibit in situ oxidation, and additionally, Y is typically introduced during mechanical alloying to form Y-rich oxides in Fe-based ODS alloys. Alloys with Y content between 1.5 and 15 wt% were prepared using a laboratory scale arc-melting furnace. These alloys were two phase mixtures of Fe and Fe17Y2. First, samples were oxidized between 600 and 800 °C for 2 to 72 hours, using a Rhines pack to maintain low oxygen partial pressures so that in situ oxidation could occur. Oxidation rates were accelerated when compared to traditional theory, and were not well described by a single parabolic rate constant throughout the duration of the experiment. While results agreed with Wagner theory that increased Y content should lead to decreased oxidation rates, this was attributed to a depletion of oxygen supply from the Rhines pack over time. Samples were also subjected to plastic deformation to observe how changes in microstructure influenced kinetics. Connectivity of the oxidizable phase was found to be critical to promoting the fastest rates of oxidation. Oxidation studies where then carried out using thermogravimetric analysis. A gaseous mixture of Ar-H2 was passed through a dew point control unit to vary oxidant partial pressure between 10-25 and 10-20 atm. Flow rate of the gas parallel to the sample surface was also altered. Canonical correlation analysis was then used to analyze and simplify the relationships between input and output variables. This analysis pointed to the importance of quantifying the relationship between the size of formed oxides and changes in oxidation kinetics over time. Where sustained parabolic kinetics were observed, oxides were small throughout the depth of internal oxidation. The effects of oxide size on penetration depth were then numerically modeled and incorporated into existing oxidation theory to show that the observed kinetics could be qualitatively described. After oxidation experiments, severe plastic deformation was applied to both oxidized and unoxidized microstructures using equal channel angular pressing. By manipulating pressing temperature and the number of passes, microstructures were altered to varying degrees of success. No oxide refinement was observed, but increasing temperatures and number of passes allowed for even dispersion of both oxides and Fe17Y2 intermetallic.

Evaluation of in-situ deformation experiments of TRIP steel

NASA Astrophysics Data System (ADS)

Procházka, J.; Kučerová, L.; Bystrianský, M.

2017-02-01

The paper reports on the behaviour of low alloyed TRIP (transformation induced plasticity) steel with Niobium during tensile test. The structures were analysed using in-situ tensile testing coupled with electron backscattering diffraction (EBSD) analysis carried out in scanning electron microscope (SEM). Steel specimens were of same chemical composition; however three different annealing temperatures, 800 °C, 850 °C and 950 °C, were applied to the material during the heat treatment. The treatment consisted of annealing for 20 minutes in the furnace; cooling in salt bath after the heating and holding at 425 °C for 20 minutes for all the samples. Untreated bar was used as reference material. Flat samples for deformation stage were cut out of the heat-treated bars. In situ documentation of microstructure and crystallography development were carried out during the deformation experiments. High deformation lead to significant degradation of EBSD signal.

Evolution of Near-Surface Internal and External Oxide Morphology During High-Temperature Selective Oxidation of Steels

NASA Astrophysics Data System (ADS)

Story, Mary E.; Webler, Bryan A.

2018-05-01

In this work we examine some observations made using high-temperature confocal scanning laser microscopy (HT-CSLM) during selective oxidation experiments. A plain carbon steel and advanced high-strength steel (AHSS) were selectively oxidized at high temperature (850-900°C) in either low oxygen or water vapor atmospheres. Surface evolution, including thermal grooving along grain boundaries and oxide growth, was viewed in situ during heating. Experiments investigated the influence of the microstructure and oxidizing atmosphere on selective oxidation behavior. Sequences of CSLM still frames collected during the experiment were processed with ImageJ to obtain histograms that showed a general darkening trend indicative of oxidation over time with all samples. Additional ex situ scanning electron microscopy and energy dispersive spectroscopy analysis supported in situ observations. Distinct oxidation behavior was observed for each case. Segregation, grain orientation, and extent of internal oxidation were all found to strongly influence surface evolution.

In Situ formation of microstructures near live cells using spatially structured near-infrared laser microbeam

NASA Astrophysics Data System (ADS)

Ingle, Ninad; Gu, Ling; Mohanty, Samarendra K.

2011-03-01

Here, we report in situ formation of microstructures from the regular constituents of culture media near live cells using spatially-structured near infrared (NIR) laser beam. Irradiation with the continuous wave (cw) NIR laser microbeam for few seconds onto the regular cell culture media containing fetal bovine serum resulted in accumulation of dense material inside the media as evidenced by phase contrast microscopy. The time to form the phase dense material was found to depend on the laser beam power. Switching off the laser beam led to diffusion of phase dark material. However, the proteins could be stitched together by use of carbon nanoparticles and continuous wave (cw) Ti: Sapphire laser beam. Further, by use of spatially-structured beam profiles different structures near live cells could be formed. The microfabricated structure could be held by the Gravito-optical trap and repositioned by movement of the sample stage. Orientation of these microstructures was achieved by rotating the elliptical laser beam profile. Thus, multiple microstructures were formed and organized near live cells. This method would enable study of response of cells/axons to the immediate physical hindrance provided by such structure formation and also eliminate the biocompatibility requirement posed on artificial microstructure materials.

In-situ Observation of Cross-Sectional Microstructural Changes and Stress Distributions in Fracturing TiN Thin Film during Nanoindentation.

PubMed

Zeilinger, Angelika; Todt, Juraj; Krywka, Christina; Müller, Martin; Ecker, Werner; Sartory, Bernhard; Meindlhumer, Michael; Stefenelli, Mario; Daniel, Rostislav; Mitterer, Christian; Keckes, Jozef

2016-03-07

Load-displacement curves measured during indentation experiments on thin films depend on non-homogeneous intrinsic film microstructure and residual stress gradients as well as on their changes during indenter penetration into the material. To date, microstructural changes and local stress concentrations resulting in plastic deformation and fracture were quantified exclusively using numerical models which suffer from poor knowledge of size dependent material properties and the unknown intrinsic gradients. Here, we report the first in-situ characterization of microstructural changes and multi-axial stress distributions in a wedge-indented 9 μm thick nanocrystalline TiN film volume performed using synchrotron cross-sectional X-ray nanodiffraction. During the indentation, needle-like TiN crystallites are tilted up to 15 degrees away from the indenter axis in the imprint area and strongly anisotropic diffraction peak broadening indicates strain variation within the X-ray nanoprobe caused by gradients of giant compressive stresses. The morphology of the multiaxial stress distributions with local concentrations up to -16.5 GPa correlate well with the observed fracture modes. The crack growth is influenced decisively by the film microstructure, especially by the micro- and nano-scopic interfaces. This novel experimental approach offers the capability to interpret indentation response and indenter imprint morphology of small graded nanostructured features.

Controllable Synthesis of Tunable Microstructures of Self-Supporting Graphene Films from Opened Bubble to Cube via in Situ Template-Modulating.

PubMed

Li, Na; Yang, Qiao; Liu, Xing; Huang, Xuankai; Zhang, Haiyan; Wang, Chengxin

2017-12-06

Three-dimensional (3D) microstructured building units have replaced layer-to-layer stacked designs in transparent graphene films to fully exploit the advantages of two-dimensional graphene. However, it is still challenging to precisely control the size and microstructures of these building blocks to develop multifunctional graphene-based materials that satisfy the performance requirements of diverse applications. In this study, we propose a controllable method to regulate the microstructures of building units to form structures ranging from opened bubbles and cubes, while the size decreased from 20 to 3 μm, via an in situ template-modulating technology. NaCl was used as either a liquid or solid template by changing the dc bias. The reduced size and dense arrangement of the building units not only provide an improved mass loading for the transparent films but also build multiple pathways for fast ion/electron transmission, enhancing their promise for various practical applications. Generally, we provide a convenient protocol for finely regulating the microstructure and size of these building units, resulting in multifunctional films with a controllable transmittance, which enables the use of these graphene-based architectures as transparent electrodes in various applications and extends the family of multifunctional materials that will present new possibilities for electronics and other devices.

Thermomechanical In Situ Monitoring of Bi2Te3 Thin Film and Its Relationship with Microstructure and Thermoelectric Performances

NASA Astrophysics Data System (ADS)

Jeong, Min-Woo; Na, Sekwon; Shin, Haishan; Park, Hong-Bum; Lee, Hoo-Jeong; Joo, Young-Chang

2018-07-01

Performance enhancement has been studied for thin-film thermoelectric materials for small-scale energy applications. The microstructural evolution of bismuth telluride (Bi2Te3) was investigated with respect to performance enhancement via in situ thermomechanical analysis due to the post-annealing process. The thermomechanical behavior of Bi2Te3 changes gradually at approximately 200 °C with the formation of a quintuple-layer structure, which was confirmed by X-ray diffraction, transmission electron microscopy and Raman spectroscopy. It was found that highly oriented (006), (0015) was formed with a quintuple-layer structure parallel to the substrate, and the E g 2 Raman vibration mode of Bi2Te3 significantly increased after forming the layer structure with decreased defects. Therefore, the slope of the stress curve was affected by the longer atomic distance of the van der Waals bonds with the formation of (00 l) oriented layered-structure grain. The decreased number of defects in the layer structure affects the electrical and thermal properties of the Bi2Te3 thin film. Due to the microstructural evolution, the power factor of Bi2Te3 was enhanced by approximately 14.8 times by the quintuple-layer structure of Bi2Te3 formed during the annealing process, which contributed to a better understanding of the performance enhancement via post-annealing and to research on other highly oriented layer structure materials.

Thermomechanical In Situ Monitoring of Bi2Te3 Thin Film and Its Relationship with Microstructure and Thermoelectric Performances

NASA Astrophysics Data System (ADS)

Jeong, Min-Woo; Na, Sekwon; Shin, Haishan; Park, Hong-Bum; Lee, Hoo-Jeong; Joo, Young-Chang

2018-04-01

Performance enhancement has been studied for thin-film thermoelectric materials for small-scale energy applications. The microstructural evolution of bismuth telluride (Bi2Te3) was investigated with respect to performance enhancement via in situ thermomechanical analysis due to the post-annealing process. The thermomechanical behavior of Bi2Te3 changes gradually at approximately 200 °C with the formation of a quintuple-layer structure, which was confirmed by X-ray diffraction, transmission electron microscopy and Raman spectroscopy. It was found that highly oriented (006), (0015) was formed with a quintuple-layer structure parallel to the substrate, and the Eg 2Raman vibration mode of Bi2Te3 significantly increased after forming the layer structure with decreased defects. Therefore, the slope of the stress curve was affected by the longer atomic distance of the van der Waals bonds with the formation of (00l) oriented layered-structure grain. The decreased number of defects in the layer structure affects the electrical and thermal properties of the Bi2Te3 thin film. Due to the microstructural evolution, the power factor of Bi2Te3 was enhanced by approximately 14.8 times by the quintuple-layer structure of Bi2Te3 formed during the annealing process, which contributed to a better understanding of the performance enhancement via post-annealing and to research on other highly oriented layer structure materials.

In Situ Foaming of Porous (La 0.6 Sr 0.4 ) 0.98 (Co 0.2 Fe 0.8 ) O 3-δ (LSCF) Cathodes for Solid Oxide Fuel Cell Applications

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

Gandavarapu, Sodith; Sabolsky, Edward; Sabolsky, Katarzyna

2013-07-18

A binder system containing polyurethane precursors was used to in situ foam (direct foam) a (La{sub 0.6}Sr{sub 0.4}){sub 0.98} (Co{sub 0.2} Fe{sub 0.8}) O{sub 3-{ delta}} (LSCF) composition for solid oxide fuel cell (SOFC) cathode applications. The relation between in situ foaming parameters on the final microstructure and electrochemical properties was characterized by microscopy and electrochemical impedance spectroscopy (EIS), respectively. The optimal porous cathode architecture was formed with a 70 vol% solids loading within a polymer precursor composition with a volume ratio of 8:4:1 (isocyanate: PEG: surfactant) in a terpineol-based ink vehicle. The resultant microstructure displayed a broad pore sizemore » distribution with highly elongated pore structure.« less

Absorption kinetics of vitamin E nanoemulsion and green tea microstructures by intestinal in situ single perfusion technique in rats.

PubMed

Saratale, Rijuta Ganesh; Lee, Hee-Seok; Koo, Yong Eui; Saratale, Ganesh Dattatraya; Kim, Young Jun; Imm, Jee Young; Park, Yooheon

2018-04-01

The absorption kinetics of food ingredients such as nanoemulsified vitamin E and green tea microstructures were evaluated by the intestinal in situ single perfusion technique. Absorption rate, sub-acute oral toxicity and organ morphology in a rat model were examined. The intestinal in situ single perfusion technique and HPLC analysis were applied to investigate the absorption rate of selected materials by examining time-dependent changes in the serum levels of catechin and dl-α-tocopherol. The acute toxicity test and histopathological evaluation were applied to analyze the safety of microsized green tea and nanosized vitamin E in a rat model. Total serum dl-α-tocopherol levels significantly increased with nanosized vitamin E administration (P<0.05). Rats treated to nanosized vitamin E until 90min after administration showed significantly increased absorption rate of serum dl-α-tocopherol levels at each time point (10min interval) (P<0.001). Rats administered 2000mg/kg of nanosized vitamin E and microsized green tea did not show signs of acute toxicity or death after 14days of observation. In addition, macroscopic analysis showed that there were no changes in representative organ sections of rats following the oral administration of food-related nanoscale materials. We successfully demonstrated that using nanosized vitamin E increased absorption rate to a greater extent than normal food-related material, and these results occurs via safety analyses on food-related nanoscale materials for human consumption. These results could be useful for the design and development of novel nanoemulsified vitamin E and microsized green tea formulations that can overcome the problem of their bioavailability and improve their efficacy while still maintaining their essential therapeutic efficacies. Copyright © 2018 Elsevier Ltd. All rights reserved.

Densification of LSGM electrolytes using activated microwave sintering

NASA Astrophysics Data System (ADS)

Kesapragada, S. V.; Bhaduri, S. B.; Bhaduri, S.; Singh, P.

Lanthanum gallate doped with alkaline rare earths (LSGM) powders were densified using an activated microwave sintering process for developing a dense stable electrolyte layer for applications in intermediate temperature-solid oxide fuel cells (IT-SOFCs). Due to heat generation in situ, the process of sintering gets activated with faster kinetics compared to a conventional sintering process. The effect of various microwave process parameters on the microstructure and phase formation was studied. The sintered pellets were characterized using scanning electron microscopy-energy dispersive analysis (SEM-EDAX), and X-ray diffraction (XRD). The density of LSGM pellets microwave sintered at 1350 °C for 20 min is greater than 95% theoretical density with a fine grained microstructure (˜2-3 μm) and without the presence of other phase(s).

In situ roughening of polymeric microstructures.

PubMed

Shadpour, Hamed; Allbritton, Nancy L

2010-04-01

A method to perform in situ roughening of arrays of microstructures weakly adherent to an underlying substrate was presented. SU8, 1002F, and polydimethylsiloxane (PDMS) microstructures were roughened by polishing with a particle slurry. The roughness and the percentage of dislodged or damaged microstructures was evaluated as a function of the roughening time for both SU8 and 1002F structures. A maximal RMS roughness of 7-18 nm for the surfaces was obtained within 15-30 s of polishing with the slurry. This represented a 4-9 fold increase in surface roughness relative to that of the native surface. Less than 0.8% of the microstructures on the array were removed or damaged after 5 min of polishing. Native and roughened arrays were assessed for their ability to support fibronectin adhesion and cell attachment and growth. The quantity of adherent fibronectin was increased on roughened arrays by two-fold over that on native arrays. Cell adhesion to the roughened surfaces was also increased compared to native surfaces. Surface roughening with the particle slurry also improved the ability to stamp molecules onto the substrate during microcontact printing. Roughening both the PDMS stamp and substrate resulted in up to a 20-fold improvement in the transfer of BSA-Alexa Fluor 647 from the stamp to the substrate. Thus roughening of micrometer-scale surfaces with a particle slurry increased the adhesion of biomolecules as well as cells to microstructures with little to no damage to largescale arrays of the structures.

In-Situ Roughening of Polymeric Microstructures

PubMed Central

Shadpour, Hamed; Allbritton, Nancy L.

2010-01-01

A method to perform in-situ roughening of arrays of microstructures weakly adherent to an underlying substrate was presented. SU8, 1002F, and polydimethylsiloxane (PDMS) microstructures were roughened by polishing with a particle slurry. The roughness and the percentage of dislodged or damaged microstructures was evaluated as a function of the roughening time for both SU8 and 1002F structures. A maximal RMS roughness of 7-18 nm for the surfaces was obtained within 15 to 30 s of polishing with the slurry. This represented a 4-9 fold increase in surface roughness relative to that of the native surface. Less than 0.8% of the microstructures on the array were removed or damage after 5 min of polishing. Native and roughened arrays were assessed for their ability to support fibronectin adhesion and cell attachment and growth. The quantity of adherent fibronectin was increased on roughened arrays by two-fold over that on native arrays. Cell adhesion to the roughened surfaces was also increased compared to native surfaces. Surface roughening with the particle slurry also improved the ability to stamp molecules onto the substrate during microcontact printing. Roughening both the PDMS stamp and substrate resulted in up to a 20-fold improvement in the transfer of BSA-Alexa Fluor 647 from the stamp to the substrate. Thus roughening of micron-scale surfaces with a particle slurry increased the adhesion of biomolecules as well as cells to microstructures with little to no damage to large scale arrays of the structures. PMID:20423129

Visualizing Stress and Temperature Distribution During Elevated Temperature Deformation of IN-617 Using Nanomechanical Raman Spectroscopy

NASA Astrophysics Data System (ADS)

Zhang, Yang; Wang, Hao; Tomar, Vikas

2018-04-01

This work presents direct measurements of stress and temperature distribution during the mesoscale microstructural deformation of Inconel-617 (IN-617) during 3-point bending tests as a function of temperature. A novel nanomechanical Raman spectroscopy (NMRS)-based measurement platform was designed for simultaneous in situ temperature and stress mapping as a function of microstructure during deformation. The temperature distribution was found to be directly correlated to stress distribution for the analyzed microstructures. Stress concentration locations are shown to be directly related to higher heat conduction and result in microstructural hot spots with significant local temperature variation.

Formation of Foam-like Microstructural Carbon Material by Carbonization of Porous Coordination Polymers through a Ligand-Assisted Foaming Process.

PubMed

Kongpatpanich, Kanokwan; Horike, Satoshi; Fujiwara, Yu-Ichi; Ogiwara, Naoki; Nishihara, Hirotomo; Kitagawa, Susumu

2015-09-14

Porous carbon material with a foam-like microstructure has been synthesized by direct carbonization of porous coordination polymer (PCP). In situ generation of foaming agents by chemical reactions of ligands in PCP during carbonization provides a simple way to create lightweight carbon material with a foam-like microstructure. Among several substituents investigated, the nitro group has been shown to be the key to obtain the unique foam-like microstructure, which is due to the fast kinetics of gas evolution during carbonization. Foam-like microstructural carbon materials showed higher pore volume and specific capacitance compared to a microporous carbon. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimized Setup and Protocol for Magnetic Domain Imaging with In Situ Hysteresis Measurement

PubMed Central

Liu, Jun; Wilson, John; Davis, Claire; Peyton, Anthony

2017-01-01

This paper elaborates the sample preparation protocols required to obtain optimal domain patterns using the Bitter method, focusing on the extra steps compared to standard metallographic sample preparation procedures. The paper proposes a novel bespoke rig for dynamic domain imaging with in situ BH (magnetic hysteresis) measurements and elaborates the protocols for the sensor preparation and the use of the rig to ensure accurate BH measurement. The protocols for static and ordinary dynamic domain imaging (without in situ BH measurements) are also presented. The reported method takes advantage of the convenience and high sensitivity of the traditional Bitter method and enables in situ BH measurement without interrupting or interfering with the domain wall movement processes. This facilitates establishing a direct and quantitative link between the domain wall movement processes–microstructural feature interactions in ferritic steels with their BH loops. This method is anticipated to become a useful tool for the fundamental study of microstructure–magnetic property relationships in steels and to help interpret the electromagnetic sensor signals for non-destructive evaluation of steel microstructures. PMID:29155796

In situ synthesized TiB-TiN reinforced Ti6Al4V alloy composite coatings: microstructure, tribological and in-vitro biocompatibility.

PubMed

Das, Mitun; Bhattacharya, Kaushik; Dittrick, Stanley A; Mandal, Chitra; Balla, Vamsi Krishna; Sampath Kumar, T S; Bandyopadhyay, Amit; Manna, Indranil

2014-01-01

Wear resistant TiB-TiN reinforced Ti6Al4V alloy composite coatings were deposited on Ti substrate using laser based additive manufacturing technology. Ti6Al4V alloy powder premixed with 5wt% and 15wt% of boron nitride (BN) powder was used to synthesize TiB-TiN reinforcements in situ during laser deposition. Influences of laser power, scanning speed and concentration of BN on the microstructure, mechanical, in vitro tribological and biological properties of the coatings were investigated. Microstructural analysis of the composite coatings showed that the high temperature generated due to laser interaction with Ti6Al4V alloy and BN results in situ formation of TiB and TiN phases. With increasing BN concentration, from 5wt% to 15wt%, the Young's modulus of the composite coatings, measured by nanoindentation, increased from 170±5GPa to 204±14GPa. In vitro tribological tests showed significant increase in the wear resistance with increasing BN concentration. Under identical test conditions TiB-TiN composite coatings with 15wt% BN exhibited an order of magnitude less wear rate than CoCrMo alloy-a common material for articulating surfaces of orthopedic implants. Average top surface hardness of the composite coatings increased from 543±21HV to 877±75HV with increase in the BN concentration. In vitro biocompatibility and flow cytometry study showed that these composite coatings were non-toxic, exhibit similar cell-materials interactions and biocompatibility as that of commercially pure titanium (CP-Ti) samples. In summary, excellent in vitro wear resistance, high stiffness and suitable biocompatibility make these composite coatings as a potential material for load-bearing articulating surfaces towards orthopaedic implants. © 2013 Elsevier Ltd. All rights reserved.

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

In-situ electrochemical-AFM study of localized corrosion of AlxCoCrFeNi high-entropy alloys in chloride solution

NASA Astrophysics Data System (ADS)

Shi, Yunzhu; Collins, Liam; Balke, Nina; Liaw, Peter K.; Yang, Bin

2018-05-01

In-situ electrochemical (EC)-AFM is employed to investigate the localized corrosion of the AlxCoCrFeNi high-entropy alloys (HEAs). Surface topography changes on the micro/sub-micro scale are monitored at different applied anodizing potentials in a 3.5 wt% NaCl solution. The microstructural evolutions with the increased Al content in the alloys are characterized by SEM, TEM, EDS and EBSD. The results show that by increasing the Al content, the microstructure changes from single solid-solution to multi-phases, leading to the segregations of elements. Due to the microstructural variations in the AlxCoCrFeNi HEAs, localized corrosion processes in different ways after the breakdown of the passive film, which changes from pitting to phase boundary corrosion. The XPS results indicate that an increased Al content in the alloys/phases corresponds to a decreased corrosion resistance of the surface passive film.

In Situ Imaging during Compression of Plastic Bonded Explosives for Damage Modeling

NASA Astrophysics Data System (ADS)

Yeager, John; Manner, Virginia; Patterson, Brian; Walters, David; Cordes, Nikolaus; Henderson, Kevin; Tappan, Bryce; Luscher, Darby

2017-06-01

The microstructure of plastic bonded explosives (PBXs) is known to influence behavior during insults such as deformation, heating or initiation to detonation. Obtaining three-dimensional microstructural data can be difficult due in part to fragility of the material and small feature size. X-ray computed tomography (CT) is an ideal characterization technique but the explosive crystals and binder in formulations such as PBX 9501 do not have sufficient x-ray contrast to differentiate between the components. Here, we have formulated several PBXs using octahydro-1,3,5,7-tetranitro-1,3,5,7- tetrazocine (HMX) crystals and low-density binder systems. The full three-dimensional microstructure of these samples has been characterized using microscale CT during uniaxial mechanical compression in an interrupted in situ modality. The rigidity of the binder was observed to significantly influence fracture, crystal-binder delamination, and material flow. Additionally, the segmented, 3D images were meshed for finite element simulation. Initial results of the mesoscale modeling exhibit qualitatively similar delamination. Los Alamos National Laboratory - LDRD.

In-situ Observation of Cross-Sectional Microstructural Changes and Stress Distributions in Fracturing TiN Thin Film during Nanoindentation

PubMed Central

Zeilinger, Angelika; Todt, Juraj; Krywka, Christina; Müller, Martin; Ecker, Werner; Sartory, Bernhard; Meindlhumer, Michael; Stefenelli, Mario; Daniel, Rostislav; Mitterer, Christian; Keckes, Jozef

2016-01-01

Load-displacement curves measured during indentation experiments on thin films depend on non-homogeneous intrinsic film microstructure and residual stress gradients as well as on their changes during indenter penetration into the material. To date, microstructural changes and local stress concentrations resulting in plastic deformation and fracture were quantified exclusively using numerical models which suffer from poor knowledge of size dependent material properties and the unknown intrinsic gradients. Here, we report the first in-situ characterization of microstructural changes and multi-axial stress distributions in a wedge-indented 9 μm thick nanocrystalline TiN film volume performed using synchrotron cross-sectional X-ray nanodiffraction. During the indentation, needle-like TiN crystallites are tilted up to 15 degrees away from the indenter axis in the imprint area and strongly anisotropic diffraction peak broadening indicates strain variation within the X-ray nanoprobe caused by gradients of giant compressive stresses. The morphology of the multiaxial stress distributions with local concentrations up to −16.5 GPa correlate well with the observed fracture modes. The crack growth is influenced decisively by the film microstructure, especially by the micro- and nano-scopic interfaces. This novel experimental approach offers the capability to interpret indentation response and indenter imprint morphology of small graded nanostructured features. PMID:26947558

Crystal plasticity analysis of stress partitioning mechanisms and their microstructural dependence in advanced steels

DOE PAGES

Pu, Chao; Gao, Yanfei

2015-01-23

Two-phase advanced steels contain an optimized combination of high yield strength and large elongation strain at failure, as a result of stress partitioning between a hard phase (martensite) and a ductile phase (ferrite or austenite). Provided with strong interfaces between the constituent phases, the failure in the brittle martensite phase will be delayed by the surrounding geometric constraints, while the rule of mixture will dictate a large strength of the composite. To this end, the microstructural design of these composites is imperative especially in terms of the stress partitioning mechanisms among the constituent phases. Based on the characteristic microstructures ofmore » dual phase and multilayered steels, two polycrystalline aggregate models are constructed to simulate the microscopic lattice strain evolution of these materials during uniaxial tensile tests. By comparing the lattice strain evolution from crystal plasticity finite element simulations with advanced in situ diffraction measurements in literature, this study investigates the correlations between the material microstructure and the micromechanical interactions on the intergranular and interphase levels. Finally, it is found that although the applied stress will be ultimately accommodated by the hard phase and hard grain families, the sequence of the stress partitioning on grain and phase levels can be altered by microstructural designs. Implications of these findings on delaying localized failure are also discussed.« less

2D-COS of in situ μ-Raman and in situ IR spectra for structure evolution characterisation of NEP-deposited cobalt oxide catalyst during n-nonane combustion

NASA Astrophysics Data System (ADS)

Chlebda, Damian K.; Jodłowski, Przemysław J.; Jędrzejczyk, Roman J.; Łojewska, Joanna

2017-11-01

New catalytic systems are still in development to meet the challenge of regulations concerning the emission of volatile organic compounds (VOCs). This is because such compounds have a significant impact on air quality and some of them are toxic to the environment and human beings. The catalytic combustion process of VOCs over non-noble metal catalysts is of great interest to researchers. The high conversion parameters and cost effective preparation makes them a valuable alternative to monoliths and noble metal catalysts. In this study, the cobalt catalyst was prepared by non-equilibrium plasma deposition of organic precursor on calcined kanthal steel. Thus prepared, cobalt oxide based microstructural short-channel reactors were tested for n-nonane combustion and the catalyst surfaces were examined by in situ μ-Raman spectroscopy and in situ infrared spectroscopy. The spectra collected at various temperatures were used in generalised two-dimensional correlation analysis to establish the sequential order of spectral intensity changes and correlate the simultaneous changes in bands selectively coupled by different interaction mechanisms. The 2D synchronous and asynchronous contour maps were proved to be a valuable extension to the standard analysis of the temperature dependent 1D spectra.

In situ TEM and synchrotron characterization of U–10Mo thin specimen annealed at the fast reactor temperature regime

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

Yun, Di, E-mail: diyun1979@xjtu.edu.cn; Xi'an Jiao Tong University, 28 Xian Ning West Road, Xi'an 710049; Mo, Kun

2015-12-15

U–Mo metallic alloys have been extensively used for the Reduced Enrichment for Research and Test Reactors (RERTR) program, which is now known as the Office of Material Management and Minimization under the Conversion Program. This fuel form has also recently been proposed as fast reactor metallic fuels in the recent DOE Ultra-high Burnup Fast Reactor project. In order to better understand the behavior of U–10Mo fuels within the fast reactor temperature regime, a series of annealing and characterization experiments have been performed. Annealing experiments were performed in situ at the Intermediate Voltage Electron Microscope (IVEM-Tandem) facility at Argonne National Laboratorymore » (ANL). An electro-polished U–10Mo alloy fuel specimen was annealed in situ up to 700 °C. At an elevated temperature of about 540 °C, the U–10Mo specimen underwent a relatively slow microstructure transition. Nano-sized grains were observed to emerge near the surface. At the end temperature of 700 °C, the near-surface microstructure had evolved to a nano-crystalline state. In order to clarify the nature of the observed microstructure, Laue diffraction and powder diffraction experiments were carried out at beam line 34-ID of the Advanced Photon Source (APS) at ANL. Phases present in the as-annealed specimen were identified with both Laue diffraction and powder diffraction techniques. The U–10Mo was found to recrystallize due to thermally-induced recrystallization driven by a high density of pre-existing dislocations. A separate in situ annealing experiment was carried out with a Focused Ion Beam processed (FIB) specimen. A similar microstructure transition occurred at a lower temperature of about 460 °C with a much faster transition rate compared to the electro-polished specimen. - Highlights: • TEM annealing experiments were performed in situ at the IVEM facility up to fast reactor temperature. • At 540 °C, the U-10Mo specimen underwent a slow microstructure transition where nano-sized grains were observed to emerge. • UO{sub 2} phase exists at the thin area of the as-annealed specimen whereas U-10Mo γ phase dominated at the thicker part. • Bcc γ U-10Mo recrystallized to become nano-meter sized crystallites near the specimen surface. • A separateannealing experiment was conducted with a FIB processed specimen where similar transition occurred at a lower temperature of 460 °C with a faster rate.« less

Volmer-Weber growth stages of polycrystalline metal films probed by in situ and real-time optical diagnostics

NASA Astrophysics Data System (ADS)

Abadias, G.; Simonot, L.; Colin, J. J.; Michel, A.; Camelio, S.; Babonneau, D.

2015-11-01

The Volmer-Weber growth of high-mobility metal films is associated with the development of a complex compressive-tensile-compressive stress behavior as the film deposition proceeds through nucleation of islands, coalescence, and formation of a continuous layer. The tensile force maximum has been attributed to the end of the islands coalescence stage, based on ex situ morphological observations. However, microstructural rearrangements are likely to occur in such films during post-deposition, somewhat biasing interpretations solely based on ex situ analysis. Here, by combining two simultaneous in situ and real-time optical sensing techniques, based on surface differential reflectance spectroscopy (SDRS) and change in wafer curvature probed by multibeam optical stress sensor (MOSS), we provide direct evidence that film continuity does coincide with tensile stress maximum during sputter deposition of a series of metal (Ag, Au, and Pd) films on amorphous SiOx. Stress relaxation after growth interruption was testified from MOSS, whose magnitude scaled with adatom mobility, while no change in SDRS signal could be revealed, ruling out possible changes of the surface roughness at the micron scale.

Spectral and raw quasi in-situ energy dispersive X-ray data captured via a TEM analysis of an ODS austenitic stainless steel sample under 1 MeV Kr2+ high temperature irradiation.

PubMed

Brooks, Adam J; Yao, Zhongwen

2017-10-01

The data presented in this article is related to the research experiment, titled: ' Quasi in-situ energy dispersive X-ray spectroscopy observation of matrix and solute interactions on Y-Ti-O oxide particles in an austenitic stainless steel under 1 MeV Kr 2+ high temperature irradiation' (Brooks et al., 2017) [1]. Quasi in-situ analysis during 1 MeV Kr 2+ 520 °C irradiation allowed the same microstructural area to be observed using a transmission electron microscope (TEM), on an oxide dispersion strengthened (ODS) austenitic stainless steel sample. The data presented contains two sets of energy dispersive X-ray spectroscopy (EDX) data collected before and after irradiation to 1.5 displacements-per-atom (~1.25×10 -3  dpa/s with 7.5×10 14  ions cm -2 ). The vendor software used to process and output the data is the Bruker Esprit v1.9 suite. The data includes the spectral (counts vs. keV energy) of the quasi in-situ scanned region (512×512 pixels at 56k magnification), along with the EDX scanning parameters. The.raw files from the Bruker Esprit v1.9 output are additionally included along with the.rpl data information files. Furthermore included are the two quasi in-situ HAADF images for visual comparison of the regions before and after irradiation. This in-situ experiment is deemed ' quasi' due to the thin foil irradiation taking place at an external TEM facility. We present this data for critical and/or extended analysis from the scientific community, with applications applying to: experimental data correlation, confirmation of results, and as computer based modeling inputs.

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

Yu, Cun; Aoun, Bachir; Cui, Lishan

Microstructure evolution of a cold-drawn NiTi shape memory alloy wire was investigated by means of in-situ synchrotron high-energy X-ray diffraction during continuous heating. The cold-drawn wire contained amorphous regions and nano-crystalline domains in its microstructure. Pair distribution function analysis revealed that the amorphous regions underwent structural relaxation via atomic rearrangement when heated above 100 °C. The nano-crystalline domains were found to exhibit a strong cold work induced lattice strain anisotropy having a preferential <111> fiber orientation along the wire axial direction. The lattice strain anisotropy systematically decreased upon heating above 200 °C, implying a structural recovery. A broad conical texturemore » was formed in the wire specimen after crystallization similar in detail to the initial <111> texture axial orientation of the nano-crystalline domains produced by the severe cold wire drawing deformation.« less

Phase Transformations and Formation of Ultra-Fine Microstructure During Hydrogen Sintering and Phase Transformation (HSPT) Processing of Ti-6Al-4V

NASA Astrophysics Data System (ADS)

Sun, Pei; Fang, Zhigang Zak; Koopman, Mark; Xia, Yang; Paramore, James; Ravi Chandran, K. S.; Ren, Yang; Lu, Jun

2015-12-01

The hydrogen sintering and phase transformation (HSPT) process is a novel powder metallurgy method for producing Ti alloys, particularly the Ti-6Al-4V alloy, with ultra-fine microstructure in the as-sintered state. The ultra-fine microstructure is obtained as a direct result of the use of H2 gas during sintering. The refinement of the microstructure during HSPT is similar to that of thermal hydrogen processing (THP) of bulk Ti alloys. For both THP and HSPT of Ti-6Al-4V alloy, the mechanisms of the grain refinement depend on the phase equilibria and phase transformations in the presence of hydrogen, which are surprisingly still not well established to date and are still subjected to research and debate. In recent work by the present authors, a pseudo-binary phase diagram of (Ti-6Al-4V)-H has been determined by using in situ synchrotron XRD and TGA/DSC techniques. Aided by this phase diagram, the current paper focuses on the series of phase transformations during sintering and cooling of Ti-6Al-4V in a hydrogen atmosphere and the mechanisms for the formation of the ultra-fine microstructures obtained. Using experimental techniques, including in situ synchrotron XRD, SEM, EBSD, and TEM, the microstructural refinement was found to be the result of (1) the precipitation of ultra-fine α/α2 within coarse β grains during an isothermal hold at intermediate temperatures, and (2) the eutectoid transformation of β → α + δ at approximately 473 K (200 °C).

In situ, 3D characterization of the deformation mechanics of a superelastic NiTi shape memory alloy single crystal under multiscale constraint

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

Paranjape, Harshad M.; Paul, Partha P.; Amin-Ahmadi, Behnam

Microstructural elements in NiTi shape memory alloys (SMAs) – precipitates, phase boundaries, inclusions, grain boundaries – can be viewed as sources of multiscale constraint that influence their deformation response. In this paper, we characterized in situ, and in 3D, the deformation and the evolution of microstructure during a tension test in a superelastic NiTi specimen containing some of these sources of constraint. The method used was far-field high-energy X-ray diffraction microscopy (ff-HEDM), complemented by electron microscopy. We simulated the local stress state in the specimen using a microstructural model informed by the experimental data. Using these combined microstructure, deformation, andmore » stress data, we report three phenomena, and relate them to specific sources of constraint. During initial elastic loading, axial lattice strain in austenite increased monotonically. On partial stress-induced phase transformation to martensite, the stress redistributed to both phases leading to a stress relaxation in austenite. The specimen contained a dense distribution of inclusions, which led to the activation of martensite habit plane variants that produce less than theoretical maximum transformation strain. Large Ni 4Ti 3 precipitates potentially contributed to the poor transformation response. Under load, proportional gradients in local rotation and elastic stretch developed in the martensite phase, because of the constraint at phase interfaces. Finally, this combined ff-HEDM, electron microscopy, microstructural simulation toolbox provides a versatile method to understand the effect of constraint on inelastic deformation in other alloys with hierarchical microstructure.« less

In situ, 3D characterization of the deformation mechanics of a superelastic NiTi shape memory alloy single crystal under multiscale constraint

DOE PAGES

Paranjape, Harshad M.; Paul, Partha P.; Amin-Ahmadi, Behnam; ...

2017-11-20

Microstructural elements in NiTi shape memory alloys (SMAs) – precipitates, phase boundaries, inclusions, grain boundaries – can be viewed as sources of multiscale constraint that influence their deformation response. In this paper, we characterized in situ, and in 3D, the deformation and the evolution of microstructure during a tension test in a superelastic NiTi specimen containing some of these sources of constraint. The method used was far-field high-energy X-ray diffraction microscopy (ff-HEDM), complemented by electron microscopy. We simulated the local stress state in the specimen using a microstructural model informed by the experimental data. Using these combined microstructure, deformation, andmore » stress data, we report three phenomena, and relate them to specific sources of constraint. During initial elastic loading, axial lattice strain in austenite increased monotonically. On partial stress-induced phase transformation to martensite, the stress redistributed to both phases leading to a stress relaxation in austenite. The specimen contained a dense distribution of inclusions, which led to the activation of martensite habit plane variants that produce less than theoretical maximum transformation strain. Large Ni 4Ti 3 precipitates potentially contributed to the poor transformation response. Under load, proportional gradients in local rotation and elastic stretch developed in the martensite phase, because of the constraint at phase interfaces. Finally, this combined ff-HEDM, electron microscopy, microstructural simulation toolbox provides a versatile method to understand the effect of constraint on inelastic deformation in other alloys with hierarchical microstructure.« less

Analysis of Particle-Stimulated Nucleation (PSN)-Dominated Recrystallization for Hot-Rolled 7050 Aluminum Alloy

NASA Astrophysics Data System (ADS)

Adam, Khaled F.; Long, Zhengdong; Field, David P.

2017-04-01

In 7xxx series aluminum alloys, the constituent large and small second-phase particles present during deformation process. The fraction and spatial distribution of these second-phase particles significantly influence the recrystallized structure, kinetics, and texture in the subsequent treatment. In the present work, the Monte Carlo Potts model was used to model particle-stimulated nucleation (PSN)-dominated recrystallization and grain growth in high-strength aluminum alloy 7050. The driving force for recrystallization is deformation-induced stored energy, which is also strongly affected by the coarse particle distribution. The actual microstructure and particle distribution of hot-rolled plate were used as an initial point for modeling of recrystallization during the subsequent solution heat treatment. Measurements from bright-field TEM images were performed to enhance qualitative interpretations of the developed microstructure. The influence of texture inhomogeneity has been demonstrated from a theoretical point of view using pole figures. Additionally, in situ annealing measurements in SEM were performed to track the orientational and microstructural changes and to provide experimental support for the recrystallization mechanism of PSN in AA7050.

Microstructure Evolution and Mechanical Properties of Al-TiB2/TiC In Situ Aluminum-Based Composites during Accumulative Roll Bonding (ARB) Process

PubMed Central

Nie, Jinfeng; Wang, Fang; Li, Yusheng; Cao, Yang; Liu, Xiangfa; Zhao, Yonghao; Zhu, Yuntian

2017-01-01

In this study, a kind of Al-TiB2/TiC in situ composite was successfully prepared using the melt reaction method and the accumulative roll-bonding (ARB) technique. The microstructure evolution of the composites with different deformation treatments was characterized using field emission scanning electron microscopy (FESEM) and a transmission electron microscope (TEM). The mechanical properties of the Al-TiB2/TiC in situ composite were also studied with tensile and microhardness tests. It was found that the distribution of reinforcement particles becomes more homogenous with an increasing ARB cycle. Meanwhile, the mechanical properties showed great improvement during the ARB process. The ultimate tensile strength (UTS) and microhardness of the composites were increased to 173.1 MPa and 63.3 Hv after two ARB cycles, respectively. Furthermore, the strengthening mechanism of the composite was analyzed based on its fracture morphologies. PMID:28772467

In situ dynamic observations of perovskite crystallisation and microstructure evolution intermediated from [PbI6]4- cage nanoparticles

NASA Astrophysics Data System (ADS)

Hu, Qin; Zhao, Lichen; Wu, Jiang; Gao, Ke; Luo, Deying; Jiang, Yufeng; Zhang, Ziyi; Zhu, Chenhui; Schaible, Eric; Hexemer, Alexander; Wang, Cheng; Liu, Yi; Zhang, Wei; Grätzel, Michael; Liu, Feng; Russell, Thomas P.; Zhu, Rui; Gong, Qihuang

2017-06-01

Hybrid lead halide perovskites have emerged as high-performance photovoltaic materials with their extraordinary optoelectronic properties. In particular, the remarkable device efficiency is strongly influenced by the perovskite crystallinity and the film morphology. Here, we investigate the perovskites crystallisation kinetics and growth mechanism in real time from liquid precursor continually to the final uniform film. We utilize some advanced in situ characterisation techniques including synchrotron-based grazing incident X-ray diffraction to observe crystal structure and chemical transition of perovskites. The nano-assemble model from perovskite intermediated [PbI6]4- cage nanoparticles to bulk polycrystals is proposed to understand perovskites formation at a molecular- or nano-level. A crystallisation-depletion mechanism is developed to elucidate the periodic crystallisation and the kinetically trapped morphology at a mesoscopic level. Based on these in situ dynamics studies, the whole process of the perovskites formation and transformation from the molecular to the microstructure over relevant temperature and time scales is successfully demonstrated.

Time-Resolved In Situ Measurements During Rapid Alloy Solidification: Experimental Insight for Additive Manufacturing

NASA Astrophysics Data System (ADS)

McKeown, Joseph T.; Zweiacker, Kai; Liu, Can; Coughlin, Daniel R.; Clarke, Amy J.; Baldwin, J. Kevin; Gibbs, John W.; Roehling, John D.; Imhoff, Seth D.; Gibbs, Paul J.; Tourret, Damien; Wiezorek, Jörg M. K.; Campbell, Geoffrey H.

2016-03-01

Additive manufacturing (AM) of metals and alloys is becoming a pervasive technology in both research and industrial environments, though significant challenges remain before widespread implementation of AM can be realized. In situ investigations of rapid alloy solidification with high spatial and temporal resolutions can provide unique experimental insight into microstructure evolution and kinetics that are relevant for AM processing. Hypoeutectic thin-film Al-Cu and Al-Si alloys were investigated using dynamic transmission electron microscopy to monitor pulsed-laser-induced rapid solidification across microsecond timescales. Solid-liquid interface velocities measured from time-resolved images revealed accelerating solidification fronts in both alloys. The observed microstructure evolution, solidification product, and presence of a morphological instability at the solid-liquid interface in the Al-4 at.%Cu alloy are related to the measured interface velocities and small differences in composition that affect the thermophysical properties of the alloys. These time-resolved in situ measurements can inform and validate predictive modeling efforts for AM.

Time-Resolved In Situ Measurements During Rapid Alloy Solidification: Experimental Insight for Additive Manufacturing

DOE PAGES

McKeown, Joseph T.; Zweiacker, Kai; Liu, Can; ...

2016-01-27

In research and industrial environments, additive manufacturing (AM) of metals and alloys is becoming a pervasive technology, though significant challenges remain before widespread implementation of AM can be realized. In situ investigations of rapid alloy solidification with high spatial and temporal resolutions can provide unique experimental insight into microstructure evolution and kinetics that are relevant for AM processing. Hypoeutectic thin-film Al–Cu and Al–Si alloys were investigated using dynamic transmission electron microscopy to monitor pulsed-laser-induced rapid solidification across microsecond timescales. Solid–liquid interface velocities measured from time-resolved images revealed accelerating solidification fronts in both alloys. We observed microstructure evolution, solidification product, andmore » presence of a morphological instability at the solid–liquid interface in the Al–4 at.%Cu alloy are related to the measured interface velocities and small differences in composition that affect the thermophysical properties of the alloys. These time-resolved in situ measurements can inform and validate predictive modeling efforts for AM.« less

In situ dynamic observations of perovskite crystallisation and microstructure evolution intermediated from [PbI6]4− cage nanoparticles

PubMed Central

Hu, Qin; Zhao, Lichen; Wu, Jiang; Gao, Ke; Luo, Deying; Jiang, Yufeng; Zhang, Ziyi; Zhu, Chenhui; Schaible, Eric; Hexemer, Alexander; Wang, Cheng; Liu, Yi; Zhang, Wei; Grätzel, Michael; Liu, Feng; Russell, Thomas P.; Zhu, Rui; Gong, Qihuang

2017-01-01

Hybrid lead halide perovskites have emerged as high-performance photovoltaic materials with their extraordinary optoelectronic properties. In particular, the remarkable device efficiency is strongly influenced by the perovskite crystallinity and the film morphology. Here, we investigate the perovskites crystallisation kinetics and growth mechanism in real time from liquid precursor continually to the final uniform film. We utilize some advanced in situ characterisation techniques including synchrotron-based grazing incident X-ray diffraction to observe crystal structure and chemical transition of perovskites. The nano-assemble model from perovskite intermediated [PbI6]4− cage nanoparticles to bulk polycrystals is proposed to understand perovskites formation at a molecular- or nano-level. A crystallisation-depletion mechanism is developed to elucidate the periodic crystallisation and the kinetically trapped morphology at a mesoscopic level. Based on these in situ dynamics studies, the whole process of the perovskites formation and transformation from the molecular to the microstructure over relevant temperature and time scales is successfully demonstrated. PMID:28635947

Multiscale modelling and experimentation of hydrogen embrittlement in aerospace materials

NASA Astrophysics Data System (ADS)

Jothi, Sathiskumar

Pulse plated nickel and nickel based superalloys have been used extensively in the Ariane 5 space launcher engines. Large structural Ariane 5 space launcher engine components such as combustion chambers with complex microstructures have usually been manufactured using electrodeposited nickel with advanced pulse plating techniques with smaller parts made of nickel based superalloys joined or welded to the structure to fabricate Ariane 5 space launcher engines. One of the major challenges in manufacturing these space launcher components using newly developed materials is a fundamental understanding of how different materials and microstructures react with hydrogen during welding which can lead to hydrogen induced cracking. The main objective of this research has been to examine and interpret the effects of microstructure on hydrogen diffusion and hydrogen embrittlement in (i) nickel based superalloy 718, (ii) established and (iii) newly developed grades of pulse plated nickel used in the Ariane 5 space launcher engine combustion chamber. Also, the effect of microstructures on hydrogen induced hot and cold cracking and weldability of three different grades of pulse plated nickel were investigated. Multiscale modelling and experimental methods have been used throughout. The effect of microstructure on hydrogen embrittlement was explored using an original multiscale numerical model (exploiting synthetic and real microstructures) and a wide range of material characterization techniques including scanning electron microscopy, 2D and 3D electron back scattering diffraction, in-situ and ex-situ hydrogen charged slow strain rate tests, thermal spectroscopy analysis and the Varestraint weldability test. This research shows that combined multiscale modelling and experimentation is required for a fundamental understanding of microstructural effects in hydrogen embrittlement in these materials. Methods to control the susceptibility to hydrogen induced hot and cold cracking and to improve the resistance to hydrogen embrittlement in aerospace materials are also suggested. This knowledge can play an important role in the development of new hydrogen embrittlement resistant materials. A novel micro/macro-scale coupled finite element method incorporating multi-scale experimental data is presented with which it is possible to perform full scale component analyses in order to investigate hydrogen embrittlement at the design stage. Finally, some preliminary and very encouraging results of grain boundary engineering based techniques to develop alloys that are resistant to hydrogen induced failure are presented. Keywords: Hydrogen embrittlement; Aerospace materials; Ariane 5 combustion chamber; Pulse plated nickel; Nickel based super alloy 718; SSRT test; Weldability test; TDA; SEM/EBSD; Hydrogen induced hot and cold cracking; Multiscale modelling and experimental methods.

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.

Microstructure Effects on Spall Strength of Titanium-based Bulk Metallic Glass Composites

NASA Astrophysics Data System (ADS)

Diaz, Rene; Hofmann, Douglas; Thadhani, Naresh; Georgia Tech Team; GT-JPL Collaboration

2017-06-01

The spall strength of Ti-based metallic glass composites is investigated as a function of varying volume fractions (0-80%) of in-situ formed crystalline dendrites. With increasing dendrite content, the topology changes such that neither the harder glass nor the softer dendrites dominate the microstructure. Plate-impact experiments were performed using the 80-mm single-stage gas gun over impact stresses up to 18 GPa. VISAR interferometry was used to obtain rear free-surface velocity profiles revealing the velocity pullback spall failure signals. The spall strengths were higher than for Ti-6Al-4V alloy, and remained high up to impact stress. The influence of microstructure on the spall strength is indicated by the constants of the power law fit with the decompression strain rate. Differences in fracture behavior reveal void nucleation as a dominant mechanism affecting the spall strength. The microstructure with neither 100% glass nor with very high crystalline content, provides the most tortuous path for fracture and therefore highest spall strength. The results allow projection of spall strength predictions for design of in-situ formed metallic glass composites. ARO Grant # W911NF-09 ``1-0403 NASA JPL Contract # 1492033 ``Prime # NNN12AA01C; NSF GRFP Grant #DGE-1148903; and NDSE & G.

Development of ceramic matrix composites for application in the ceramic technology for Advanced Heat Engines Project: Phase 2a, Development of in-situ toughened silicon nitride. Final report

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

Pollinger, J.; Newson, D.; Yeh, H.

1992-06-01

The objective of this program was to develop a net shape forming process for an in-situ reinforced Si{sub 3}N{sub 4} (AS-700). AS-700 was initially developed using cold isostatic pressing (CIP) of alcohol milled powders. The CIP`ed AS-700 material exhibited a moderate strength (690 MPa) and high toughness (9 MPa{radical}m) at room temperature. In addition to net-shape process development, optimization of AS-700 properties was also investigated through the refinement of densification processes, and evaluation of the effect of Si{sub 3}N{sub 4} powder properties on resulting microstructure and mechanical properties. Slip casting was chosen as the net-shape forming process. A slip castingmore » process was successfully developed for forming green parts ranging from thin plates to thick cylinders, and to large complex shaped turbine rotors. The densification cycle was optimized to achieve full density parts without any cracks or warpage, and with comparable properties and microstructure to the CIP`ed baseline AS-700 material. The evaluation of six (6) alternate Si{sub 3}N{sub 4} powders indicated that Si{sub 3}N{sub 4} powders have a very strong influence on the development of resulting AS-700 in-situ microstructures and mechanical properties. The AS-700 slip casting process and optimized densification process were then combined and a number of test specimens were fabricated. The mechanical properties and microstructure of the optimized slip cast AS-700 Si{sub 3}N{sub 4} were then fully characterized. The key property values are: 695 MPa at room temperature, 446 MPa at 1370{degree}C flexural strengths and 8.25 MPa{radical}m toughness.« less

Texture evolution during isothermal, isostrain, and isobaric loading of polycrystalline shape memory NiTi

NASA Astrophysics Data System (ADS)

Nicholson, D. E.; Padula, S. A.; Benafan, O.; Vaidyanathan, R.

2017-06-01

In situ neutron diffraction was used to provide insights into martensite variant microstructures during isothermal, isobaric, and isostrain loading in shape memory NiTi. The results show that variant microstructures were equivalent for the corresponding strain, and more importantly, the reversibility and equivalency were immediately evident in variant microstructures that were first formed isobarically but then reoriented to near random self-accommodated microstructures following isothermal deformation. Variant microstructures formed isothermally were not significantly affected by a subsequent thermal cycle under constant strain. In all loading cases considered, the resulting variant microstructure correlated with strain and did not correlate with stress. Based on the ability to select a variant microstructure for a given strain despite thermomechanical loading history, the results demonstrated here can be obtained by following any sequence of thermomechanical loading paths over multiple cycles. Thus, for training shape memory alloys (repeating thermomechanical cycling to obtain the desired variant microstructure), optimal paths can be selected so as to minimize the number of training cycles required, thereby increasing the overall stability and fatigue life of these alloys in actuator or medical applications.

Microstructure and Mechanical Behaviors of Titanium Matrix Composites Containing In Situ Whiskers Synthesized via Plasma Activated Sintering.

PubMed

Sun, Yi; Zhang, Jian; Luo, Guoqiang; Shen, Qiang; Zhang, Lianmeng

2018-04-02

In this paper, titanium matrix composites with in situ TiB whiskers were synthesized by the plasma activated sintering technique; crystalline boron and amorphous boron were used as reactants for in situ reactions, respectively. The influence of the sintering process and the crystallography type of boron on the microstructure and mechanical properties of composites were studied and compared. The densities were evaluated using Archimedes' principle. The microstructure and mechanical properties were characterized by SEM, XRD, EBSD, TEM, a universal testing machine, and a Vickers hardness tester. The prepared composite material showed a high density and excellent comprehensive performance under the PAS condition of 20 MPa at 1000 °C for 3 min. Amorphous boron had a higher reaction efficiency than crystalline boron, and it completely reacted with the titanium matrix to generate TiB whiskers, while there was still a certain amount of residual crystalline boron combining well with the titanium matrix at 1100 °C. The composite samples with a relative density of 98.33%, Vickers hardness of 389.75 HV, compression yield strength of up to 1190 MPa, and an ultimate compressive strength of up to 1710 MPa were obtained. Compared with the matrix material, the compressive strength of TC4 titanium alloy containing crystalline boron and amorphous boron was increased by 7.64% and 15.50%, respectively.

Microstructure and Mechanical Behaviors of Titanium Matrix Composites Containing In Situ Whiskers Synthesized via Plasma Activated Sintering

PubMed Central

Luo, Guoqiang; Shen, Qiang; Zhang, Lianmeng

2018-01-01

In this paper, titanium matrix composites with in situ TiB whiskers were synthesized by the plasma activated sintering technique; crystalline boron and amorphous boron were used as reactants for in situ reactions, respectively. The influence of the sintering process and the crystallography type of boron on the microstructure and mechanical properties of composites were studied and compared. The densities were evaluated using Archimedes’ principle. The microstructure and mechanical properties were characterized by SEM, XRD, EBSD, TEM, a universal testing machine, and a Vickers hardness tester. The prepared composite material showed a high density and excellent comprehensive performance under the PAS condition of 20 MPa at 1000 °C for 3 min. Amorphous boron had a higher reaction efficiency than crystalline boron, and it completely reacted with the titanium matrix to generate TiB whiskers, while there was still a certain amount of residual crystalline boron combining well with the titanium matrix at 1100 °C. The composite samples with a relative density of 98.33%, Vickers hardness of 389.75 HV, compression yield strength of up to 1190 MPa, and an ultimate compressive strength of up to 1710 MPa were obtained. Compared with the matrix material, the compressive strength of TC4 titanium alloy containing crystalline boron and amorphous boron was increased by 7.64% and 15.50%, respectively. PMID:29614842

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

Mechanical properties and deformation mechanism of Al2O3 determined from in situ transmission electron microscopy compression

NASA Astrophysics Data System (ADS)

Lin, Kai-Peng; Stachiv, Ivo; Fang, Te-Hua

2017-07-01

The mechanical properties and deformation mechanism of alumina (Al2O3) ceramic nanopillars and microstructures have been studied using in situ transmission electron microscopy (TEM) compression and nanoindentation experiments. It has been found that the Young’s modulus of Al2O3 nanopillars significantly increases with a decrease of its thickness; it ranges from 54.8 GPa for the nanopillar of radius 175 nm to 347.5 GPa for the one of radius of 75 nm. The hardness of Al2O3 microstructures estimated by the nanoindentation is between 3.19 to 20.60 GPa. The Raman spectra of Al2O3 substrate has a production peak (577.3 cm-1) between 418.3 and 645.2 (cm-1) peaks. The strain hardening behavior of Al2O3 microstructures has been observed and the impact of size on the compressive and bending behavior of Al2O3 micro-pillared structures is also examined and explained.

3D Imaging of a Dislocation Loop at the Onset of Plasticity in an Indented Nanocrystal.

PubMed

Dupraz, M; Beutier, G; Cornelius, T W; Parry, G; Ren, Z; Labat, S; Richard, M-I; Chahine, G A; Kovalenko, O; De Boissieu, M; Rabkin, E; Verdier, M; Thomas, O

2017-11-08

Structural quality and stability of nanocrystals are fundamental problems that bear important consequences for the performances of small-scale devices. Indeed, at the nanoscale, their functional properties are largely influenced by elastic strain and depend critically on the presence of crystal defects. It is thus of prime importance to be able to monitor, by noninvasive means, the stability of the microstructure of nano-objects against external stimuli such as mechanical load. Here we demonstrate the potential of Bragg coherent diffraction imaging for such measurements, by imaging in 3D the evolution of the microstructure of a nanocrystal exposed to in situ mechanical loading. Not only could we observe the evolution of the internal strain field after successive loadings, but we also evidenced a transient microstructure hosting a stable dislocation loop. The latter is fully characterized from its characteristic displacement field. The mechanical behavior of this small crystal is clearly at odds with what happens in bulk materials where many dislocations interact. Moreover, this original in situ experiment opens interesting possibilities for the investigation of plastic deformation at the nanoscale.

Validation of calcaneus trabecular microstructure measurements by HR-pQCT.

PubMed

Metcalf, Louis M; Dall'Ara, Enrico; Paggiosi, Margaret A; Rochester, John R; Vilayphiou, Nicolas; Kemp, Graham J; McCloskey, Eugene V

2018-01-01

Assessment of calcaneus microstructure using high-resolution peripheral quantitative computed tomography (HR-pQCT) might be used to improve fracture risk predictions or to assess responses to pharmacological and physical interventions. To develop a standard clinical protocol for the calcaneus, we validated calcaneus trabecular microstructure measured by HR-pQCT against 'gold-standard' micro-CT measurements. Ten human cadaveric feet were scanned in situ using HR-pQCT (isotropic 82μm voxel size) at 100, 150 and 200ms integration times, and at 100ms integration time following removal of the calcaneus from the foot (ex vivo). Dissected portions of these bones were scanned using micro-computed tomography (micro-CT) at an isotropic 17.4μm voxel size. HR-pQCT images were rigidly registered to those obtained with micro-CT and divided into multiple 5mm sided cubes to evaluate and compare morphometric parameters between the modalities. Standard HR-pQCT measurements (derived bone volume fraction (BV/TV d ); trabecular number, Tb.N; derived trabecular thickness, Tb.Th d ; derived trabecular spacing, Tb.Sp d ) and corresponding micro-CT voxel-based measurements (BV/TV, Tb.N, Tb.Th, Tb.Sp) were compared. A total of 108 regions of interest were analysed across the 10 specimens. At all integration times HR-pQCT BV/TV d was strongly correlated with micro-CT BV/TV (r 2 =0.95-0.98, RMSE=1%), but BV/TV d was systematically lower than that measured by micro-CT (mean bias=5%). In contrast, HR-pQCT systematically overestimated Tb.N at all integration times; of the in situ scans, 200ms yielded the lowest mean bias and the strongest correlation with micro-CT (r 2 =0.61, RMSE=0.15mm -1 ). Regional analysis revealed greater accuracy for Tb.N in the superior regions of the calcaneus at all integration times in situ (mean bias=0.44-0.85mm -1 ; r 2 =0.70-0.88, p<0.001 versus mean bias=0.63-1.46mm -1 ; r 2 ≤0.08, p≥0.21 for inferior regions). Tb.Sp d was underestimated by HR-pQCT compared to micro-CT, but showed similar trends with integration time and the region evaluated as Tb.N. HR-pQCT Tb.Th d was also underestimated and moderately correlated (r 2 =0.53-0.59) with micro-CT Tb.Th, independently from the integration time. Stronger correlations, smaller biases and error were found in the scans of the calcaneus ex vivo compared to in situ. Calcaneus trabecular BV/TV d and trabecular microstructure, particularly in the superior region of the calcaneus, can be assessed by HR-pQCT. The highest integration time examined, 200ms, compared best with micro-CT. Weaker correlations for microstructure at inferior regions, and also with lower integration times, might limit the use of the proposed protocol, which warrants further investigation in vivo. Copyright © 2017 The Authors. Published by Elsevier Inc. All rights reserved.

Measuring in-vivo and in-situ ex-vivo the 3D deformation of the lamina cribrosa microstructure under elevated intraocular pressure

NASA Astrophysics Data System (ADS)

Wei, Junchao; Yang, Bin; Voorhees, Andrew P.; Tran, Huong; Brazile, Bryn; Wang, Bo; Schuman, Joel; Smith, Matthew A.; Wollstein, Gadi; Sigal, Ian A.

2018-02-01

Elevated intraocular pressure (IOP) deforms the lamina cribrosa (LC), a structure within the optic nerve head (ONH) in the back of the eye. Evidence suggests that these deformations trigger events that eventually cause irreversible blindness, and have therefore been studied in-vivo using optical coherence tomography (OCT), and ex-vivo using OCT and a diversity of techniques. To the best of our knowledge, there have been no in-situ ex-vivo studies of LC mechanics. Our goal was two-fold: to introduce a technique for measuring 3D LC deformations from OCT, and to determine whether deformations of the LC induced by elevated IOP differ between in-vivo and in-situ ex-vivo conditions. A healthy adult rhesus macaque monkey was anesthetized and IOP was controlled by inserting a 27- gauge needle into the anterior chamber of the eye. Spectral domain OCT was used to obtain volumetric scans of the ONH at normal and elevated IOPs. To improve the visibility of the LC microstructure the scans were first processed using a novel denoising technique. Zero-normalized cross-correlation was used to find paired corresponding locations between images. For each location pair, the components of the 3D strain tensor were determined using non-rigid image registration. A mild IOP elevation from 10 to 15mmHg caused LC effective strains as large as 3%, and about 50% larger in-vivo than in-situ ex-vivo. The deformations were highly heterogeneous, with substantial 3D components, suggesting that accurate measurement of LC microstructure deformation requires high-resolution volumes. This technique will help improve understanding of LC biomechanics and how IOP contributes to glaucoma.

In-situ investigation of stress-induced martensitic transformation in Ti–Nb binary alloys with low Young's modulus [In-situ high-energy X-ray diffraction investigation on stress-induced martensitic transformation in Ti-Nb binary alloys

DOE PAGES

Chang, L. L.; Wang, Y. D.; Ren, Y.

2015-11-04

Microstructure evolution, mechanical behaviors of cold rolled Ti-Nb alloys with different Nb contents subjected to different heat treatments were investigated. Here, optical microstructure and phase compositions of Ti-Nb alloys were characterized using optical microscopy and X-ray diffractometre, while mechanical behaviors of Ti-Nb alloys were examined by using tension tests. Stress-induced martensitic transformation in a Ti-30. at%Nb binary alloy was in-situ explored by synchrotron-based high-energy X-ray diffraction (HE-XRD). The results obtained suggested that mechanical behavior of Ti-Nb alloys, especially Young's modulus was directly dependent on chemical compositions and heat treatment process. According to the results of HE-XRD, α"-V1 martensite generated priormore » to the formation of α"-V2 during loading and a partial reversible transformation from α"-V1 to β phase was detected while α"-V2 tranformed to β completely during unloading.« less

Effect of Mo on Microstructures and Wear Properties of In Situ Synthesized Ti(C,N)/Ni-Based Composite Coatings by Laser Cladding.

PubMed

Wu, Fan; Chen, Tao; Wang, Haojun; Liu, Defu

2017-09-06

Using Ni60 alloy, C, TiN and Mo mixed powders as the precursor materials, in situ synthesized Ti(C,N) particles reinforcing Ni-based composite coatings are produced on Ti6Al4V alloys by laser cladding. Phase constituents, microstructures and wear properties of the composite coatings with 0 wt % Mo, 4 wt % Mo and 8 wt % Mo additions are studied comparatively. Results indicate that Ti(C,N) is formed by the in situ metallurgical reaction, the (Ti,Mo)(C,N) rim phase surrounding the Ti(C,N) ceramic particle is synthesized with the addition of Mo, and the increase of Mo content is beneficial to improve the wear properties of the cladding coatings. Because of the effect of Mo, the grains are remarkably refined and a unique core-rim structure that is uniformly dispersed in the matrix appears; meanwhile, the composite coatings with Mo addition exhibit high hardness and excellent wear resistance due to the comprehensive action of dispersion strengthening, fine grain strengthening and solid solution strengthening.

Effect of Mo on Microstructures and Wear Properties of In Situ Synthesized Ti(C,N)/Ni-Based Composite Coatings by Laser Cladding

PubMed Central

Chen, Tao; Wang, Haojun

2017-01-01

Using Ni60 alloy, C, TiN and Mo mixed powders as the precursor materials, in situ synthesized Ti(C,N) particles reinforcing Ni-based composite coatings are produced on Ti6Al4V alloys by laser cladding. Phase constituents, microstructures and wear properties of the composite coatings with 0 wt % Mo, 4 wt % Mo and 8 wt % Mo additions are studied comparatively. Results indicate that Ti(C,N) is formed by the in situ metallurgical reaction, the (Ti,Mo)(C,N) rim phase surrounding the Ti(C,N) ceramic particle is synthesized with the addition of Mo, and the increase of Mo content is beneficial to improve the wear properties of the cladding coatings. Because of the effect of Mo, the grains are remarkably refined and a unique core-rim structure that is uniformly dispersed in the matrix appears; meanwhile, the composite coatings with Mo addition exhibit high hardness and excellent wear resistance due to the comprehensive action of dispersion strengthening, fine grain strengthening and solid solution strengthening. PMID:28878190

A technique for recording polycrystalline structure and orientation during in situ deformation cycles of rock analogues using an automated fabric analyser.

PubMed

Peternell, M; Russell-Head, D S; Wilson, C J L

2011-05-01

Two in situ plane-strain deformation experiments on norcamphor and natural ice using synchronous recording of crystal c-axis orientations have been performed with an automated fabric analyser and a newly developed sample press and deformation stage. Without interrupting the deformation experiment, c-axis orientations are determined for each pixel in a 5 × 5 mm sample area at a spatial resolution of 5 μm/pixel. In the case of norcamphor, changes in microstructures and associated crystallographic information, at a strain rate of ∼2 × 10(-5) s(-1), were recorded for the first time during a complete in situ deformation-cycle experiment that consisted of an annealing, deformation and post-deformation annealing path. In the case of natural ice, slower external strain rates (∼1 × 10(-6) s(-1)) enabled the investigation of small changes in the polycrystal aggregate's crystallography and microstructure for small amounts of strain. The technical setup and first results from the experiments are presented. © 2010 The Authors Journal of Microscopy © 2010 Royal Microscopical Society.

In situ dynamic observations of perovskite crystallisation and microstructure evolution intermediated from [PbI 6] 4– cage nanoparticles

DOE PAGES

Hu, Qin; Zhao, Lichen; Wu, Jiang; ...

2017-06-21

Hybrid lead halide perovskites have emerged as high-performance photovoltaic materials with their extraordinary optoelectronic properties. In particular, the remarkable device efficiency is strongly influenced by the perovskite crystallinity and the film morphology. Here, we investigate the perovskites crystallisation kinetics and growth mechanism in real time from liquid precursor continually to the final uniform film. We utilize some advanced in situ characterisation techniques including synchrotron-based grazing incident X-ray diffraction to observe crystal structure and chemical transition of perovskites. The nano-assemble model from perovskite intermediated [PbI 6] 4– cage nanoparticles to bulk polycrystals is proposed to understand perovskites formation at a molecular-more » or nano-level. A crystallisation-depletion mechanism is developed to elucidate the periodic crystallisation and the kinetically trapped morphology at a mesoscopic level. Based on these in situ dynamics studies, the whole process of the perovskites formation and transformation from the molecular to the microstructure over relevant temperature and time scales is successfully demonstrated.« less

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

Sun, Pei; Fang, Zhigang Zak; Koopman, Mark

The hydrogen sintering and phase transformation (HSPT) process is a novel powder metallurgy method for producing Ti alloys, particularly the Ti-6Al-4V alloy, with ultra-fine microstructure in the as-sintered state. The ultra-fine microstructure is obtained as a direct result of the use of H-2 gas during sintering. The refinement of the microstructure during HSPT is similar to that of thermal hydrogen processing (THP) of bulk Ti alloys. For both THP and HSPT of Ti-6Al-4V alloy, the mechanisms of the grain refinement depend on the phase equilibria and phase transformations in the presence of hydrogen, which are surprisingly still not well establishedmore » to date and are still subjected to research and debate. In recent work by the present authors, a pseudo-binary phase diagram of (Ti-6Al-4V)-H has been determined by using in situ synchrotron XRD and TGA/DSC techniques. Aided by this phase diagram, the current paper focuses on the series of phase transformations during sintering and cooling of Ti-6Al-4V in a hydrogen atmosphere and the mechanisms for the formation of the ultra-fine microstructures obtained. Using experimental techniques, including in situ synchrotron XRD, SEM, EBSD, and TEM, the microstructural refinement was found to be the result of (1) the precipitation of ultra-fine alpha/alpha(2) within coarse beta grains during an isothermal hold at intermediate temperatures, and (2) the eutectoid transformation of beta -> alpha + delta d at approximately 473 K (200 degrees C). (C) The Minerals, Metals & Materials Society and ASM International 2015« less

Performance of Sustainable Fly Ash and Slag Cement Mortars Exposed to Simulated and Real In Situ Mediterranean Conditions along 90 Warm Season Days.

PubMed

Ortega, José Marcos; Esteban, María Dolores; Sánchez, Isidro; Climent, Miguel Ángel

2017-10-31

Nowadays, cement manufacture is one of the most polluting worldwide industrial sectors. In order to reduce its CO₂ emissions, the clinker replacement by ground granulated blast-furnace slag and fly ash is becoming increasingly common. Both additions are well-studied when the hardening conditions of cementitious materials are optimum. Therefore, the main objective of this research was to study the short-term effects of exposure, to both laboratory simulated and real in situ Mediterranean climate environments, on the microstructure and durability-related properties of mortars made using commercial slag and fly ash cements, as well as ordinary Portland cement. The real in situ condition consisted of placing the samples at approximately 100 m away from the Mediterranean Sea. The microstructure was analysed using mercury intrusion porosimetry. The effective porosity, the capillary suction coefficient and the non-steady state chloride migration coefficient were also studied. In view of the results obtained, the non-optimum laboratory simulated Mediterranean environment was a good approach to the real in situ one. Finally, mortars prepared using sustainable cements with slag and fly ash exposed to both Mediterranean climate environments, showed adequate service properties in the short-term (90 days), similar to or even better than those in mortars made with ordinary Portland cement.

A literature review of in situ transmission electron microscopy technique in corrosion studies.

PubMed

Song, Zhengwei; Xie, Zhi-Hui

2018-06-18

One of the biggest challenges in corrosion investigation is foreseeing precisely how and where materials will degenerate in a designated condition owing to scarceness of accurate corrosion mechanisms. Recent fast development of in situ transmission electron microscopy (TEM) technique makes it achievable to better understand the corrosion mechanism and physicochemical processes at the interfaces between samples and gases or electrolytes by dynamical capture the microstructural and chemical changes with high resolution within a realistic or near-realistic environment. However, a detailed and in-depth account summing up the development and latest achievements of in situ TEM techniques, especially the application of emerging liquid and electrochemical cells in the community of corrosion study in the last several years is lacking and is urgently needed for its heathy development. To fill this gap, this critical review summarizes firstly the key scientific issues in corrosion research, followed by introducing the configurations of several typical closed-type cells. Then, the achievements of in situ TEM using open-type or closed-type cells in corrosion study are presented in detail. The study directions in the future are commented finally in terms of spatial and temporal resolution, electron radiation, and linkage between microstructure and electrochemical performance in corrosion community. Copyright © 2018 Elsevier Ltd. All rights reserved.

Microstructure and mechanical properties investigation of in situ TiB2 and ZrB2 reinforced Al-4Cu composites

NASA Astrophysics Data System (ADS)

Lutfi Anis, Ahmad; Ramli, Rosmamuhammadani; Darham, Widyani; Zakaria, Azlan; Talari, Mahesh Kumar

2016-02-01

Conventional Al-Cu alloys exhibit coarse grain structure leading to inferior mechanical properties in as-cast condition. Expensive thermo-mechanical treatments are needed to improve microstructure and corresponding mechanical properties. In situ Al-based composites were developed to improve mechanical properties by dispersion strengthening and grain refinement obtained by the presence of particulates in the melt during solidification. In this work Al-4Cu - 3TiB2 and Al-4Cu-3ZrB2 in situ composites were prepared by liquid casting method. XRD, electron microscopy and mechanical tests were performed on suitably sectioned and metallographically prepared surfaces to investigate the phase distribution, hardness and tensile properties. It was found that the reinforcement particles were segregated along the grain boundaries of Al dendrites. Tensile fracture morphology for both Al-4Cu - 3TiB2 and Al-4Cu-3ZrB2 were analyzed and compared to determine the fracture propagation mechanism in the composites. Al-4Cu-3ZrB2 in situ composites displayed higher strength and hardness compared to Al-4Cu-3TiB2 which could be ascribed to the stronger interfacial bonding between the Al dendrites and ZrB2 particulates as evidenced from fractographs.

How microfracture roughness can be used to distinguish between exhumed cracks and in-situ flow paths in shales

NASA Astrophysics Data System (ADS)

Pluymakers, Anne; Kobchenko, Maya; Renard, François

2017-01-01

Flow through fractures in shales is of importance to many geoengineering purposes. Shales are not only caprocks to hydrocarbon reservoirs and nuclear waste or CO2 storage sites, but also potential source and reservoir rocks for hydrocarbons. The presence of microfractures in shales controls their permeability and transport properties. Using X-ray micro-tomography and white light interferometry we scanned borehole samples obtained from 4 km depth in the Pomeranian shales in Poland. These samples contain open exhumation/drying cracks as well as intact vein-rock interfaces plus one striated slip surface. At micron resolution and above tensile drying cracks exhibit a power-law roughness with a scaling exponent, called the Hurst exponent H, of 0.3. At sub-micron resolution we capture the properties of the clay interface only, with H = 0.6. In contrast, the in-situ formed veins and slip surface exhibit H = 0.4-0.5, which is deemed representative for in-situ fractures. These results are discussed in relation to the shale microstructure and linear elastic fracture mechanics theory. The data imply that the Hurst roughness exponent can be used as a microstructural criterion to distinguish between exhumation and in-situ fractures, providing a step forward towards the characterization of potential flow paths at depth in shales.

Investigation of the Microstructure Evolution in a Fe-17Mn-1.5Al-0.3C Steel via In Situ Synchrotron X-ray Diffraction during a Tensile Test

PubMed Central

Song, Wenwen; Bleck, Wolfgang

2017-01-01

The quantitative characterization of the microstructure evolution in high-Mn steel during deformation is of great importance to understanding its strain-hardening behavior. In the current study, in situ high-energy synchrotron X-ray diffraction was employed to characterize the microstructure evolution in a Fe-17Mn-1.5Al-0.3C steel during a tensile test. The microstructure at different engineering strain levels—in terms of ε-martensite and α’-martensite volume fractions, the stacking fault probability, and the twin fault probability—was analyzed by the Rietveld refinement method. The Fe-17Mn-1.5Al-0.3C steel exhibits a high ultimate tensile strength with a superior uniform elongation and a high strain-hardening rate. The remaining high strain-hardening rate at the strain level about 0.025 to 0.35 results from ε-martensite dominant transformation-induced-plasticity (TRIP) effect. The increase in the strain-hardening rate at the strain level around 0.35 to 0.43 is attributed to the synergetic α’-martensite dominant TRIP and twinning-induced-plasticity (TWIP) effects. An evaluation of the stacking fault energy (SFE) of the Fe-17Mn-1.5Al-0.3C steel by the synchrotron measurements shows good agreement with the thermodynamic calculation of the SFE. PMID:28946692

Investigation of the Microstructure Evolution in a Fe-17Mn-1.5Al-0.3C Steel via In Situ Synchrotron X-ray Diffraction during a Tensile Test.

PubMed

Ma, Yan; Song, Wenwen; Bleck, Wolfgang

2017-09-25

The quantitative characterization of the microstructure evolution in high-Mn steel during deformation is of great importance to understanding its strain-hardening behavior. In the current study, in situ high-energy synchrotron X-ray diffraction was employed to characterize the microstructure evolution in a Fe-17Mn-1.5Al-0.3C steel during a tensile test. The microstructure at different engineering strain levels-in terms of ε-martensite and α'-martensite volume fractions, the stacking fault probability, and the twin fault probability-was analyzed by the Rietveld refinement method. The Fe-17Mn-1.5Al-0.3C steel exhibits a high ultimate tensile strength with a superior uniform elongation and a high strain-hardening rate. The remaining high strain-hardening rate at the strain level about 0.025 to 0.35 results from ε-martensite dominant transformation-induced-plasticity (TRIP) effect. The increase in the strain-hardening rate at the strain level around 0.35 to 0.43 is attributed to the synergetic α'-martensite dominant TRIP and twinning-induced-plasticity (TWIP) effects. An evaluation of the stacking fault energy (SFE) of the Fe-17Mn-1.5Al-0.3C steel by the synchrotron measurements shows good agreement with the thermodynamic calculation of the SFE.

Application of Finite Element, Phase-field, and CALPHAD-based Methods to Additive Manufacturing of Ni-based Superalloys.

PubMed

Keller, Trevor; Lindwall, Greta; Ghosh, Supriyo; Ma, Li; Lane, Brandon M; Zhang, Fan; Kattner, Ursula R; Lass, Eric A; Heigel, Jarred C; Idell, Yaakov; Williams, Maureen E; Allen, Andrew J; Guyer, Jonathan E; Levine, Lyle E

2017-10-15

Numerical simulations are used in this work to investigate aspects of microstructure and microseg-regation during rapid solidification of a Ni-based superalloy in a laser powder bed fusion additive manufacturing process. Thermal modeling by finite element analysis simulates the laser melt pool, with surface temperatures in agreement with in situ thermographic measurements on Inconel 625. Geometric and thermal features of the simulated melt pools are extracted and used in subsequent mesoscale simulations. Solidification in the melt pool is simulated on two length scales. For the multicomponent alloy Inconel 625, microsegregation between dendrite arms is calculated using the Scheil-Gulliver solidification model and DICTRA software. Phase-field simulations, using Ni-Nb as a binary analogue to Inconel 625, produced microstructures with primary cellular/dendritic arm spacings in agreement with measured spacings in experimentally observed microstructures and a lesser extent of microsegregation than predicted by DICTRA simulations. The composition profiles are used to compare thermodynamic driving forces for nucleation against experimentally observed precipitates identified by electron and X-ray diffraction analyses. Our analysis lists the precipitates that may form from FCC phase of enriched interdendritic compositions and compares these against experimentally observed phases from 1 h heat treatments at two temperatures: stress relief at 1143 K (870 °C) or homogenization at 1423 K (1150 °C).

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.

Nano-scale zirconia and hafnia dielectrics grown by atomic layer deposition: Crystallinity, interface structures and electrical properties

NASA Astrophysics Data System (ADS)

Kim, Hyoungsub

With the continued scaling of transistors, leakage current densities across the SiO2 gate dielectric have increased enormously through direct tunneling. Presently, metal oxides having higher dielectric constants than SiO2 are being investigated to reduce the leakage current by increasing the physical thickness of the dielectric. Many possible techniques exist for depositing high-kappa gate dielectrics. Atomic layer deposition (ALD) has drawn attention as a method for preparing ultrathin metal oxide layers with excellent electrical characteristics and near-perfect film conformality due to the layer-by-layer nature of the deposition mechanism. For this research, an ALD system using ZrCl4/HfCl4 and H2O was built and optimized. The microstructural and electrical properties of ALD-ZrO2 and HfO2 grown on SiO2/Si substrates were investigated and compared using various characterization tools. In particular, the crystallization kinetics of amorphous ALD-HfO2 films were studied using in-situ annealing experiments in a TEM. The effect of crystallization on the electrical properties of ALD-HfO 2 was also investigated using various in-situ and ex-situ post-deposition anneals. Our results revealed that crystallization had little effect on the magnitude of the gate leakage current or on the conduction mechanisms. Building upon the results for each metal oxide separately, more advanced investigations were made. Several nanolaminate structures using ZrO2 and HfO2 with different sequences and layer thicknesses were characterized. The effects of the starting microstructure on the microstructural evolution of nanolaminate stacks were studied. Additionally, a promising new approach for engineering the thickness of the SiO2-based interface layer between the metal oxide and silicon substrate after deposition of the metal oxide layer was suggested. Through experimental measurements and thermodynamic analysis, it is shown that a Ti overlayer, which exhibits a high oxygen solubility, can effectively getter oxygen from the interface layer, thus decomposing SiO2 and reducing the interface layer thickness in a controllable fashion. As one of several possible applications, ALD-ZrO2 and HfO 2 gate dielectric films were deposited on Ge (001) substrates with different surface passivations. After extensive characterization using various microstructural, electrical, and chemical analyses, excellent MOS electrical properties of high-kappa gate dielectrics on Ge were successfully demonstrated with optimized surface nitridation of the Ge substrates.

Laser engineered net shaping of quasi-continuous network microstructural TiB reinforced titanium matrix bulk composites: Microstructure and wear performance

NASA Astrophysics Data System (ADS)

Hu, Yingbin; Ning, Fuda; Wang, Hui; Cong, Weilong; Zhao, Bo

2018-02-01

Titanium (Ti) and its alloys have been successfully applied to the aeronautical and biomedical industries. However, their poor tribological properties restrict their fields of applications under severe wear conditions. Facing to these challenges, this study investigated TiB reinforced Ti matrix composites (TiB-TMCs), fabricated by in-situ laser engineered net shaping (LENS) process, through analyzing parts quality, microstructure formation mechanisms, microstructure characterizations, and workpiece wear performance. At high B content areas (original B particle locations), reaction between Ti and B particles took place, generating flower-like microstructure. At low B content areas, eutectic TiB nanofibers contacted with each other with the formation of crosslinking microstructure. The crosslinking microstructural TiB aggregated and connected at the boundaries of Ti grains, forming a three-dimensional quasi-continuous network microstructure. The results show that compared with commercially pure Ti bulk parts, the TiB-TMCs exhibited superior wear performance (i.e. indentation wear resistance and friction wear resistance) due to the present of TiB reinforcement and the innovative microstructures formed inside TiB-TMCs. In addition, the qualities of the fabricated parts were improved with fewer interior defects by optimizing laser power, thus rendering better wear performance.

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

Sun, Pei; Fang, Z. Zak; Koopman, Mark

Hydrogen has been investigated for decades as a temporary alloying element to refine the microstructure of Ti-6Al-4V, and is now being used in a novel powder metallurgy method known as "hydrogen sintering and phase transformation". Pseudo-binary phase diagrams of (Ti-6Al-4V)-xH have been studied and developed, but are not well established due to methodological limitations. In this paper, in situ studies of phase transformations during hydrogenation and dehydrogenation of (Ti-6Al-4V)-xH alloys were conducted using high-energy synchrotron X-ray diffraction (XRD), thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The eutectoid phase transformation of β ↔ α + δ was observed in themore » (Ti-6Al-4V)-xH alloy via in situ synchrotron XRD at 211 °C with a hydrogen concentration of 37.5 at.% (measured using TGA-DSC). The relationships of hydrogen composition to partial pressure and temperature were investigated in the temperature range 450-900°C. Based on these results, a partial pseudo-binary phase diagram of (Ti-6Al-4V)-xH is proposed for hydrogen compositions up to 60 at.% in the temperature range 100-900°C. Using the data collected in real time under controlled parameters of temperature, composition and hydrogen partial pressure, this work characterizes relevant phase transformations and microstructural evolution for practical titanium-hydrogen technologies of Ti-6Al-4V.« less

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

NASA Astrophysics Data System (ADS)

Guo, Qianying; Thompson, Gregory B.

2018-04-01

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

Using Converter Dust to Produce Low Cost Cementitious Composites by in situ Carbon Nanotube and Nanofiber Synthesis

PubMed Central

Ludvig, Péter; Calixto, José M.; Ladeira, Luiz O.; Gaspar, Ivan C.P.

2011-01-01

Carbon nanotubes (CNTs) and nanofibers (CNFs) were synthesized on clinker and silica fume particles in order to create a low cost cementitious nanostructured material. The synthesis was carried out by an in situ chemical vapor deposition (CVD) process using converter dust, an industrial byproduct, as iron precursor. The use of these materials reduces the cost, with the objective of application in large-scale nanostructured cement production. The resulting products were analyzed by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA) and were found to be polydisperse in size and to have defective microstructure. Some enhancement in the mechanical behavior of cement mortars was observed due to the addition of these nano-size materials. The contribution of these CNTs/CNFs to the mechanical strength of mortar specimens is similar to that of high quality CNTs incorporated in mortars by physical mixture. PMID:28880007

Observation of conducting filament growth in nanoscale resistive memories

NASA Astrophysics Data System (ADS)

Yang, Yuchao; Gao, Peng; Gaba, Siddharth; Chang, Ting; Pan, Xiaoqing; Lu, Wei

2012-03-01

Nanoscale resistive switching devices, sometimes termed memristors, have recently generated significant interest for memory, logic and neuromorphic applications. Resistive switching effects in dielectric-based devices are normally assumed to be caused by conducting filament formation across the electrodes, but the nature of the filaments and their growth dynamics remain controversial. Here we report direct transmission electron microscopy imaging, and structural and compositional analysis of the nanoscale conducting filaments. Through systematic ex-situ and in-situ transmission electron microscopy studies on devices under different programming conditions, we found that the filament growth can be dominated by cation transport in the dielectric film. Unexpectedly, two different growth modes were observed for the first time in materials with different microstructures. Regardless of the growth direction, the narrowest region of the filament was found to be near the dielectric/inert-electrode interface in these devices, suggesting that this region deserves particular attention for continued device optimization.

A method to investigate the electron scattering characteristics of ultrathin metallic films by in situ electrical resistance measurements.

PubMed

Trindade, I G; Fermento, R; Leitão, D; Sousa, J B

2009-07-01

In this article, a method to measure the electrical resistivity/conductivity of metallic thin films during layer growth on specific underlayers is described. The in situ monitoring of an underlayer electrical resistance, its change upon the incoming of new material atoms/molecules, and the growth of a new layer are presented. The method is easy to implement and allows obtaining in situ experimental curves of electrical resistivity dependence upon film thickness with a subatomic resolution, providing insight in film growth microstructure characteristics, specular/diffuse electron scattering surfaces, and optimum film thicknesses.

Influence of Primary Water Chemistry on Oxides Formed on Alloy 600 and Alloy 690

NASA Astrophysics Data System (ADS)

Devine, Thomas M.

The results of in situ SERS investigations of Alloys' 600 and 690 surface films were combined with the results of a number of ex situ studies conducted by other researchers who used a variety of experimental techniques. Comparing the results of different investigations revealed the surface films' composition and microstructure were most sensitive to alloy composition and the concentrations of aqueous metal cations (especially Fe+2).

Metastable solidification of hypereutectic Co 2Si-CoSi composition: Microstructural studies and in-situ observations

DOE PAGES

Wang, Yeqing; Gao, Jianrong; Kolbe, Matthias; ...

2017-09-18

Metastable solidification of undercooled Co 60Si 40 melts was investigated by microstructural studies and in-situ high-energy X-ray diffraction. Five solidification paths were identified. Three of them were observed at low undercoolings, which show uncoupled and coupled growth of stable β-Co 2Si and CoSi compounds. The other paths were observed at high undercoolings, which show peritectic and primary crystallization of a metastable Co 5Si 3 compound. The β-Co 2Si and Co 5Si 3 compounds crystallize into a hexagonal crystal structure and experience solid-state decomposition. Microstructure formation depends on solidification path. The coupled and uncoupled growth of the stable compounds produces amore » regular lamellar eutectic structure and an anomalous eutectic structure, respectively. The crystallization and solid-state decomposition of the metastable Co 5Si 3 compound brings about a fine-grained two-phase mixture, which represents another type of anomalous eutectic structure. Here, the results provide proof of two rare mechanisms of anomalous eutectic formation and shed light onto metastable phase relations in the undercooled region of the Co-Si system.« less

Metastable solidification of hypereutectic Co 2Si-CoSi composition: Microstructural studies and in-situ observations

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

Wang, Yeqing; Gao, Jianrong; Kolbe, Matthias

Metastable solidification of undercooled Co 60Si 40 melts was investigated by microstructural studies and in-situ high-energy X-ray diffraction. Five solidification paths were identified. Three of them were observed at low undercoolings, which show uncoupled and coupled growth of stable β-Co 2Si and CoSi compounds. The other paths were observed at high undercoolings, which show peritectic and primary crystallization of a metastable Co 5Si 3 compound. The β-Co 2Si and Co 5Si 3 compounds crystallize into a hexagonal crystal structure and experience solid-state decomposition. Microstructure formation depends on solidification path. The coupled and uncoupled growth of the stable compounds produces amore » regular lamellar eutectic structure and an anomalous eutectic structure, respectively. The crystallization and solid-state decomposition of the metastable Co 5Si 3 compound brings about a fine-grained two-phase mixture, which represents another type of anomalous eutectic structure. Here, the results provide proof of two rare mechanisms of anomalous eutectic formation and shed light onto metastable phase relations in the undercooled region of the Co-Si system.« less

X-ray Computed Tomography Imaging of the Microstructure of Sand Particles Subjected to High Pressure One-Dimensional Compression

PubMed Central

al Mahbub, Asheque; Haque, Asadul

2016-01-01

This paper presents the results of X-ray CT imaging of the microstructure of sand particles subjected to high pressure one-dimensional compression leading to particle crushing. A high resolution X-ray CT machine capable of in situ imaging was employed to capture images of the whole volume of a sand sample subjected to compressive stresses up to 79.3 MPa. Images of the whole sample obtained at different load stages were analysed using a commercial image processing software (Avizo) to reveal various microstructural properties, such as pore and particle volume distributions, spatial distribution of void ratios, relative breakage, and anisotropy of particles. PMID:28774011

X-ray Computed Tomography Imaging of the Microstructure of Sand Particles Subjected to High Pressure One-Dimensional Compression.

PubMed

Al Mahbub, Asheque; Haque, Asadul

2016-11-03

This paper presents the results of X-ray CT imaging of the microstructure of sand particles subjected to high pressure one-dimensional compression leading to particle crushing. A high resolution X-ray CT machine capable of in situ imaging was employed to capture images of the whole volume of a sand sample subjected to compressive stresses up to 79.3 MPa. Images of the whole sample obtained at different load stages were analysed using a commercial image processing software (Avizo) to reveal various microstructural properties, such as pore and particle volume distributions, spatial distribution of void ratios, relative breakage, and anisotropy of particles.

Lightweight Mg-based composites with thermodynamically stable interfaces by in-situ combustion synthesis

NASA Astrophysics Data System (ADS)

Jo, Ilguk

Lightweight Mg-based composites have been produced by in-situ combustion synthesis of the Al-Ti-C reaction system. The characteristics of the in-situ composites were investigated in terms of phase evolution and interfacial stability using various analysis techniques. The structural analysis results showed that full conversion of the Al-Ti-C reactants into spherical TiC reinforcements with sizes around 1mum was achieved by the combustion reaction. In-situ formed TiC had less oxygen and higher Al contents at the interface than ex-situ formed TiC; these clean interfaces with an Al layer on the reinforcements were shown to yield interfacial stability. For these reasons, the in-situ composites exhibited higher theoretical densities and also good mechanical properties compared with ex-situ produced composites. The interfacial characteristics of molten Mg with the Al-Ti-C reactants and the commercial TiC+Al substrates were evaluated using an infiltration technique under an argon atmosphere. Infiltration length increased with time at temperature, yielding activation energies (Ea) for each system. The value of Ea for the Al-Ti-C system (307.31kJ/mol) is lower than that for the other system (350.84kJ/mol); the high Ea value indicates that the infiltration is not a simple viscosity-controlled phenomenon but involves a chemical reaction. Formation of the Al3Ti phase was observed from the crystal structural analysis of the infiltrated area; thus, existence of reaction promoting the wetting of Mg. The phase evolution, reaction mechanism and kinetics of the Al-Ti-C reaction were studied using DSC and HT-XRD. It was confirmed that, along with the melting of Al, there was formation of Al3Ti by reaction between Al and Ti. A detailed structural analysis indicates that, the reaction mechanism involves melting of Al followed by formation and growth of Al 3Ti, which then contacts the graphite powder and initiates the combustion reaction. The effect of important process parameters, such as the Al content and the reactant sizes, on the microstructure of the resulting in-situ composites is discussed. Feasibility and castability of the composites were investigated by high pressure die casting the composite preforms into automotive parts and durability tests were conducted on the cast parts.

Progressive Assessment on the Decomposition Reaction of Na Superionic Conducting Ceramics.

PubMed

Jung, Jae-Il; Kim, Daekyeom; Kim, Hyojin; Jo, Yong Nam; Park, Jung Sik; Kim, Youngsik

2017-01-11

The successful analysis on the microstructure of Hong-type Na superionic conducting (NASICON) ceramics revealed that it consists of several heterogeneous phases: NASICON grains with rectangular shapes, monoclinic round ZrO 2 particles, grain boundaries, a SiO 2 -rich vitrified phase, Na-rich amorphous particles, and pores. A dramatic microstructural evolution of NASICON ceramics was demonstrated via an in situ analysis, which showed that NASICON grains sequentially lost their original morphology and were transformed into comminuted particles (as indicated by the immersion of bulk NASICON samples into seawater at a temperature of 80 °C). The consecutive X-ray diffraction analysis represented that the significant shear stress inside NASICON ceramics caused their structural decomposition, during which H 3 O + ions occupied ceramic Na + sites (predominantly along the (1̅11) and (1̅33) planes), while the original Na + cations came out in the (020) plane of the NASICON ceramic crystalline structure. The results of time-of-flight secondary-ion mass spectrometry analysis confirmed that large concentrations of Cl - and Na + ions were distributed across the surface of NASICON ceramics, leading to local densification of a 20 μm thick surface layer after treatment within seawater solution at a temperature of 80 °C.

Characterizing the Effects of Washing by Different Detergents on the Wavelength-Scale Microstructures of Silk Samples Using Mueller Matrix Polarimetry.

PubMed

Dong, Yang; He, Honghui; He, Chao; Zhou, Jialing; Zeng, Nan; Ma, Hui

2016-08-10

Silk fibers suffer from microstructural changes due to various external environmental conditions including daily washings. In this paper, we take the backscattering Mueller matrix images of silk samples for non-destructive and real-time quantitative characterization of the wavelength-scale microstructure and examination of the effects of washing by different detergents. The 2D images of the 16 Mueller matrix elements are reduced to the frequency distribution histograms (FDHs) whose central moments reveal the dominant structural features of the silk fibers. A group of new parameters are also proposed to characterize the wavelength-scale microstructural changes of the silk samples during the washing processes. Monte Carlo (MC) simulations are carried out to better understand how the Mueller matrix parameters are related to the wavelength-scale microstructure of silk fibers. The good agreement between experiments and simulations indicates that the Mueller matrix polarimetry and FDH based parameters can be used to quantitatively detect the wavelength-scale microstructural features of silk fibers. Mueller matrix polarimetry may be used as a powerful tool for non-destructive and in situ characterization of the wavelength-scale microstructures of silk based materials.

Characterizing the Effects of Washing by Different Detergents on the Wavelength-Scale Microstructures of Silk Samples Using Mueller Matrix Polarimetry

PubMed Central

Dong, Yang; He, Honghui; He, Chao; Zhou, Jialing; Zeng, Nan; Ma, Hui

2016-01-01

Silk fibers suffer from microstructural changes due to various external environmental conditions including daily washings. In this paper, we take the backscattering Mueller matrix images of silk samples for non-destructive and real-time quantitative characterization of the wavelength-scale microstructure and examination of the effects of washing by different detergents. The 2D images of the 16 Mueller matrix elements are reduced to the frequency distribution histograms (FDHs) whose central moments reveal the dominant structural features of the silk fibers. A group of new parameters are also proposed to characterize the wavelength-scale microstructural changes of the silk samples during the washing processes. Monte Carlo (MC) simulations are carried out to better understand how the Mueller matrix parameters are related to the wavelength-scale microstructure of silk fibers. The good agreement between experiments and simulations indicates that the Mueller matrix polarimetry and FDH based parameters can be used to quantitatively detect the wavelength-scale microstructural features of silk fibers. Mueller matrix polarimetry may be used as a powerful tool for non-destructive and in situ characterization of the wavelength-scale microstructures of silk based materials. PMID:27517919

Effect of in-situ TiC particulate on the wear resistance of spray-deposited 7075 Al matrix composite

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

Wang Feng; Liu Huimin; Yang Bin

2005-05-15

TiC reinforced 7075 Al matrix composites have been fabricated by a melt in-situ reaction spray deposition. The microstructures of spray-deposited alloys were studied using scanning electron microscopy (SEM) and X-ray diffraction (XRD). The dry sliding wear behavior of the alloys was investigated using a pin-on-disc machine under four loads, namely 8.9, 17.8, 26.7 and 35.6 N. It has been found that the wear behavior of the alloys was dependent on the TiC content in the microstructure and the applied load. At a lower load (8.9 N), with increasing TiC content, the wear rate of the alloy was decreased. At amore » higher loads (26.7, 35.6 N), a spray-deposited 7075 Al alloy exhibited superior wear resistance to the 7075/TiC composites.« less

Portable vibro-acoustic testing system for in situ microstructure characterization and metrology

NASA Astrophysics Data System (ADS)

Smith, James A.; Nichol, Corrie I.; Zuck, Larry D.; Fatemi, Mostafa

2018-04-01

There is a need in research reactors like the one at INL to inspect irradiated materials and structures. The goal of this work is to develop a portable scanning infrastructure for a material characterization technique called vibro-acoustography (VA) that has been developed by the Idaho National laboratory for nuclear applications to characterize fuel, cladding materials, and structures. The proposed VA technology is based on ultrasound and acoustic waves; however, it provides information beyond what is available from the traditional ultrasound techniques and can expand the knowledge on nuclear material characterization and microstructure evolution. This paper will report on the development of a portable scanning system that will be set up to characterize materials and components in open water reactors and canals in situ. We will show some initial laboratory results of images generated by vibro-acoustics of surrogate fuel plates and graphite structures and discuss the design of the portable system.

The microstructural characterization of an in situ grown Si{sub 3}N{sub 4} whisker-reinforced BAS glass-ceramic matrix composite

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

Yu, Feng; Ortiz-Longo, C.R.; White, K.W.

The microstructure of barium aluminum silicate (BAS)/silicon nitride in situ whisker reinforced ceramic matrix composite was examined by X-ray diffraction, transmission electron microscopy, electron diffraction and energy-dispersive X-ray microanalysis. Although the authors can not conclusively exclude the presence of orthorhombic BAS, hexagonal BAS and both {alpha}-Si{sub 3}N{sub 4} and {beta}-Si{sub 3}N{sub 4} were identified in this material. The {beta}-Si{sub 3}N{sub 4} whiskers nucleate and grow in random directions in the nearly continuous matrix of metastable hexacelsian. The crystallization process of the glass phase can be taken almost to completion but a small proportion of residual glass phase is present atmore » the interface and grains-junction. Both whisker-like and equiaxed {beta}-Si{sub 3}N{sub 4} exist in this material.« less

Visualizing In Situ Microstructure Dependent Crack Tip Stress Distribution in IN-617 Using Nano-mechanical Raman Spectroscopy

NASA Astrophysics Data System (ADS)

Zhang, Yang; Mohanty, Debapriya P.; Tomar, Vikas

2016-11-01

Inconel 617 (IN-617) is a solid solution alloy, which is widely used in applications that require high-temperature component operation due to its high-temperature stability and strength as well as strong resistance to oxidation and carburization. The current work focuses on in situ measurements of stress distribution under 3-point bending at elevated temperature in IN-617. A nanomechanical Raman spectroscopy measurement platform was designed and built based on a combination of a customized open Raman spectroscopy (NMRS) system incorporating a motorized scanning and imaging system with a nanomechanical loading platform. Based on the scanning of the crack tip notch area using the NMRS notch tip, stress distribution under applied load with micron-scale resolution for analyzed microstructures is predicted. A finite element method-based formulation to predict crack tip stresses is presented and validated using the presented experimental data.

Microstructure-Sensitive Investigation of Fracture Using Acoustic Emission Coupled With Electron Microscopy

NASA Technical Reports Server (NTRS)

Wisner, Brian; Cabal, Mike; Vanniamparambiland, Prashanth A.; Leser, William; Hochhalter, Jacob; Kontsos, Antonios

2015-01-01

A novel technique using Scanning Electron Microscopy (SEM) in conjunction with Acoustic Emission (AE) monitoring is proposed to investigate microstructure-sensitive fatigue and fracture of metals. The coupling between quasi in situ microscopy with actual in situ nondestructive evaluation falls into the ICME framework and the idea of quantitative data-driven characterization of material behavior. To validate the use of AE monitoring inside the SEM chamber, Aluminum 2024-B sharp notch specimen were tested both inside and outside the microscope using a small scale mechanical testing device. Subsequently, the same type of specimen was tested inside the SEM chamber. Load data were correlated with both AE information and observations of microcracks around grain boundaries as well as secondary cracks, voids, and slip bands. The preliminary results are in excellent agreement with similar findings at the mesoscale. Extensions of the application of this novel technique are discussed.

Microstructure and property evolutions of titanium/nano-hydroxyapatite composites in-situ prepared by selective laser melting.

PubMed

Han, Changjun; Wang, Qian; Song, Bo; Li, Wei; Wei, Qingsong; Wen, Shifeng; Liu, Jie; Shi, Yusheng

2017-07-01

Titanium (Ti)-hydroxyapatite (HA) composites have the potential for orthopedic applications due to their favorable mechanical properties, excellent biocompatibility and bioactivity. In this work, the pure Ti and nano-scale HA (Ti-nHA) composites were in-situ prepared by selective laser melting (SLM) for the first time. The phase, microstructure, surface characteristic and mechanical properties of the SLM-processed Ti-nHA composites were studied by X-ray diffraction, transmission electron microscope, atomic force microscope and tensile tests, respectively. Results show that SLM is a suitable method for fabricating the Ti-nHA composites with refined microstructure, low modulus and high strength. A novel microstructure evolution can be illustrated as: Relatively long lath-shaped grains of pure Ti evolved into short acicular-shaped and quasi-continuous circle-shaped grains with the varying contents of nHA. The elastic modulus of the Ti-nHA composites is 3.7% higher than that of pure Ti due to the effect of grain refinement. With the addition of 2% nHA, the ultimate tensile strength significantly reduces to 289MPa but still meets the application requirement of bone implants. The Ti-nHA composites exhibit a remarkable improvement of microhardness from 336.2 to 600.8 HV and nanohardness from 5.6 to 8.3GPa, compared to those of pure Ti. Moreover, the microstructure and property evolution mechanisms of the composites with the addition of HA were discussed and analyzed. It provides some new knowledge to the design and fabrication of biomedical material composites for bone implant applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

On the role of ultra-thin oxide cathode synthesis on the functionality of micro-solid oxide fuel cells: Structure, stress engineering and in situ observation of fuel cell membranes during operation

NASA Astrophysics Data System (ADS)

Lai, Bo-Kuai; Kerman, Kian; Ramanathan, Shriram

Microstructure and stresses in dense La 0.6Sr 0.4Co 0.8Fe 0.2O 3 (LSCF) ultra-thin films have been investigated to increase the physical thickness of crack-free cathodes and active area of thermo-mechanically robust micro-solid oxide fuel cell (μSOFC) membranes. Processing protocols employ low deposition rates to create a highly granular nanocrystalline microstructure in LSCF thin films and high substrate temperatures to produce linear temperature-dependent stress evolution that is dominated by compressive stresses in μSOFC membranes. Insight and trade-off on the synthesis are revealed by probing microstructure evolution and electrical conductivity in LSCF thin films, in addition to in situ monitoring of membrane deformation while measuring μSOFC performance at varying temperatures. From these studies, we were able to successfully fabricate failure-resistant square μSOFC (LSCF/YSZ/Pt) membranes with width of 250 μm and crack-free cathodes with thickness of ∼70 nm. Peak power density of ∼120 mW cm -2 and open circuit voltage of ∼0.6 V at 560 °C were achieved on a μSOFC array chip containing ten such membranes. Mechanisms affecting fuel cell performance are discussed. Our results provide fundamental insight to pathways of microstructure and stress engineering of ultra-thin, dense oxide cathodes and μSOFC membranes.

"Self-preservation" of CO(2) gas hydrates--surface microstructure and ice perfection.

PubMed

Falenty, Andrzej; Kuhs, Werner F

2009-12-10

Gas hydrates can exhibit an anomalously slow decomposition outside their thermodynamic stability field; the phenomenon is called "self-preservation" and is mostly studied at ambient pressure and at temperatures between approximately 240 K and the melting point of ice. Here, we present a combination of in situ neutron diffraction studies, pVT work, and ex situ scanning electron microscopy (SEM) on CO(2) clathrates covering a much broader p-T field, stretching from 200 to 270 K and pressures between the hydrate stability limit and 0.6 kPa (6 mbar), a pressure far outside stability. The self-preservation regime above 240 K is confirmed over a broad pressure range and appears to be caused by the annealing of an ice cover formed in the initial hydrate decomposition. Another, previously unknown regime of the self-preservation exists below this temperature, extending however only over a rather narrow pressure range. In this case, the initial ice microstructure is dominated by a fast two-dimensional growth covering rapidly the clathrate surface. All observations lend strong support to the idea that the phenomenon of self-preservation is linked to the permeability of the ice cover governed by (1) the initial microstructure of ice and/or (2) the subsequent annealing of this ice coating. The interplay of the microstructure of newly formed ice and its annealing with the ongoing decomposition reaction leads to various decomposition paths and under certain conditions to a very pronounced preservation anomaly.

Microstructural Control via Copious Nucleation Manipulated by In Situ Formed Nucleants: Large-Sized and Ductile Metallic Glass Composites.

PubMed

Song, Wenli; Wu, Yuan; Wang, Hui; Liu, Xiongjun; Chen, Houwen; Guo, Zhenxi; Lu, Zhaoping

2016-10-01

A novel strategy to control the precipitation behavior of the austenitic phase, and to obtain large-sized, transformation-induced, plasticity-reinforced bulk metallic glass matrix composites, with good tensile properties, is proposed. By inducing heterogeneous nucleation of the transformable reinforcement via potent nucleants formed in situ, the characteristics of the austenitic phase are well manipulated. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Performance of Sustainable Fly Ash and Slag Cement Mortars Exposed to Simulated and Real In Situ Mediterranean Conditions along 90 Warm Season Days

PubMed Central

Esteban, María Dolores

2017-01-01

Nowadays, cement manufacture is one of the most polluting worldwide industrial sectors. In order to reduce its CO2 emissions, the clinker replacement by ground granulated blast–furnace slag and fly ash is becoming increasingly common. Both additions are well-studied when the hardening conditions of cementitious materials are optimum. Therefore, the main objective of this research was to study the short-term effects of exposure, to both laboratory simulated and real in situ Mediterranean climate environments, on the microstructure and durability-related properties of mortars made using commercial slag and fly ash cements, as well as ordinary Portland cement. The real in situ condition consisted of placing the samples at approximately 100 m away from the Mediterranean Sea. The microstructure was analysed using mercury intrusion porosimetry. The effective porosity, the capillary suction coefficient and the non-steady state chloride migration coefficient were also studied. In view of the results obtained, the non-optimum laboratory simulated Mediterranean environment was a good approach to the real in situ one. Finally, mortars prepared using sustainable cements with slag and fly ash exposed to both Mediterranean climate environments, showed adequate service properties in the short-term (90 days), similar to or even better than those in mortars made with ordinary Portland cement. PMID:29088107

In situ imaging during compression of plastic bonded explosives for damage modeling

DOE PAGES

Manner, Virginia Warren; Yeager, John David; Patterson, Brian M.; ...

2017-06-10

Here, the microstructure of plastic bonded explosives (PBXs) is known to influence behavior during mechanical deformation, but characterizing the microstructure can be challenging. For example, the explosive crystals and binder in formulations such as PBX 9501 do not have sufficient X-ray contrast to obtain three-dimensional data by in situ, absorption contrast imaging. To address this difficulty, we have formulated a series of PBXs using octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) crystals and low-density binder systems. The binders were hydroxyl-terminated polybutadiene (HTPB) or glycidyl azide polymer (GAP) cured with a commercial blend of acrylic monomers/oligomers. The binder density is approximately half of the HMX, allowingmore » for excellent contrast using in situ X-ray computed tomography (CT) imaging. The samples were imaged during unaxial compression using micro-scale CT in an interrupted in situ modality. The rigidity of the binder was observed to significantly influence fracture, crystal-binder delamination, and flow. Additionally, 2D slices from the segmented 3D images were meshed for finite element simulation of the mesoscale response. At low stiffness, the binder and crystal do not delaminate and the crystals move with the material flow; at high stiffness, marked delamination is noted between the crystals and the binder, leading to very different mechanical properties. Initial model results exhibit qualitatively similar delamination.« less

In situ imaging during compression of plastic bonded explosives for damage modeling

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

Manner, Virginia Warren; Yeager, John David; Patterson, Brian M.

Here, the microstructure of plastic bonded explosives (PBXs) is known to influence behavior during mechanical deformation, but characterizing the microstructure can be challenging. For example, the explosive crystals and binder in formulations such as PBX 9501 do not have sufficient X-ray contrast to obtain three-dimensional data by in situ, absorption contrast imaging. To address this difficulty, we have formulated a series of PBXs using octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) crystals and low-density binder systems. The binders were hydroxyl-terminated polybutadiene (HTPB) or glycidyl azide polymer (GAP) cured with a commercial blend of acrylic monomers/oligomers. The binder density is approximately half of the HMX, allowingmore » for excellent contrast using in situ X-ray computed tomography (CT) imaging. The samples were imaged during unaxial compression using micro-scale CT in an interrupted in situ modality. The rigidity of the binder was observed to significantly influence fracture, crystal-binder delamination, and flow. Additionally, 2D slices from the segmented 3D images were meshed for finite element simulation of the mesoscale response. At low stiffness, the binder and crystal do not delaminate and the crystals move with the material flow; at high stiffness, marked delamination is noted between the crystals and the binder, leading to very different mechanical properties. Initial model results exhibit qualitatively similar delamination.« less

In Situ Imaging during Compression of Plastic Bonded Explosives for Damage Modeling.

PubMed

Manner, Virginia W; Yeager, John D; Patterson, Brian M; Walters, David J; Stull, Jamie A; Cordes, Nikolaus L; Luscher, Darby J; Henderson, Kevin C; Schmalzer, Andrew M; Tappan, Bryce C

2017-06-10

The microstructure of plastic bonded explosives (PBXs) is known to influence behavior during mechanical deformation, but characterizing the microstructure can be challenging. For example, the explosive crystals and binder in formulations such as PBX 9501 do not have sufficient X-ray contrast to obtain three-dimensional data by in situ, absorption contrast imaging. To address this difficulty, we have formulated a series of PBXs using octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) crystals and low-density binder systems. The binders were hydroxyl-terminated polybutadiene (HTPB) or glycidyl azide polymer (GAP) cured with a commercial blend of acrylic monomers/oligomers. The binder density is approximately half of the HMX, allowing for excellent contrast using in situ X-ray computed tomography (CT) imaging. The samples were imaged during unaxial compression using micro-scale CT in an interrupted in situ modality. The rigidity of the binder was observed to significantly influence fracture, crystal-binder delamination, and flow. Additionally, 2D slices from the segmented 3D images were meshed for finite element simulation of the mesoscale response. At low stiffness, the binder and crystal do not delaminate and the crystals move with the material flow; at high stiffness, marked delamination is noted between the crystals and the binder, leading to very different mechanical properties. Initial model results exhibit qualitatively similar delamination.

In Situ Imaging during Compression of Plastic Bonded Explosives for Damage Modeling

PubMed Central

Manner, Virginia W.; Yeager, John D.; Patterson, Brian M.; Walters, David J.; Stull, Jamie A.; Cordes, Nikolaus L.; Luscher, Darby J.; Henderson, Kevin C.; Schmalzer, Andrew M.; Tappan, Bryce C.

2017-01-01

The microstructure of plastic bonded explosives (PBXs) is known to influence behavior during mechanical deformation, but characterizing the microstructure can be challenging. For example, the explosive crystals and binder in formulations such as PBX 9501 do not have sufficient X-ray contrast to obtain three-dimensional data by in situ, absorption contrast imaging. To address this difficulty, we have formulated a series of PBXs using octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) crystals and low-density binder systems. The binders were hydroxyl-terminated polybutadiene (HTPB) or glycidyl azide polymer (GAP) cured with a commercial blend of acrylic monomers/oligomers. The binder density is approximately half of the HMX, allowing for excellent contrast using in situ X-ray computed tomography (CT) imaging. The samples were imaged during unaxial compression using micro-scale CT in an interrupted in situ modality. The rigidity of the binder was observed to significantly influence fracture, crystal-binder delamination, and flow. Additionally, 2D slices from the segmented 3D images were meshed for finite element simulation of the mesoscale response. At low stiffness, the binder and crystal do not delaminate and the crystals move with the material flow; at high stiffness, marked delamination is noted between the crystals and the binder, leading to very different mechanical properties. Initial model results exhibit qualitatively similar delamination. PMID:28772998

Microprobe monazite geochronology: new techniques for dating deformation and metamorphism

NASA Astrophysics Data System (ADS)

Williams, M.; Jercinovic, M.; Goncalves, P.; Mahan, K.

2003-04-01

High-resolution compositional mapping, age mapping, and precise dating of monazite on the electron microprobe are powerful additions to microstructural and petrologic analysis and important tools for tectonic studies. The in-situ nature and high spatial resolution of the technique offer an entirely new level of structurally and texturally specific geochronologic data that can be used to put absolute time constraints on P-T-D paths, constrain the rates of sedimentary, metamorphic, and deformational processes, and provide new links between metamorphism and deformation. New analytical techniques (including background modeling, sample preparation, and interference analysis) have significantly improved the precision and accuracy of the technique and new mapping and image analysis techniques have increased the efficiency and strengthened the correlation with fabrics and textures. Microprobe geochronology is particularly applicable to three persistent microstructural-microtextural problem areas: (1) constraining the chronology of metamorphic assemblages; (2) constraining the timing of deformational fabrics; and (3) interpreting other geochronological results. In addition, authigenic monazite can be used to date sedimentary basins, and detrital monazite can fingerprint sedimentary source areas, both critical for tectonic analysis. Although some monazite generations can be directly tied to metamorphism or deformation, at present, the most common constraints rely on monazite inclusion relations in porphyroblasts that, in turn, can be tied to the deformation and/or metamorphic history. Examples will be presented from deep-crustal rocks of northern Saskatchewan and from mid-crustal rocks from the southwestern USA. Microprobe monazite geochronology has been used in both regions to deconvolute overprinting deformation and metamorphic events and to clarify the interpretation of other geochronologic data. Microprobe mapping and dating are powerful companions to mass spectroscopic dating techniques. They allow geochronology to be incorporated into the microstructural analytical process, resulting in a new level of integration of time (t) into P-T-D histories.

THE PHYSICAL AND CHEMICAL MICROSTRUCTURE OF THE ACHATINA FULICA EPIPHRAGM.

PubMed

Struthers, M.; Rosair, G.; Buckman, J.; Viney, C.

2002-05-01

Microstructural characterization of Achatina fulica Bowdich, 1822 epiphragms and mucus secretions was performed to address two questions: what are the structure and composition of the reinforcing inorganic phase in the epiphragms, and what enables a durable epiphragm to form quickly in comparison to other biomineralized materials? Characterization was performed by a combination of light microscopy (relying on a variety of contrast modes), wet chemical tests, environmental scanning electron microscopy (including the use of energy dispersive X-ray analysis to obtain compositional data), and X-ray diffraction. The morphology of the inorganic phase promotes mechanical interlocking and presents a large surface for binding to the organic matrix. Strong binding occurs between the organic and inorganic phases. The inorganic phase adopts the calcite structure; its composition is Ca(0.912) Mg(0.088) CO(3). Epiphragms can form quickly because pre-grown crystals of the inorganic reinforcing phase are co-deposited with the mucus matrix. Unlike other biomineralized material, the crystals are not solution-grown in situ on an organic template in the final product.

History Dependence of the Microstructure on Time-Dependent Deformation During In-Situ Cooling of a Nickel-Based Single-Crystal Superalloy

NASA Astrophysics Data System (ADS)

Panwisawas, Chinnapat; D'Souza, Neil; Collins, David M.; Bhowmik, Ayan; Roebuck, Bryan

2018-05-01

Time-dependent plastic deformation through stress relaxation and creep deformation during in-situ cooling of the as-cast single-crystal superalloy CMSX-4® has been studied via neutron diffraction, transmission electron microscopy, electro-thermal miniature testing, and analytical modeling across two temperature regimes. Between 1000 °C and 900 °C, stress relaxation prevails and gives rise to softening as evidenced by a decreased dislocation density and the presence of long segment stacking faults in γ phase. Lattice strains decrease in both the γ matrix and γ' precipitate phases. A constitutive viscoplastic law derived from in-situ isothermal relaxation test under-estimates the equivalent plastic strain in the prediction of the stress and strain evolution during cooling in this case. It is thereby shown that the history dependence of the microstructure needs to be taken into account while deriving a constitutive law and which becomes even more relevant at high temperatures approaching the solvus. Higher temperature cooling experiments have also been carried out between 1300 °C and 1150 °C to measure the evolution of stress and plastic strain close to the γ' solvus temperature. In-situ cooling of samples using ETMT shows that creep dominates during high-temperature deformation between 1300 °C and 1220 °C, but below a threshold temperature, typically 1220 °C work hardening begins to prevail from increasing γ' fraction and resulting in a rapid increase in stress. The history dependence of prior accumulated deformation is also confirmed in the flow stress measurements using a single sample while cooling. The saturation stresses in the flow stress experiments show very good agreement with the stresses measured in the cooling experiments when viscoplastic deformation is dominant. This study demonstrates that experimentation during high-temperature deformation as well as the history dependence of the microstructure during cooling plays a key role in deriving an accurate viscoplastic constitutive law for the thermo-mechanical process during cooling from solidification.

Short-Term Behavior of Slag Concretes Exposed to a Real In Situ Mediterranean Climate Environment.

PubMed

Ortega, José Marcos; Sánchez, Isidro; Cabeza, Marta; Climent, Miguel Ángel

2017-08-08

At present, one of the most suitable ways to get a more sustainable cement industry is to reduce the CO₂ emissions generated during cement production. In order to reach that goal, the use of ground granulated blast-furnace slag as clinker replacement is becoming increasingly popular. Although the effects of this addition in the properties of cementitious materials are influenced by their hardening conditions, there are not too many experimental studies in which slag concretes have been exposed to real in situ environments. Then, the main objective of this research is to study the short-term effects of exposure to real Mediterranean climate environment of an urban site, where the action of airborne chlorides from sea water and the presence of CO₂ are combined, in the microstructure and service properties of a commercial slag cement concrete, compared to ordinary Portland cement (OPC). The microstructure was studied with mercury intrusion porosimetry. The effective porosity, capillary suction coefficient, chloride migration coefficient, carbonation front depth, and compressive strength were also analyzed. Considering the results obtained, slag concretes exposed to a real in situ Mediterranean climate environment show good service properties in the short-term (180 days), in comparison with OPC.

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

PubMed

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

2013-08-01

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

Characterization of beryllium deformation using in-situ x-ray diffraction

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

Magnuson, Eric Alan; Brown, Donald William; Clausen, Bjorn

2015-08-24

Beryllium’s unique mechanical properties are extremely important in a number of high performance applications. Consequently, accurate models for the mechanical behavior of beryllium are required. However, current models are not sufficiently microstructure aware to accurately predict the performance of beryllium under a range of processing and loading conditions. Previous experiments conducted using the SMARTS and HIPPO instruments at the Lujan Center(LANL), have studied the relationship between strain rate and texture development, but due to the limitations of neutron diffraction studies, it was not possible to measure the response of the material in real-time. In-situ diffraction experiments conducted at the Advancedmore » Photon Source have allowed the real time measurement of the mechanical response of compressed beryllium. Samples of pre-strained beryllium were reloaded orthogonal to their original load path to show the reorientation of already twinned grains. Additionally, the in-situ experiments allowed the real time tracking of twin evolution in beryllium strained at high rates. The data gathered during these experiments will be used in the development and validation of a new, microstructure aware model of the constitutive behavior of beryllium.« less

Measurement Of Hydrogen Capacities And Stability In Thin Films Of AlH Deposited By Magnetron Sputtering

NASA Astrophysics Data System (ADS)

Dissanayake, A.; AlFaify, S.; Garratt, E.; Nandasiri, M. I.; Taibu, R.; Tecos, G.; Hamdan, N. M.; Kayani, A.

2011-06-01

Thin, hydrogenated aluminum hydride films were deposited on silicon substrates using unbalanced magnetron (UBM) sputtering of a high purity aluminum target under electrically grounded conditions. Argon was used as sputtering gas and hydrogenation was carried out by diluting the growth plasma with hydrogen. The effect of hydrogen partial pressure on the final concentration of trapped elements including hydrogen has been studied using ion beam analysis (IBA) techniques. Moreover, in-situ thermal stability of trapped hydrogen in the film was carried out using Rutherford Backscattering Spectrometry (RBS), Non-Rutherford Backscattering Spectrometry (NRBS) and Elastic Recoil Detection Analysis (ERDA). Microstructure of the film was investigated by SEM analysis. Hydrogen content in the thin films was found decreasing as the films were heated above 110 °C in vacuum.

Evidence of Microfossils in Carbonaceous Chondrites

NASA Technical Reports Server (NTRS)

Hoover, Richard B.; Rozanov, Alexei Y.; Zhmur, S. I.; Gorlenko, V. M.

1998-01-01

Investigations have been carried out on freshly broken, internal surfaces of the Murchison, Efremovka and Orgueil carbonaceous chondrites using Scanning Electron Microscopes (SEM) in Russia and the Environmental Scanning Electron Microscope (ESEM) in the United States. These independent studies on different samples of the meteorites have resulted in the detection of numerous spherical and ellipsoidal bodies (some with spikes) similar to the forms of uncertain biogenicity that were designated "organized elements" by prior researchers. We have also encountered numerous complex biomorphic microstructures in these carbonaceous chondrites. Many of these complex bodies exhibit diverse characteristics reminiscent of microfossils of cyanobacteria such as we have investigated in ancient phosphorites and high carbon rocks (e.g. oil shales). Energy Dispersive Spectroscopy (EDS) analysis and 2D elemental maps shows enhanced carbon content in the bodies superimposed upon the elemental distributions characteristic of the chondritic matrix. The size, distribution, composition, and indications of cell walls, reproductive and life cycle developmental stages of these bodies are strongly suggestive of biology' These bodies appear to be mineralized and embedded within the meteorite matrix, and can not be attributed to recent surface contamination effects. Consequently, we have interpreted these in-situ microstructures to represent the lithified remains of prokaryotes and filamentous cyanobacteria. We also detected in Orgueil microstructures morphologically similar to fibrous kerite crystals. We present images of many biomorphic microstructures and possible microfossils found in the Murchison, Efremovka, and Orgueil chondrites and compare these forms with known microfossils from the Cambrian phosphate-rich rocks (phosphorites) of Khubsugul, Northern Mongolia.

Precise Analysis of Microstructural Effects on Mechanical Properties of Cast ADC12 Aluminum Alloy

NASA Astrophysics Data System (ADS)

Okayasu, Mitsuhiro; Takeuchi, Shuhei; Yamamoto, Masaki; Ohfuji, Hiroaki; Ochi, Toshihiro

2015-04-01

The effects of microstructural characteristics (secondary dendrite arm spacing, SDAS) and Si- and Fe-based eutectic structures on the mechanical properties and failure behavior of an Al-Si-Cu alloy are investigated. Cast Al alloy samples are produced using a special continuous-casting technique with which it is easy to control both the sizes of microstructures and the direction of crystal orientation. Dendrite cells appear to grow in the casting direction. There are linear correlations between SDAS and tensile properties (ultimate tensile strength σ UTS, 0.2 pct proof strength σ 0.2, and fracture strain ɛ f). These linear correlations, however, break down, especially for σ UTS vs SDAS and ɛ f vs SDAS, as the eutectic structures become more than 3 μm in diameter, when the strength and ductility ( σ UTS and ɛ f) decrease significantly. For eutectic structures larger than 3 μm, failure is dominated by the brittle eutectic phases, for which SDAS is no longer strongly correlated with σ UTS and ɛ f. In contrast, a linear correlation is obtained between σ 0.2 and SDAS, even for eutectic structures larger than 3 μm, and the eutectic structure does not have a strong effect on yield behavior. This is because failure in the eutectic phases occurs just before final fracture. In situ failure observation during tensile testing is performed using microstructural and lattice characteristics. From the experimental results obtained, models of failure during tensile loading are proposed.

Histological, chemical, and morphological reexamination of the ``heart'' of a small Late Cretaceous Thescelosaurus

NASA Astrophysics Data System (ADS)

Cleland, Timothy P.; Stoskopf, Michael K.; Schweitzer, Mary H.

2011-03-01

A three-dimensional, iron-cemented structure found in the anterior thoracic cavity of articulated Thescelosaurus skeletal remains was hypothesized to be the fossilized remains of the animal's four-chambered heart. This was important because the finding could be interpreted to support a hypothesis that non-avian dinosaurs were endothermic. Mammals and birds, the only extant organisms with four-chambered hearts and single aortae, are endotherms. The hypothesis that this Thescelosaurus has a preserved heart was controversial, and therefore, we reexamined it using higher-resolution computed tomography, paleohistological examination, X-ray diffraction analysis, X-ray photoelectron spectroscopy, and scanning electron microscopy. This suite of analyses allows for detailed morphological and chemical examination beyond what was provided in the original work. Neither the more detailed examination of the gross morphology and orientation of the thoracic "heart" nor the microstructural studies supported the hypothesis that the structure was a heart. The more advanced computed tomography showed the same three areas of low density as the earlier studies with no evidence of additional low-density areas as might be expected from examinations of an ex situ ostrich heart. Microstructural examination of a fragment taken from the "heart" was consistent with cemented sand grains, and no chemical signal consistent with a biological origin was detected. However, small patches of cell-like microstructures were preserved in the sandstone matrix of the thoracic structure. A possible biological origin for these microstructures is the focus of ongoing investigation.

Morphological evaluation of heterogeneous oolitic limestone under pressure and fluid flow using X-ray microtomography

NASA Astrophysics Data System (ADS)

Zhang, Yihuai; Lebedev, Maxim; Al-Yaseri, Ahmed; Yu, Hongyan; Nwidee, Lezorgia N.; Sarmadivaleh, Mohammad; Barifcani, Ahmed; Iglauer, Stefan

2018-03-01

Pore-scale analysis of carbonate rock is of great relevance to the oil and gas industry owing to their vast application potentials. Although, efficient fluid flow at pore scale is often disrupted owing to the tight rock matrix and complex heterogeneity of limestone microstructures, factors such as porosity, permeability and effective stress greatly impact the rock microstructures; as such an understanding of the effect of these variables is vital for various natural and engineered processes. In this study, the Savonnières limestone as a carbonate mineral was evaluated at micro scales using X-ray micro-computed tomography at high resolutions (3.43 μm and 1.25 μm voxel size) under different effective stress (0 MPa, 20 MPa) to ascertain limestone microstructure and gas permeability and porosity effect. The waterflooding (5 wt% NaCl) test was conducted using microCT in-situ scanning and nanoindentation test was also performed to evaluate microscale geomechanical heterogeneity of the rock. The nanoindentation test results showed that the nano/micro scale geomechanical properties are quite heterogeneous where the indentation modulus for the weak consolidated area was as low as 1 GPa. We observed that the fluid flow easily broke some less-consolidated areas (low indentation modulus) area, coupled with increase in porosity; and consistent with fines/particles migration and re-sedimentation were identified, although the effective stress showed only a minor effect on the rock microstructure.

Localized Pulsed Electrodeposition Process for Three-Dimensional Printing of Nanotwinned Metallic Nanostructures.

PubMed

Daryadel, Soheil; Behroozfar, Ali; Morsali, S Reza; Moreno, Salvador; Baniasadi, Mahmoud; Bykova, Julia; Bernal, Rodrigo A; Minary-Jolandan, Majid

2018-01-10

Nanotwinned-metals (nt-metals) offer superior mechanical (high ductility and strength) and electrical (low electromigration) properties compared to their nanocrystalline (nc) counterparts. These properties are advantageous in particular for applications in nanoscale devices. However, fabrication of nt-metals has been limited to films (two-dimensional) or template-based (one-dimensional) geometries, using various chemical and physical processes. In this Letter, we demonstrate the ambient environment localized pulsed electrodeposition process for direct printing of three-dimensional (3D) freestanding nanotwinned-Copper (nt-Cu) nanostructures. 3D nt-Cu structures were additively manufactured using pulsed electrodeposition at the tip of an electrolyte-containing nozzle. Focused ion beam (FIB) and transmission electron microscopy (TEM) analysis revealed that the printed metal was fully dense, and was mostly devoid of impurities and microstructural defects. FIB and TEM images also revealed nanocrystalline-nanotwinned-microstructure (nc-nt-microstructure), and confirmed the formation of coherent twin boundaries in the 3D-printed Cu. Mechanical properties of the 3D-printed nc-nt-Cu were characterized by direct printing (FIB-less) of micropillars for in situ SEM microcompression experiments. The 3D-printed nc-nt-Cu exhibited a flow stress of over 960 MPa, among the highest ever reported, which is remarkable for a 3D-printed material. The microstructure and mechanical properties of the nc-nt-Cu were compared to those of nc-Cu printed using the same process under direct current (DC) voltage.

Analysis of the Microstructure and Mechanical Properties of Titanium-Based Composites Reinforced by Secondary Phases and B4C Particles Produced via Direct Hot Pressing

PubMed Central

Montealegre-Melendez, Isabel; Arévalo, Cristina; Ariza, Enrique; Rubio-Escudero, Cristina; Kitzmantel, Michael; Neubauer, Erich

2017-01-01

In the last decade, titanium metal matrix composites (TMCs) have received considerable attention thanks to their interesting properties as a consequence of the clear interface between the matrix and the reinforcing phases formed. In this work, TMCs with 30 vol % of B4C are consolidated by hot pressing. This technique is a powder metallurgy rapid process. Incorporation of the intermetallic to the matrix, 20 vol % (Ti-Al), is also evaluated. Here, the reinforcing phases formed by the reaction between the titanium matrix and the ceramic particles, as well as the intermetallic addition, promote substantial variations to the microstructure and to the properties of the fabricated composites. The influences of the starting materials and the consolidation temperature (900 °C and 1000 °C) are investigated. By X-ray diffraction, scanning and transmission electron microscopy analysis, the in-situ-formed phases in the matrix and the residual ceramic particles were studied. Furthermore, mechanical properties are studied through tensile and bending tests in addition to other properties, such as Young’s modulus, hardness, and densification of the composites. The results show the significant effect of temperature on the microstructure and on the mechanical properties from the same starting powder. Moreover, the Ti-Al addition causes variation in the interface between the reinforcement and the matrix, thereby affecting the behaviour of the TMCs produced at the same temperature. PMID:29077066

Probing multi-scale mechanical damage in connective tissues using X-ray diffraction.

PubMed

Bianchi, Fabio; Hofmann, Felix; Smith, Andrew J; Thompson, Mark S

2016-11-01

The accumulation of microstructural collagen damage following repetitive loading is linked to painful and debilitating tendon injuries. As a hierarchical, semi-crystalline material, collagen mechanics can be studied using X-ray diffraction. The aim of the study was to describe multi-structural changes in tendon collagen following controlled plastic damage (5% permanent strain). We used small angle X-ray scattering (SAXS) to interrogate the spacing of collagen molecules within a fibril, and wide angle X-ray scattering (WAXS) to measure molecular strains under macroscopic loading. Simultaneous recordings of SAXS and WAXS patterns, together with whole-tissue strain in physiologically hydrated rat-tail tendons were made during increments of in situ tensile loading. Results showed that while tissue level modulus was unchanged, fibril modulus decreased significantly, and molecular modulus significantly increased. Further, analysis of higher order SAXS peaks suggested structural changes in the gap and overlap regions, possibly localising the damage to molecular cross-links. Our results provide new insight into the fundamental damage processes at work in collagenous tissues and point to new directions for their mitigation and repair. This article reports the first in situ loading synchrotron studies on mechanical damage in collagenous tissues. We provide new insight into the nano- and micro-structural mechanisms of damage processes. Pre-damaged tendons showed differential alteration of moduli at macro, micro and nano-scales as measured using X-ray scattering techniques. Detailed analysis of higher order diffraction peaks suggested damage is localised to molecular cross-links. The results are consistent with previous X-ray scattering studies of tendons and also with recent thermal stability studies on damaged material. Detailed understanding of damage mechanisms is essential in the development of new therapies promoting tissue repair. Copyright © 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

In situ electric properties of Ag films deposited on rough substrates

NASA Astrophysics Data System (ADS)

Zhou, Hong; Yu, Sen-Jiang; Zhang, Yong-Ju; Chen, Miao-Gen; Jiao, Zhi-Wei; Si, Ping-Zhan

2013-01-01

Silver (Ag) films have been deposited on rough substrates (including frosted glass and silicone grease), and for comparison on flat glass, by DC-magnetron sputtering, and their sheet resistances measured in situ during deposition. It is found that the growth of Ag films proceeds through three distinct stages: discontinuous, semi-continuous, and continuous regimes. The sheet resistance on rough substrates jumps in the vicinity of the percolation threshold, whereas the resistance on flat substrates decreases monotonically during deposition. The abnormal in situ electric properties on rough substrates are well explained based on the differences of the growth mechanism and microstructure of Ag films on different substrates.

Identification of ginseng root using quantitative X-ray microtomography.

PubMed

Ye, Linlin; Xue, Yanling; Wang, Yudan; Qi, Juncheng; Xiao, Tiqiao

2017-07-01

The use of X-ray phase-contrast microtomography for the investigation of Chinese medicinal materials is advantageous for its nondestructive, in situ , and three-dimensional quantitative imaging properties. The X-ray phase-contrast microtomography quantitative imaging method was used to investigate the microstructure of ginseng, and the phase-retrieval method is also employed to process the experimental data. Four different ginseng samples were collected and investigated; these were classified according to their species, production area, and sample growth pattern. The quantitative internal characteristic microstructures of ginseng were extracted successfully. The size and position distributions of the calcium oxalate cluster crystals (COCCs), important secondary metabolites that accumulate in ginseng, are revealed by the three-dimensional quantitative imaging method. The volume and amount of the COCCs in different species of the ginseng are obtained by a quantitative analysis of the three-dimensional microstructures, which shows obvious difference among the four species of ginseng. This study is the first to provide evidence of the distribution characteristics of COCCs to identify four types of ginseng, with regard to species authentication and age identification, by X-ray phase-contrast microtomography quantitative imaging. This method is also expected to reveal important relationships between COCCs and the occurrence of the effective medicinal components of ginseng.

Effect of a weak transverse magnetic field on the microstructure in directionally solidified peritectic alloys

PubMed Central

Li, Xi; Lu, Zhenyuan; Fautrelle, Yves; Gagnoud, Annie; Moreau, Rene; Ren, Zhongming

2016-01-01

Effect of a weak transverse magnetic field on the microstructures in directionally solidified Fe-Ni and Pb-Bi peritectic alloys has been investigated experimentally. The results indicate that the magnetic field can induce the formation of banded and island-like structures and refine the primary phase in peritectic alloys. The above results are enhanced with increasing magnetic field. Furthermore, electron probe micro analyzer (EPMA) analysis reveals that the magnetic field increases the Ni solute content on one side and enhances the solid solubility in the primary phase in the Fe-Ni alloy. The thermoelectric (TE) power difference at the liquid/solid interface of the Pb-Bi peritectic alloy is measured in situ, and the results show that a TE power difference exists at the liquid/solid interface. 3 D numerical simulations for the TE magnetic convection in the liquid are performed, and the results show that a unidirectional TE magnetic convection forms in the liquid near the liquid/solid interface during directional solidification under a transverse magnetic field and that the amplitude of the TE magnetic convection at different scales is different. The TE magnetic convections on the macroscopic interface and the cell/dendrite scales are responsible for the modification of microstructures during directional solidification under a magnetic field. PMID:27886265

Laser-Deposited In Situ TiC-Reinforced Nickel Matrix Composites: 3D Microstructure and Tribological Properties (Postprint)

DTIC Science & Technology

2014-04-03

reinforcements as well as nature of matrix reinforcement interface.2,8 In situ MMCs exhibit thermodynamic stability, good inter- facial bonding, and uniform...of these Ni-Ti-C composites. A dual-beam workstation (FEI Nova NanoSEM) equipped with a focused ion beam column employing a Gallium (Ga) liquid metal...commercially available solution thermodynamic models (PANDATTM from Compu- Therm), are shown in Fig. 5 a–d. The points corre- sponding to the Ni-17Ti-17C

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.

Evidence for Microfossils in Ancient Rocks and Meteorites

NASA Technical Reports Server (NTRS)

Hoover, Richard B.; Rozanov, A. Y.; Zhmur, S. I.; Gorlenko, V. M.

1998-01-01

The McKay et all. detection of chemical biomarkers and possible microfossils in an ancient meteorite from Mars (ALH84001) stimulated research in several areas of importance to the newly emerging field of Astrobiology. Their report resulted in a search for additional evidence of microfossils in ancient terrestrial rocks and meteorites. These studies of ancient rocks and meteorites were conducted independently (and later collaboratively) in the United States and Russia using the SEM, Environmental Scanning Electron Microscope (ESEM), and Field Emission Scanning Electron Microscope (FESEM). We have encountered in-situ in freshly broken carbonaceous chondrites a large number of complex microstructures that appear to be lithified microbial forms. The meteoritic microstructures have characteristics similar to the lithified remains of filamentous cyanobacteria and bacterial microfossils we have found in ancient phosphorites, ancient graphites and oil shales. Energy Dispersive Spectroscopy (EDS) and Link microprobe analysis shows the possible microfossils have a distribution of chemical elements characteristic of the meteorite rock matrix, although many exhibit a superimposed carbon enhancement. We have concluded that the mineralized bodies encountered embedded in the rock matrix of freshly fractured meteoritic surfaces can not be dismissed as recent surface contaminants. Many of the forms found in-situ in the Murchison, Efremovka, and Orgueil carbonaceous meteorites are strikingly similar to microfossils of coccoid bacteria, cyanobacteria and fungi such as we have found in the Cambrian phosphorites of Khubsugul, Mongolia and high carbon Phanerozoic and Precambrian rocks of the Siberian and Russian Platforms.

Microstructural evolution and wear behaviors of laser cladding Ti2Ni/α(Ti) dual-phase coating reinforced by TiB and TiC

NASA Astrophysics Data System (ADS)

Song, R.; Li, J.; Shao, J. Z.; Bai, L. L.; Chen, J. L.; Qu, C. C.

2015-11-01

The Ti2Ni/α(Ti) dual-phase coating reinforced by TiB and TiC was fabricated on the Ti6Al4V substrate by laser cladding. Phase constituents were confirmed by a theoretical prediction combined with X-ray diffraction (XRD) analyses. From the surface to the bottom of the coating, a regular evolution of the reinforcements' microstructure, namely TiCp+(TiB+TiC)e, (TiB+TiC)e and TiBp+(TiB+TiC)e (p and e were the abbreviations of primary and eutectic, respectively), was investigated by scanning electron microscopy (SEM). The coating possessed the higher microhardness than that of the substrate. An in situ dynamic method (in situ continuing tests at different time intervals) was designed to reveal wear behaviors at different wear stages. A quantitative calculation formula was established by a mathematic model to predict wear losses under different sliding time and applied loads in a definite precision. The wear mechanism was transformed from brittle debonding (at 10 N) to the joint action of brittle debonding and micro-cutting (at 20 N and 30 N) due to the microstructural evolution across the depth from the surface of the coating.

Simulated Fission Gas Behavior in Silicide Fuel at LWR Conditions

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

Miao, Yinbin; Mo, Kun; Yacout, Abdellatif

As a promising candidate for the accident tolerant fuel (ATF) used in light water reactors (LWRs), the fuel performance of uranium silicide (U 3Si 2) at LWR conditions needs to be well-understood. However, existing experimental post-irradiation examination (PIE) data are limited to the research reactor conditions, which involve lower fuel temperature compared to LWR conditions. This lack of appropriate experimental data significantly affects the development of fuel performance codes that can precisely predict the microstructure evolution and property degradation at LWR conditions, and therefore evaluate the qualification of U 3Si 2 as an AFT for LWRs. Considering the high cost,more » long timescale, and restrictive access of the in-pile irradiation experiments, this study aims to utilize ion irradiation to simulate the inpile behavior of the U 3Si 2 fuel. Both in situ TEM ion irradiation and ex situ high-energy ATLAS ion irradiation experiments were employed to simulate different types of microstructure modifications in U 3Si 2. Multiple PIE techniques were used or will be used to quantitatively analyze the microstructure evolution induced by ion irradiation so as to provide valuable reference for the development of fuel performance code prior to the availability of the in-pile irradiation data.« less

The effect of rotating magnetic field on the microstructure of in situ TiB2/Cu composites

NASA Astrophysics Data System (ADS)

Zou, C.; Kang, H.; Li, R.; Li, M.; Wang, W.; Chen, Z.; Wang, T.

2016-03-01

Nano ceramic particulate reinforced metal matrix composites are confronted with the problem of particle aggregation emerging in the process of solidification. It sharply deteriorates the mechanical properties of the composites. In order to improve the microstructure and particle distribution, in situ TiB2/Cu composites were prepared using Ti and Cu-B master alloys in a vacuum medium frequency induction furnace equipped with a rotating magnetic field (RMF). The effect of RMF magnetic field intensity employed on the microstructure and particles distribution of the TiB2/Cu composites were investigated. The results show that with the applied RMF, TiB2 particles are homogeneously distributed in the copper matrix, which significantly improves the mechanical properties of TiB2/Cu composites. The mechanism of RMF may be ascribed to the following two aspects. On the one hand, the electromagnetic body force generated by appropriate RMF drives forced convection in the equatorial plane of composite melt during solidification. On the other hand, a secondary flow in the meridional plane is engendered by a radial pressure gradient, thus making a strong agitation in the melt. These two effects result in a homogenous dispersion of TiB2 particles in the copper matrix, and hence excellent properties of TiB2/Cu composites were obtained.

Structural integrity of additive materials: Microstructure, fatigue behavior, and surface processing

NASA Astrophysics Data System (ADS)

Book, Todd A.

Although Additive Manufacturing (AM) offers numerous performance advantages over existing methods, AM structures are not being utilized for critical aerospace and mechanical applications due to uncertainties in their structural integrity as a result of the microstructural variations and defects arising from the AM process itself. Two of these uncertainties are the observed scatter in tensile strength and fatigue lives of direct metal laser sintering (DMLS) parts. With strain localization a precursor for material failure, this research seeks to explore the impact of microstructural variations in DMLS produced materials on strain localization. The first part of this research explores the role of the microstructure in strain localization of DMLS produced IN718 and Ti6Al4V specimens (as-built and post-processed) through the characterization of the linkage between microstructural variations, and the accumulation of plastic strain during monotonic and low cycle fatigue loading. The second part of this research explores the feasibility for the application of select surface processing techniques in-situ during the DMLS build process to alter the microstructure in AlSi10Mg to reduce strain localization and improve material cohesion. This study is based on utilizing experimental observations through the employment of advanced material characterization techniques such as digital image correlation to illustrate the impacts of DMLS microstructural variation.

Investigation of porous asphalt microstructure using optical and electron microscopy.

PubMed

Poulikakos, L D; Partl, M N

2010-11-01

Direct observations of porous asphalt concrete samples in their natural state using optical and electron microscopy techniques led to useful information regarding the microstructure of two mixes and indicated a relationship between microstructure and in situ performance. This paper presents evidence that suboptimal microstructure can lead to premature failure thus making a first step in defining well or suboptimal performing pavements with a bottom-up approach (microstructure). Laboratory and field compaction produce different samples in terms of the microstructure. Laboratory compaction using the gyratory method has produced more microcracks in mineral aggregates after the binder had cooled. Well-performing mixes used polymer-modified binders, had a more homogeneous void structure with fewer elongated voids and better interlocking of the aggregates. Furthermore, well-performing mixes showed better distribution of the mastic and better coverage of the aggregates with bitumen. Low vacuum scanning electron microscopy showed that styrene butadiene styrene polymer modification in binder exists in the form of discontinuous globules and not continuous networks. A reduction in the polymer phase was observed as a result of aging and in-service use. © 2010 The Authors Journal compilation © 2010 The Royal Microscopical Society.

TEM in situ cube-corner indentation analysis using ViBe motion detection algorithm

NASA Astrophysics Data System (ADS)

Yano, K. H.; Thomas, S.; Swenson, M. J.; Lu, Y.; Wharry, J. P.

2018-04-01

Transmission electron microscopic (TEM) in situ mechanical testing is a promising method for understanding plasticity in shallow ion irradiated layers and other volume-limited materials. One of the simplest TEM in situ experiments is cube-corner indentation of a lamella, but the subsequent analysis and interpretation of the experiment is challenging, especially in engineering materials with complex microstructures. In this work, we: (a) develop MicroViBE, a motion detection and background subtraction-based post-processing approach, and (b) demonstrate the ability of MicroViBe, in combination with post-mortem TEM imaging, to carry out an unbiased qualitative interpretation of TEM indentation videos. We focus this work around a Fe-9%Cr oxide dispersion strengthened (ODS) alloy, irradiated with Fe2+ ions to 3 dpa at 500 °C. MicroViBe identifies changes in Laue contrast that are induced by the indentation; these changes accumulate throughout the mechanical loading to generate a "heatmap" of features in the original TEM video that change the most during the loading. Dislocation loops with b = ½ <111> identified by post-mortem scanning TEM (STEM) imaging correspond to hotspots on the heatmap, whereas positions of dislocation loops with b = <100> do not correspond to hotspots. Further, MicroViBe enables consistent, objective quantitative approximation of the b = ½ <111> dislocation loop number density.

Mechanical characterization of an additively manufactured Inconel 718 theta-shaped specimen

DOE PAGES

Cakmak, Ercan; Watkins, Thomas R.; Bunn, Jeffrey R.; ...

2015-11-20

Two sets of “theta”-shaped specimens were additively manufactured with Inconel 718 powders using an electron beam melting technique with two distinct scan strategies. Light optical microscopy, mechanical testing coupled with a digital image correlation (DIC) technique, finite element modeling, and neutron diffraction with in situ loading characterizations were conducted. The cross-members of the specimens were the focus. Light optical micrographs revealed that different microstructures were formed with different scan strategies. Ex situ mechanical testing revealed each build to be stable under load until ductility was observed on the cross-members before failure. The elastic moduli were determined by forming a correlationmore » between the elastic tensile stresses determined from FEM, and the elastic strains obtained from DIC. The lattice strains were mapped with neutron diffraction during in situ elastic loading; and a good correlation between the average axial lattice strains on the cross-member and those determined from the DIC analysis was found. Lastly, the spatially resolved stresses in the elastic deformation regime are derived from the lattice strains and increased with applied load, showing a consistent distribution along the cross-member.« less

Mechanical characterization of an additively manufactured Inconel 718 theta-shaped specimen

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

Cakmak, Ercan; Watkins, Thomas R.; Bunn, Jeffrey R.

Two sets of “theta”-shaped specimens were additively manufactured with Inconel 718 powders using an electron beam melting technique with two distinct scan strategies. Light optical microscopy, mechanical testing coupled with a digital image correlation (DIC) technique, finite element modeling, and neutron diffraction with in situ loading characterizations were conducted. The cross-members of the specimens were the focus. Light optical micrographs revealed that different microstructures were formed with different scan strategies. Ex situ mechanical testing revealed each build to be stable under load until ductility was observed on the cross-members before failure. The elastic moduli were determined by forming a correlationmore » between the elastic tensile stresses determined from FEM, and the elastic strains obtained from DIC. The lattice strains were mapped with neutron diffraction during in situ elastic loading; and a good correlation between the average axial lattice strains on the cross-member and those determined from the DIC analysis was found. Lastly, the spatially resolved stresses in the elastic deformation regime are derived from the lattice strains and increased with applied load, showing a consistent distribution along the cross-member.« less

Effect of magnesium content on the microstructure and dry sliding wear behavior of centrifugally cast functionally graded A356-Mg2Si in situ composites

NASA Astrophysics Data System (ADS)

Ram, Subhash Chandra; Chattopadhyay, K.; Chakrabarty, I.

2018-04-01

Functionally graded A356 alloy (Al–7.2Si–0.3Mg) –Mg2Si in situ composites have been synthesized via centrifugal casting route. Mg2Si particles tend to migrate towards the core of the tubular product by centrifugal force. The in situ formed Mg2Si particles in composites are characterized by x-ray diffraction (XRD) analysis, Energy dispersive spectrometry (EDS), Optical, Scanning Electron and Transmission Electron Microscopy. Apart from primary blocky Mg2Si particles the matrix contains other phases viz. Al-Si eutectic, pseudo-binary Al-Mg2Si eutectic and Al-Fe-Si intermetallics. Density is found to decrease and %porosity is increased with increase in volume fraction of Mg2Si. Maximum hardness was observed at the inner core region due to maximum segregation of Mg2Si particles and gradually decreases towards the outer periphery region. The dry sliding wear was evaluated with varying parameters such as normal loads (N) and sliding distances (m). A substantial increase in wear resistance at the inner core region is observed. From the worn surface characterization, the wear mechanisms have been explained.

Quantitative Analysis of Three-dimensional Microstructure of Li-ion Battery Electrodes

NASA Astrophysics Data System (ADS)

Liu, Zhao

Li-ion batteries (LIBs) have attracted considerable attention in the past two decades due to their widespread applications in portable electronics, and their growing use in electric vehicles and large-scale grid storage. Increasing battery energy density and powder density while maintaining long life, along with battery safety, are the biggest challenges that limit their further development. Various approaches with materials and chemistry have been employed to improve performance. However, one less-studied aspect that also impacts performance is the electrode microstructure. In particular, three-dimensional (3D) electrode microstructural data for LIB electrodes, which were not widely available prior to this thesis, can provide important input for understanding and improving LIB performance. The focus of this thesis is to apply 3D tomographic techniques, together with electrochemical performance data, to obtain LIB microstructure-performance correlations. Two advanced 3D structural analysis techniques, focused ion beam-scanning electron microscopy (FIB-SEM) and transmission X-ray microscopy (TXM) nanotomography, are used to quantify LIB electrode microstructure. 3D characterization of LIB electrode microstructure is used to obtain a deeper understanding of mechanisms that limit LIB performance. Microstructural characterization before and after cycling is used to explore capacity loss mechanisms. It is hoped that the results can guide electrode microstructures design to improve performance and stability. Two types of commercial electrodes, LiCoO2 and LiCoO 2/Li(Ni1/3Mn1/3Co1/3)O2, are studied using FIB-SEM and TXM. Both methods were found to be applicable to quantifying the oxide particle microstructure, including volume fraction, surface area, and particle size distribution, and results agreed well. However, structural inhomogeneity found in these commercial samples, limited the capability to resolve microstructural changes during cycling. In order to also quantify carbonaceous phases in the electrodes, which strongly correlate with LIB transport properties, a three-phase FIB-SEM method was developed where silicone resin was infiltrated into electrode pores, providing good image contrast with the carbon particles. Structural parameters including phase connectivity and tortuosity are quantified for commercial LiCoO 2 and laboratory-made LiFePO4 electrodes to help understand the transport process in these electrodes. For LiCoO2 electrodes, a heterogeneous tortuosity distribution observed in the electrolyte phase may result in inhomogeneous charge/discharge states, and consequently cause battery degradation. For LiFePO4 electrodes, highly percolated and less tortuous carbon found in a templated electrode explain its better high-C-rate performance. Finally, laboratory-made LiMn2O4 electrodes were electrochemically cycled with different operation parameters, including cycle number, temperature, and operating voltage. Quantitative analyses on 3D TXM data sets indicate particle fracture, mainly due to tetragonal to cubic phase transformations induced by the Jahn-Teller effect, resulting in electrode degradation. Moreover, high temperature operation is found to enhance active material dissolution and can also accelerate cell degradation. This ex-situ method, which combines electrochemical cycling and statistical analysis, proved to be an effective approach to provide insight for the interpretation of complex mechanical and electrochemical interactions within the electrodes.

3D microstructural evolution of primary recrystallization and grain growth in cold rolled single-phase aluminum alloys

NASA Astrophysics Data System (ADS)

Adam, Khaled; Zöllner, Dana; Field, David P.

2018-04-01

Modeling the microstructural evolution during recrystallization is a powerful tool for the profound understanding of alloy behavior and for use in optimizing engineering properties through annealing. In particular, the mechanical properties of metallic alloys are highly dependent upon evolved microstructure and texture from the softening process. In the present work, a Monte Carlo (MC) Potts model was used to model the primary recrystallization and grain growth in cold rolled single-phase Al alloy. The microstructural representation of two kinds of dislocation densities, statistically stored dislocations and geometrically necessary dislocations were quantified based on the ViscoPlastic Fast Fourier transform method. This representation was then introduced into the MC Potts model to identify the favorable sites for nucleation where orientation gradients and entanglements of dislocations are high. Additionally, in situ observations of non-isothermal microstructure evolution for single-phase aluminum alloy 1100 were made to validate the simulation. The influence of the texture inhomogeneity is analyzed from a theoretical point of view using an orientation distribution function for deformed and evolved texture.

Crystal Plasticity Model Validation Using Combined High-Energy Diffraction Microscopy Data for a Ti-7Al Specimen

DOE PAGES

Turner, Todd J.; Shade, Paul A.; Bernier, Joel V.; ...

2016-11-18

High-Energy Diffraction Microscopy (HEDM) is a 3-d x-ray characterization method that is uniquely suited to measuring the evolving micromechanical state and microstructure of polycrystalline materials during in situ processing. The near-field and far-field configurations provide complementary information; orientation maps computed from the near-field measurements provide grain morphologies, while the high angular resolution of the far-field measurements provide intergranular strain tensors. The ability to measure these data during deformation in situ makes HEDM an ideal tool for validating micro-mechanical deformation models that make their predictions at the scale of individual grains. Crystal Plasticity Finite Element Models (CPFEM) are one such classmore » of micro-mechanical models. While there have been extensive studies validating homogenized CPFEM response at a macroscopic level, a lack of detailed data measured at the level of the microstructure has hindered more stringent model validation efforts. We utilize an HEDM dataset from an alphatitanium alloy (Ti-7Al), collected at the Advanced Photon Source, Argonne National Laboratory, under in situ tensile deformation. The initial microstructure of the central slab of the gage section, measured via near-field HEDM, is used to inform a CPFEM model. The predicted intergranular stresses for 39 internal grains are then directly compared to data from 4 far-field measurements taken between ~4% and ~80% of the macroscopic yield strength. In conclusion, the intergranular stresses from the CPFEM model and far-field HEDM measurements up to incipient yield are shown to be in good agreement, and implications for application of such an integrated computational/experimental approach to phenomena such as fatigue and crack propagation is discussed.« less

Microstructure selection in thin-sample directional solidification of an Al-Cu alloy: In situ X-ray imaging and phase-field simulations

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

Clarke, A. J.; Tourret, D.; Song, Y.

We study microstructure selection during during directional solidification of a thin metallic sample. We combine in situ X-ray radiography of a dilute Al-Cu alloy solidification experiments with three-dimensional phase-field simulations. Here we explore a range of temperature gradient G and growth velocity V and build a microstructure selection map for this alloy. We investigate the selection of the primary dendritic spacing Λ and tip radius ρ. While ρ shows a good agreement between experimental measurements and dendrite growth theory, with ρ~V $-$1/2, Λ is observed to increase with V (∂Λ/∂V > 0), in apparent disagreement with classical scaling laws formore » primary dendritic spacing, which predict that ∂Λ/∂V<0. We show through simulations that this trend inversion for Λ(V) is due to liquid convection in our experiments, despite the thin sample configuration. We use a classical diffusion boundary-layer approximation to semi-quantitatively incorporate the effect of liquid convection into phase-field simulations. This approximation is implemented by assuming complete solute mixing outside a purely diffusive zone of constant thickness that surrounds the solid-liquid interface. This simple method enables us to quantitatively match experimental measurements of the planar morphological instability threshold and primary spacings over an order of magnitude in V. Lastly, we explain the observed inversion of ∂Λ/∂V by a combination of slow transient dynamics of microstructural homogenization and the influence of the sample thickness.« less

Microstructure selection in thin-sample directional solidification of an Al-Cu alloy: In situ X-ray imaging and phase-field simulations

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

Clarke, A. J.; Tourret, D.; Song, Y.

We study microstructure selection during directional solidification of a thin metallic sample. We combine in situ X-ray radiography of a dilute Al-Cu alloy solidification experiments with three-dimensional phase-field simulations. We explore a range of temperature gradient G and growth velocity V and build a microstructure selection map for this alloy. We investigate the selection of the primary dendritic spacing Lambda and tip radius rho. While rho shows a good agreement between experimental measurements and dendrite growth theory, with rho similar to V-1/2, Lambda is observed to increase with V (partial derivative Lambda/partial derivative V > 0), in apparent disagreement withmore » classical scaling laws for primary dendritic spacing, which predict that partial derivative Lambda/partial derivative V <0. We show through simulations that this trend inversion for Lambda(V) is due to liquid convection in our experiments, despite the thin sample configuration. We use a classical diffusion boundary-layer approximation to semi-quantitatively incorporate the effect of liquid convection into phase-field simulations. This approximation is implemented by assuming complete solute mixing outside a purely diffusive zone of constant thickness that surrounds the solid-liquid interface. This simple method enables us to quantitatively match experimental measurements of the planar morphological instability threshold and primary spacings over an order of magnitude in V. We explain the observed inversion of partial derivative Lambda/partial derivative V by a combination of slow transient dynamics of microstructural homogenization and the influence of the sample thickness.« less

Microstructure selection in thin-sample directional solidification of an Al-Cu alloy: In situ X-ray imaging and phase-field simulations

DOE PAGES

Clarke, A. J.; Tourret, D.; Song, Y.; ...

2017-05-01

We study microstructure selection during during directional solidification of a thin metallic sample. We combine in situ X-ray radiography of a dilute Al-Cu alloy solidification experiments with three-dimensional phase-field simulations. Here we explore a range of temperature gradient G and growth velocity V and build a microstructure selection map for this alloy. We investigate the selection of the primary dendritic spacing Λ and tip radius ρ. While ρ shows a good agreement between experimental measurements and dendrite growth theory, with ρ~V $-$1/2, Λ is observed to increase with V (∂Λ/∂V > 0), in apparent disagreement with classical scaling laws formore » primary dendritic spacing, which predict that ∂Λ/∂V<0. We show through simulations that this trend inversion for Λ(V) is due to liquid convection in our experiments, despite the thin sample configuration. We use a classical diffusion boundary-layer approximation to semi-quantitatively incorporate the effect of liquid convection into phase-field simulations. This approximation is implemented by assuming complete solute mixing outside a purely diffusive zone of constant thickness that surrounds the solid-liquid interface. This simple method enables us to quantitatively match experimental measurements of the planar morphological instability threshold and primary spacings over an order of magnitude in V. Lastly, we explain the observed inversion of ∂Λ/∂V by a combination of slow transient dynamics of microstructural homogenization and the influence of the sample thickness.« less

Irradiation-induced microstructural evolution and mechanical properties in iron with and without helium

NASA Astrophysics Data System (ADS)

Okuniewski, Maria Ann

Ferritic-martensitic steels have been identified as candidate structural materials for Generation IV reactors, fusion systems, and accelerator driven systems (ADS). These steels have been selected because of their superior radiation resistance to void swelling, irradiation creep, and helium (He) and hydrogen (H) embrittlement at higher temperatures (T/Tm > 0.4). In fusion and ADS reactors the structural materials will be subjected to irradiation damage, as well as the introduction of He and H. The He and H can be introduced via (n,alpha) and (n,p) threshold reactions, respectively. Also protons can be directly implanted from the beam in an ADS. In fusion and ADS environments the He generation is approximately 10 appm/dpa and 150 appm/dpa. The H generation is approximately three to ten times higher than He production in ADS environments. The impact of these large generation rates of He and H impurities on microstructural evolution during irradiation is not well understood. The irradiation-induced microstructural evolution and its relationship to mechanical properties in body-centered cubic (bcc) iron (Fe) with and without He was systematically investigated. The bcc Fe was selected as a simplified material to serve as a basis for a reactor structural material that was exposed to varying He-to-damage ratios to simulate fusion (10 appm/dpa) and ADS (150 appm/dpa) environments. Through utilizing relatively pure, single crystal, bcc Fe, microstructural and mechanical properties effects from alloying elements can be reduced, if not eliminated. Ion irradiations were carried out at two temperature regimes (300 and 450°C). A coordinated group of experiments and simulations were carried out. Following specimen irradiations, the resultant microstructure and mechanical properties were evaluated with both non-destructive and destructive experimental techniques. The experimental techniques included positron annihilation spectroscopy (PAS), specifically, Doppler broadening spectroscopy (DBS) and positron annihilation lifetime spectroscopy (PALS); in-situ and ex-situ transmission electron microscopy (TEM), nanoindentation, and atomic force microscopy (AFM). Kinetic lattice Monte Carlo (KLMC) was selected as the modeling technique since it has the capability of producing mesoscale results that can be directly compared to the length and time scales of the experimental work. ATomic SUPerposition (ATSUP) was utilized to calculate positron lifetimes and W parameters in Fe as a function of vacancy concentration. The results of the experiments and simulations were directly compared and related. The major findings included: (1) A link was established between the irradiated microstructure and its impact on mechanical properties. This was achieved through the quantitative evaluation of the ex-situ TEM defect analyses and the relationship of nanohardness to yield strength. The microstructural results from KMC modeling were also related to the mechanical properties through the Dispersed Barrier Model. (2) KMC was identified as a complementary technique for microstructural evaluation since it resulted in a distribution of defects that were not visible via TEM, however they are known to be present based on the PAS results. (3) PAS results and KMC simulations were compared with ATSUP calculations to quantify defect size versus positron lifetime.

Ultrasonic-assisted in-situ fabrication of BiOBr modified Bi2O2CO3 microstructure with enhanced photocatalytic performance.

PubMed

Cheng, Lijun; Hu, Xumin; Hao, Liang

2018-06-01

Via an ultrasonic-assisted in-situ etching method, BiOBr modified Bi 2 O 2 CO 3 microstructures were fabricated in short time. The samples were characterized by XRD, SEM, TEM, BET, UV-Vis, XPS and PL spectra methods. Rhodamine B (RhB) aqueous solution was applied to evaluate the photocatalytic activities of the as-prepared samples. The results showed that the sample prepared at pH of 2 in which the molar ratio of BiOBr and Bi 2 O 2 CO 3 was 0.69:1 had the largest specific surface area, the best utilization for ultraviolet and visible light and efficient separation efficiency of charge carriers, contributing to its best photocatalytic activity. O 2 - was proved to be main active species in RhB photodegradation process. Last, the photocatalytic mechanism of the composite was discussed in detail. Copyright © 2018 Elsevier B.V. All rights reserved.

In-situ transport and microstructural evolution in GaN Schottky diodes and epilayers exposed to swift heavy ion irradiation

NASA Astrophysics Data System (ADS)

Kumar, Ashish; Singh, R.; Kumar, Parmod; Singh, Udai B.; Asokan, K.; Karaseov, Platon A.; Titov, Andrei I.; Kanjilal, D.

2018-04-01

A systematic investigation of radiation hardness of Schottky barrier diodes and GaN epitaxial layers is carried out by employing in-situ electrical resistivity and cross sectional transmission electron microscopy (XTEM) microstructure measurements. The change in the current transport mechanism of Au/n-GaN Schottky barrier diodes due to irradiation is reported. The role of irradiation temperature and ion type was also investigated. Creation of damage is studied in low and medium electron energy loss regimes by selecting different ions, Ag (200 MeV) and O (100 MeV) at various fluences at two irradiation temperatures (80 K and 300 K). GaN resistivity increases up to 6 orders of magnitude under heavy Ag ions. Light O ion irradiation has a much lower influence on sheet resistance. The presence of isolated defect clusters in irradiated GaN epilayers is evident in XTEM investigation which is explained on the basis of the thermal spike model.

In Situ XRD Studies of the Process Dynamics During Annealing in Cold-Rolled Copper

NASA Astrophysics Data System (ADS)

Dey, Santu; Gayathri, N.; Bhattacharya, M.; Mukherjee, P.

2016-12-01

The dynamics of the release of stored energy during annealing along two different crystallographic planes, i.e., {111} and {220}, in deformed copper have been investigated using in situ X-ray diffraction measurements at 458 K and 473 K (185 °C and 200 °C). The study has been carried out on 50 and 80 pct cold-rolled Cu sheets. The microstructures of the rolled samples have been characterized using optical microscopy and electron backscattered diffraction measurements. The microstructural parameters were evaluated from the X-ray diffractogram using the Scherrer equation and the modified Rietveld method. The stored energy along different planes was determined using the modified Stibitz formula from the X-ray peak broadening, and the bulk stored energy was evaluated using differential scanning calorimetry. The process dynamics of recovery and recrystallization as observed through the release of stored energy have been modeled as the second-order and first-order processes, respectively.

In situ formation of titanium carbide using titanium and carbon-nanotube powders by laser cladding

NASA Astrophysics Data System (ADS)

Savalani, M. M.; Ng, C. C.; Li, Q. H.; Man, H. C.

2012-01-01

Titanium metal matrix composite coatings are considered to be important candidates for high wear resistance applications. In this study, TiC reinforced Ti matrix composite layers were fabricated by laser cladding with 5, 10, 15 and 20 wt% carbon-nanotube. The effects of the carbon-nanotube content on phase composition, microstructure, micro-hardness and dry sliding wear resistance of the coating were studied. Microstructural observation using scanning electron microscopy showed that the coatings consisted of a matrix of alpha-titanium phases and the reinforcement phase of titanium carbide in the form of fine dendrites, indicating that titanium carbide was synthesized by the in situ reaction during laser irradiation. Additionally, measurements on the micro-hardness and dry sliding wear resistance of the coatings indicated that the mechanical properties were affected by the amount of carbon-nanotube in the starting precursor materials and were enhanced by increasing the carbon-nanotube content. Results indicated that the composite layers exhibit high hardness and excellent wear resistance.

Novel symmetrical coralloid Cu 3D superstructures: Solid-state synthesis from a Cu-carboxylate MOF and their in-situ thermal conversion

NASA Astrophysics Data System (ADS)

Chen, Lingyun; Shen, Yongming; Bai, Junfeng; Wang, Chunzhao

2009-08-01

We describe here a one-step solid-state process for the synthesis of metal three-dimensional (3D) superstructures from a metal-organic framework (MOF). Novel symmetrical coralloid Cu 3D superstructures with surface interspersed with clusters of Cu nanoparticles were successfully synthesized by thermolysis of the [Cu 3( btc) 2] ( btc=benzene-1,3,5-tricarboxylato) MOF in a one-end closed horizontal tube furnace (OCTF). The obtained products were characterized by TGA, FT-IR, XRD, EDX, SEM, TEM, HRTEM and SAED. Different reaction conditions were discussed. Furthermore, the synthesized Cu samples were converted into CuO microstructures by in-situ calcination in the air. In addition, the possible formation mechanism was also proposed. This method is a simple and facile route, which builds a direct linkage between metal-carboxylate MOF crystals and metal nano- or microstructures and also opens a new application field of MOFs.

Preliminary in situ and real-time study of directional solidification of metallic alloys by x-ray imaging techniques

NASA Astrophysics Data System (ADS)

Nguyen Thi, H.; Jamgotchian, H.; Gastaldi, J.; Härtwig, J.; Schenk, T.; Klein, H.; Billia, B.; Baruchel, J.; Dabo, Y.

2003-05-01

During directional solidification of a binary alloy, the solid-liquid interface exhibits a variety of patterns that are due to the Mullins-Sekerka instability and governed by the growth conditions. It is well known that properties of the grown material are largely controlled by the microstructures left in the solid during processing. Thus, a precise mastering of the solidification is essential to tailor products in a reproducible fashion to a specified quality. One major difficulty for this study is the real-time and in situ observation of the interface, especially for metallic alloys. A possibility is to use an intense and coherent third generation x-ray beam. By combining different x-ray imaging techniques (absorption/phase contrast radiography and diffraction topography), we have studied the directional melting and solidification of aluminium-based alloys. The preliminary results show the great potential of these techniques for the study of the coupling between stress effects and microstructure formation in solidification processing.

The power of in situ pulsed laser deposition synchrotron characterization for the detection of domain formation during growth of Ba0.5Sr0.5TiO3 on MgO.

PubMed

Bauer, Sondes; Lazarev, Sergey; Molinari, Alan; Breitenstein, Andreas; Leufke, Philipp; Kruk, Robert; Hahn, Horst; Baumbach, Tilo

2014-03-01

A highly sophisticated pulsed laser deposition (PLD) chamber has recently been installed at the NANO beamline at the synchrotron facility ANKA (Karlsruhe, Germany), which allows for comprehensive studies on the PLD growth process of dielectric, ferroelectric and ferromagnetic thin films in epitaxial oxide heterostructures or even multilayer systems by combining in situ reflective high-energy diffraction with the in situ synchrotron high-resolution X-ray diffraction and surface diffraction methods. The modularity of the in situ PLD chamber offers the opportunity to explore the microstructure of the grown thin films as a function of the substrate temperature, gas pressure, laser fluence and target-substrate separation distance. Ba0.5Sr0.5TiO3 grown on MgO represents the first system that is grown in this in situ PLD chamber and studied by in situ X-ray reflectivity, in situ two-dimensional reciprocal space mapping of symmetric X-ray diffraction and acquisition of time-resolved diffraction profiles during the ablation process. In situ PLD synchrotron investigation has revealed the occurrence of structural distortion as well as domain formation and misfit dislocation which all depend strongly on the film thickness. The microstructure transformation has been accurately detected with a time resolution of 1 s. The acquisition of two-dimensional reciprocal space maps during the PLD growth has the advantage of simultaneously monitoring the changes of the crystalline structure as well as the formation of defects. The stability of the morphology during the PLD growth is demonstrated to be remarkably affected by the film thickness. A critical thickness for the domain formation in Ba0.5Sr0.5TiO3 grown on MgO could be determined from the acquisition of time-resolved diffraction profiles during the PLD growth. A splitting of the diffraction peak into two distinguishable peaks has revealed a morphology change due to modification of the internal strain during growth.

Analysis of sintered polymer scaffolds using concomitant synchrotron computed tomography and in situ mechanical testing.

PubMed

Dhillon, A; Schneider, P; Kuhn, G; Reinwald, Y; White, L J; Levchuk, A; Rose, F R A J; Müller, R; Shakesheff, K M; Rahman, C V

2011-12-01

The mechanical behaviour of polymer scaffolds plays a vital role in their successful use in bone tissue engineering. The present study utilised novel sintered polymer scaffolds prepared using temperature-sensitive poly(DL-lactic acid-co-glycolic acid)/poly(ethylene glycol) particles. The microstructure of these scaffolds was monitored under compressive strain by image-guided failure assessment (IGFA), which combined synchrotron radiation computed tomography (SR CT) and in situ micro-compression. Three-dimensional CT data sets of scaffolds subjected to a strain rate of 0.01%/s illustrated particle movement within the scaffolds with no deformation or cracking. When compressed using a higher strain rate of 0.02%/s particle movement was more pronounced and cracks between sintered particles were observed. The results from this study demonstrate that IGFA based on simultaneous SR CT imaging and micro-compression testing is a useful tool for assessing structural and mechanical scaffold properties, leading to further insight into structure-function relationships in scaffolds for bone tissue engineering applications.

The Microstructure Analysis of Barium M- Hexaferrite Particles Coated by Pani Conducting Material with In Situ Polymerization Process

NASA Astrophysics Data System (ADS)

Zainuri, M.; Amalia, L.

2017-05-01

Barium M-Hexaferrite (BaM) was synthesized by coprecipitation method and doped with Zn. Polyaniline (PANI) was synthesized by chemically and doped DBSA. The composite of PANI/BaM was synthesized by in situ polymerization method. The phase identification of the sample was performed by XRD, FTIR and SEM. Based on XRD data, the phase composition of BaM and hematite are 85.52 % and 14.48%. The characteristic peaks of PANI occur at 3435, 1637, 1473, 1298, 1127, 1009, and 799 cm-1. The characteristic metal oxide stretching peaks of BaM occurs at 575 and 437 cm-1. There is no phase changing in PANI/BaM composite. Based on SEM photography, the shape of BaM is hexagonal. The particle size of BaM powder ranges from 400-700 nm. The qualitative interfacial bonding between PANI and BaM particles are conducted very well and the both materials have good wettability.

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

Srivastava, Himanshu; Ganguli, Tapas; Deb, S. K.

The in-situ growth of CuO nanowires was studied by Energy Dispersive X-ray Diffraction (EDXRD) to observe the mechanism of growth. The study was carried out for comparison at two temperatures—at 500 °C, the optimum temperature of the nanowires growth, and at 300 °C just below the temperature range of the growth. The in situ observation revealed the successive oxidation of Cu foil to Cu{sub 2}O layer and finally to CuO layer. Further analysis showed the presence of a compressive stress in CuO layer due to interface at CuO and Cu{sub 2}O layers. The compressive stress was found to increase withmore » the growth of the nanowires at 500 °C while it relaxed with the growth of CuO layer at 300 °C. The present results do not support the existing model of stress relaxation induced growth of nanowires. Based on the detailed Transmission Electron Microscope, Scanning Electron Microscope, and EDXRD results, a microstructure based growth model has been suggested.« less

Mechanisms for Ductile Rupture - FY16 ESC Progress Report

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

Boyce, Brad L.; Carroll, Jay D.; Noell, Phillip

2017-01-01

Ductile rupture in metals is generally a multi-step process of void nucleation, growth, and coalescence. Particle decohesion and particle fracture are generally invoked as the primary microstructural mechanisms for room-temperature void nucleation. However, because high-purity materials also fail by void nucleation and coalescence, other microstructural features must also act as sites for void nucleation. Early studies of void initiation in high-purity materials, which included post-mortem fracture surface characterization using scanning electron microscopy (SEM) and high-voltage electron microscopy (HVEM) and in-situ HVEM observations of fracture, established the presence of dislocation cell walls as void initiation sites in high-purity materials. Direct experimentalmore » evidence for this contention was obtained during in-situ HVEM tensile tests of Be single crystals. Voids between 0.2 and 1 μm long appeared suddenly along dislocation cell walls during tensile straining. However, subsequent attempts to replicate these results in other materials, particularly α -Fe single crystals, were unsuccessful because of the small size of the dislocation cells, and these remain the only published in-situ HVEM observations of void nucleation at dislocation cell walls in the absence of a growing macrocrack. Despite this challenge, other approaches to studying void nucleation in high-purity metals also indicate that dislocation cell walls are nucleation sites for voids.« less

Short-Term Behavior of Slag Concretes Exposed to a Real In Situ Mediterranean Climate Environment

PubMed Central

Sánchez, Isidro

2017-01-01

At present, one of the most suitable ways to get a more sustainable cement industry is to reduce the CO2 emissions generated during cement production. In order to reach that goal, the use of ground granulated blast-furnace slag as clinker replacement is becoming increasingly popular. Although the effects of this addition in the properties of cementitious materials are influenced by their hardening conditions, there are not too many experimental studies in which slag concretes have been exposed to real in situ environments. Then, the main objective of this research is to study the short-term effects of exposure to real Mediterranean climate environment of an urban site, where the action of airborne chlorides from sea water and the presence of CO2 are combined, in the microstructure and service properties of a commercial slag cement concrete, compared to ordinary Portland cement (OPC). The microstructure was studied with mercury intrusion porosimetry. The effective porosity, capillary suction coefficient, chloride migration coefficient, carbonation front depth, and compressive strength were also analyzed. Considering the results obtained, slag concretes exposed to a real in situ Mediterranean climate environment show good service properties in the short-term (180 days), in comparison with OPC. PMID:28786936

ZT 0.1 Electron-Carrying Polymer Thermoelectric Composites with In Situ SnCl 2 Microstructure Growth (Open Access)

DTIC Science & Technology

2015-05-08

derivatives as potential dopants , [ 21 ] achieving elec- trical conductivities of nearly 0.01 S cm −1 and PF of 0.6 W m −1 K −2 . Segalman and co-workers...Weinheim cobalt (III) acetylacetonate (Co(acac) 3 )) to show more broadly that weakly doping microstructured inclusions can act synergis- tically with...P3 ) and PBTTT-C14 ( P4 ). The weak dopant Co(acac) 3 will form large crystals readily in p-type polymers such as P3 and P4 . S > 2000 µV K

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

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

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

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

Advanced Si solid phase crystallization for vertical channel in vertical NANDs

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

Lee, Sangsoo; Son, Yong-Hoon; Semiconductor R and D Center, Samsung Electronics Co., Ltd., Hwasung 445-701

The advanced solid phase crystallization (SPC) method using the SiGe/Si bi-layer structure is proposed to obtain high-mobility poly-Si thin-film transistors in next generation vertical NAND (VNAND) devices. During the SPC process, the top SiGe thin film acts as a selective nucleation layer to induce surface nucleation and equiaxial microstructure. Subsequently, this SiGe thin film microstructure is propagated to the underlying Si thin film by epitaxy-like growth. The initial nucleation at the SiGe surface was clearly observed by in situ transmission electron microscopy (TEM) when heating up to 600 °C. The equiaxial microstructures of both SiGe nucleation and Si channel layers weremore » shown in the crystallized bi-layer plan-view TEM measurements. Based on these experimental results, the large-grained and less-defective Si microstructure is expected to form near the channel region of each VNAND cell transistor, which may improve the electrical characteristics.« less

Microstructure and Sliding Wear Performance of Cr7C3-(Ni,Cr)3(Al,Cr) Coating Deposited from Cr7C3 In Situ Formed Atomized Powder

NASA Astrophysics Data System (ADS)

Zhu, Hong-Bin; Shen, Jie; Gao, Feng; Yu, Yueguang; Li, Changhai

2017-01-01

This work is aimed at developing a new type of Cr7C3-(Ni,Cr)3(Al,Cr) coating for parts used in heavy-duty diesel engines. The feedstock, in which the stripe-shaped Cr7C3 was in situ formed, was firstly prepared by vacuum melting and gas atomization and then subjected by high-velocity oxy-fuel spraying to form the coatings. The carbon content, microstructure and phase constitution of the powders, as well as the sprayed coatings, were analyzed by chemical analysis, SEM and XRD. The hardness and sliding wear performance of the sprayed coatings were also tested and compared to a commercial Cr3C2-NiCr coating used on piston rings. The results showed that the content of carbon in feedstock was almost the same as designed, and that the volume content of in situ formed Cr7C3 was increased with carbon and chromium added. The major phases of the powders and sprayed coatings are Cr7C3 and Cr-alloyed Ni3Al. Only a small amount of carbon lost during the spraying process. As Cr7C3 content increased in the coatings, the microhardness at room temperature was firstly increased to about 1000Hv0.3. The microhardness of the coatings stayed almost constant, while the testing temperature was raised up to 700 °C for 0.5 h, which illustrates the potential application of the investigated coatings under high temperature conditions. The coatings containing 70 and 77 vol.% Cr7C3 showed the most promising wear resistance, lower friction coefficient and better tribological compatibility to gray cast iron counterpart than other tested Cr7C3-(Ni,Cr)3(Al,Cr) coatings and the reference Cr3C2-NiCr coating.

Thermomechanical behavior and microstructural evolution of a Ni(Pd)-rich Ni 24.3Ti 49.7Pd 26 high temperature shape memory alloy

DOE PAGES

Benafan, O.; Garg, A.; Noebe, R. D.; ...

2015-04-20

We investigated the effect of thermomechanical cycling on a slightly Ni(Pd)-rich Ni 24.3Ti 49.7Pd 26 (near stochiometric Ni–Ti basis with Pd replacing Ni) high temperature shape memory alloy. Furthermore, aged tensile specimens (400 °C/24 h/furnace cooled) were subjected to constant-stress thermal cycling in conjunction with microstructural assessment via in situ neutron diffraction and transmission electron microscopy (TEM), before and after testing. It was shown that in spite of the slightly Ni(Pd)-rich composition and heat treatment used to precipitation harden the alloy, the material exhibited dimensional instabilities with residual strain accumulation reaching 1.5% over 10 thermomechanical cycles. This was attributed tomore » insufficient strengthening of the material (insufficient volume fraction of precipitate phase) to prevent plasticity from occurring concomitant with the martensitic transformation. In situ neutron diffraction revealed the presence of retained martensite while cycling under 300 MPa stress, which was also confirmed by transmission electron microscopy of post-cycled samples. Neutron diffraction analysis of the post-thermally-cycled samples under no-load revealed residual lattice strains in the martensite and austenite phases, remnant texture in the martensite phase, and peak broadening of the austenite phase. The texture we developed in the martensite phase was composed mainly of those martensitic tensile variants observed during thermomechanical cycling. Presence of a high density of dislocations, deformation twins, and retained martensite was revealed in the austenite state via in-situ TEM in the post-cycled material, providing an explanation for the observed peak broadening in the neutron diffraction spectra. Despite the dimensional instabilities, this alloy exhibited a biased transformation strain on the order of 3% and a two-way shape memory effect (TWSME) strain of ~2%, at relatively high actuation temperatures.« less

Acoustic Scattering Classification of Zooplankton and Microstructure

DTIC Science & Technology

2001-09-30

As part of this investigation, we have been observing concentrations of siphonulae, a larval form of the gas-bearing zooplankton siphonophore . The...situ measurements of acoustic target strengths of siphonophores , a gas-bearing zooplankter,” ICES J. Mar. Sci. 58: 740-749. Warren, J.D., T.K

Plasma-Sprayed Ti6Al4V Alloy Composite Coatings Reinforced with In Situ Formed TiB-TiN

NASA Astrophysics Data System (ADS)

Anand, Akrity; Das, Mitun; Kundu, Biswanath; Balla, Vamsi Krishna; Bodhak, Subhadip; Gangadharan, S.

2017-12-01

Plasma spraying was used to deposit premixed Ti6Al4V + 15 wt.% BN powder on titanium substrate to fabricate Ti6Al4V matrix composite coatings reinforced with in situ synthesized TiB-TiN. The formation of in situ TiB-TiN reinforcements increased with plasma power. The in situ reaction appears to be complete under present experimental conditions but with considerable oxidation of Ti in the composite coatings. The hardness of composite coatings was 7 times higher (855HV), and the in vitro wear rate (2.4 × 10-5 mm3/N m) was one order of magnitude less than that of titanium substrate. However, the microstructural non-uniformity decreased the corrosion resistance of these composite coatings in Hank's balanced salt solution.

Microstructure of Thin Films

DTIC Science & Technology

1990-02-07

Proceedings, Thin film Technologies II, 652, 256-263, (1986) B. Schmitt, J.P. Borgogno, G. Albrand and E. Pelletier, "In situ and air index measurements...34 SPIE Proceedings, "Optical Components and Systems", 805, 128 (1987) 11 B. Schmitt, J.P. Borgogno, G. Albrand and E. Pelletier. "In situ and air index...aT , m..a, lot,, o ,,f,02,d I4 k -1-1..... autocovariance lengths, less than 0.5 um, indicate that , 514n, ob0 o p’,Ofclllc....,,o,,oy0,1- agua sblrt

Surface 3D Micro Free Forms: Multifunctional Microstructured Mesoporous α-Alumina by in Situ Slip Casting Using Excimer Laser Ablated Polycarbonate Molds.

PubMed

Rowthu, Sriharitha; Böhlen, Karl; Bowen, Paul; Hoffmann, Patrik

2015-11-11

Ceramic surface microstructuring is a rapidly growing field with a variety of applications in tribology, wetting, biology, and so on. However, there are limitations to large-area microstructuring and fabrication of three-dimensional (3D) micro free forms. Here, we present a route to obtain intricate surface structures through in situ slip casting using polydimethylsiloxane (PDMS) negative molds which are replicated from excimer laser ablated polycarbonate (PC) master molds. PC sheets are ablated with a nanosecond KrF (λ = 248 nm) excimer laser mask projection system to obtain micron-scale 3D surface features over a large area of up to 3 m(2). Complex surface structures that include 3D free forms such as 3D topography of Switzerland, shallow structures such as diffractive optical elements (60 nm step) and conical micropillars have been obtained. The samples are defect-free produced with thicknesses of up to 10 mm and 120 mm diameter. The drying process of the slip cast alumina slurry takes place as a one-dimensional process, through surface evaporation and water permeation through the PDMS membrane. This allows homogeneous one-dimensional shrinkage during the drying process, independent of the sample's lateral dimensions. A linear mass diffusion model has been proposed to predict and explain the drying process of these ceramic colloidal suspensions. The calculated drying time is linearly proportional to the height of the slurry and the thickness of the negatively structured PDMS and is validated by the experimental results. An experimentally observed optimum Sylgard PDMS thickness range of ∼400 μm to 1 mm has achieved the best quality microstructured green compacts. Further, the model predicts that the drying time is independent of the microstructured areas and was validated using experimental observations carried out with microstructured areas of 300 mm(2), 1200 mm(2), and 120 cm(2). Therefore, in principle, the structures can be further replicated in areas up to 3 m(2) with the same drying time for the same slurry height. The surface-structured ceramics display interesting wetting properties, for example, eicosane-coated mesoporous microstructured alumina shows superhydrophobic behavior. Additionally, ceramic bulk samples could be further used as second-generation very hard and low-wear molds for further microfabrication.

Structure, electrical characteristics, and high-temperature stability of aerosol jet printed silver nanoparticle films

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

Rahman, Md Taibur; McCloy, John; Panat, Rahul, E-mail: rahul.panat@wsu.edu, E-mail: rvchintalapalle@utep.edu

Printed electronics has emerged as a versatile eco-friendly fabrication technique to create sintered nanoparticle (NP) films on arbitrary surfaces with an excellent control over the film microstructure. While applicability of such films for high-temperature applications is not explored previously, herein we report the high-temperature electrical stability of silver (Ag) metal NP films fabricated using an Aerosol Jet based printing technique and demonstrate that this behavior is dictated by changes in the film microstructure. In-situ high temperature (24–500 °C) impedance spectroscopy measurements show that the real part of the impedance increases with increasing temperature up to 150 °C, at which point a decreasingmore » trend prevails until 300 °C, followed again by an increase in impedance. The electrical behavior is correlated with the in-situ grain growth of the Ag NP films, as observed afterwards by scanning electron microscopy and X-ray diffraction (XRD), and could be tailored by controlling the initial microstructure through sintering conditions. Using combined diffraction and spectroscopic analytical methods, it is demonstrated the Aerosol Jet printed Ag NP films exhibit enhanced thermal stability and oxidation resistance. In addition to establishing the conditions for stability of Ag NP films, the results provide a fundamental understanding of the effect of grain growth and reduction in grain boundary area on the electrical stability of sintered NP films.« less

Structure, electrical characteristics, and high-temperature stability of aerosol jet printed silver nanoparticle films

NASA Astrophysics Data System (ADS)

Rahman, Md Taibur; McCloy, John; Ramana, C. V.; Panat, Rahul

2016-08-01

Printed electronics has emerged as a versatile eco-friendly fabrication technique to create sintered nanoparticle (NP) films on arbitrary surfaces with an excellent control over the film microstructure. While applicability of such films for high-temperature applications is not explored previously, herein we report the high-temperature electrical stability of silver (Ag) metal NP films fabricated using an Aerosol Jet based printing technique and demonstrate that this behavior is dictated by changes in the film microstructure. In-situ high temperature (24-500 °C) impedance spectroscopy measurements show that the real part of the impedance increases with increasing temperature up to 150 °C, at which point a decreasing trend prevails until 300 °C, followed again by an increase in impedance. The electrical behavior is correlated with the in-situ grain growth of the Ag NP films, as observed afterwards by scanning electron microscopy and X-ray diffraction (XRD), and could be tailored by controlling the initial microstructure through sintering conditions. Using combined diffraction and spectroscopic analytical methods, it is demonstrated the Aerosol Jet printed Ag NP films exhibit enhanced thermal stability and oxidation resistance. In addition to establishing the conditions for stability of Ag NP films, the results provide a fundamental understanding of the effect of grain growth and reduction in grain boundary area on the electrical stability of sintered NP films.

3D characterization of trans- and inter-lamellar fatigue crack in (α + β) Ti alloy

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

Babout, Laurent, E-mail: Laurent.babout@p.lodz.pl; Jopek, Łukasz; Preuss, Michael

2014-12-15

This paper presents a three dimensional image processing strategy that has been developed to quantitatively analyze and correlate the path of a fatigue crack with the lamellar microstructure found in Ti-6246. The analysis is carried out on X-ray microtomography images acquired in situ during uniaxial fatigue testing. The crack, the primary β-grain boundaries and the α lamellae have been segmented separately and merged for the first time to allow a better characterization and understanding of their mutual interaction. This has particularly emphasized the role of translamellar crack growth at a very high propagation angle with regard to the lamellar orientation,more » supporting the central role of colonies favorably oriented for basal 〈a〉 slip to guide the crack in the fully lamellar microstructure of Ti alloy. - Highlights: • 3D tomography images reveal strong short fatigue crack interaction with α lamellae. • Proposed 3D image processing methodology makes their segmentation possible. • Crack-lamellae orientation maps show prevalence of translamellar cracking. • Angle study comforts the influence of basal/prismatic slip on crack path.« less

Single-source-precursor synthesis of dense SiC/HfCxN1-x-based ultrahigh-temperature ceramic nanocomposites

NASA Astrophysics Data System (ADS)

Wen, Qingbo; Xu, Yeping; Xu, Binbin; Fasel, Claudia; Guillon, Olivier; Buntkowsky, Gerd; Yu, Zhaoju; Riedel, Ralf; Ionescu, Emanuel

2014-10-01

A novel single-source precursor was synthesized by the reaction of an allyl hydrido polycarbosilane (SMP10) and tetrakis(dimethylamido)hafnium(iv) (TDMAH) for the purpose of preparing dense monolithic SiC/HfCxN1-x-based ultrahigh temperature ceramic nanocomposites. The materials obtained at different stages of the synthesis process were characterized via Fourier transform infrared (FT-IR) as well as nuclear magnetic resonance (NMR) spectroscopy. The polymer-to-ceramic transformation was investigated by means of MAS NMR and FT-IR spectroscopy as well as thermogravimetric analysis (TGA) coupled with in situ mass spectrometry. Moreover, the microstructural evolution of the synthesized SiHfCN-based ceramics annealed at different temperatures ranging from 1300 °C to 1800 °C was characterized by elemental analysis, X-ray diffraction, Raman spectroscopy and transmission electron microscopy (TEM). Based on its high temperature behavior, the amorphous SiHfCN-based ceramic powder was used to prepare monolithic SiC/HfCxN1-x-based nanocomposites using the spark plasma sintering (SPS) technique. The results showed that dense monolithic SiC/HfCxN1-x-based nanocomposites with low open porosity (0.74 vol%) can be prepared successfully from single-source precursors. The average grain size of both HfC0.83N0.17 and SiC phases was found to be less than 100 nm after SPS processing owing to a unique microstructure: HfC0.83N0.17 grains were embedded homogeneously in a β-SiC matrix and encapsulated by in situ formed carbon layers which acted as a diffusion barrier to suppress grain growth. The segregated Hf-carbonitride grains significantly influenced the electrical conductivity of the SPS processed monolithic samples. While Hf-free polymer-derived SiC showed an electrical conductivity of ca. 1.8 S cm-1, the electrical conductivity of the Hf-containing material was analyzed to be ca. 136.2 S cm-1.A novel single-source precursor was synthesized by the reaction of an allyl hydrido polycarbosilane (SMP10) and tetrakis(dimethylamido)hafnium(iv) (TDMAH) for the purpose of preparing dense monolithic SiC/HfCxN1-x-based ultrahigh temperature ceramic nanocomposites. The materials obtained at different stages of the synthesis process were characterized via Fourier transform infrared (FT-IR) as well as nuclear magnetic resonance (NMR) spectroscopy. The polymer-to-ceramic transformation was investigated by means of MAS NMR and FT-IR spectroscopy as well as thermogravimetric analysis (TGA) coupled with in situ mass spectrometry. Moreover, the microstructural evolution of the synthesized SiHfCN-based ceramics annealed at different temperatures ranging from 1300 °C to 1800 °C was characterized by elemental analysis, X-ray diffraction, Raman spectroscopy and transmission electron microscopy (TEM). Based on its high temperature behavior, the amorphous SiHfCN-based ceramic powder was used to prepare monolithic SiC/HfCxN1-x-based nanocomposites using the spark plasma sintering (SPS) technique. The results showed that dense monolithic SiC/HfCxN1-x-based nanocomposites with low open porosity (0.74 vol%) can be prepared successfully from single-source precursors. The average grain size of both HfC0.83N0.17 and SiC phases was found to be less than 100 nm after SPS processing owing to a unique microstructure: HfC0.83N0.17 grains were embedded homogeneously in a β-SiC matrix and encapsulated by in situ formed carbon layers which acted as a diffusion barrier to suppress grain growth. The segregated Hf-carbonitride grains significantly influenced the electrical conductivity of the SPS processed monolithic samples. While Hf-free polymer-derived SiC showed an electrical conductivity of ca. 1.8 S cm-1, the electrical conductivity of the Hf-containing material was analyzed to be ca. 136.2 S cm-1. Electronic supplementary information (ESI) available: Raman spectroscopy characterization of the SiHfCN-based ceramics. See DOI: 10.1039/c4nr03376k

Investigations on the Mechanical Properties of Conducting Polymer Coating-Substrate Structures and Their Influencing Factors

PubMed Central

Wang, Xi-Shu; Tang, Hua-Ping; Li, Xu-Dong; Hua, Xin

2009-01-01

This review covers recent advances and work on the microstructure features, mechanical properties and cracking processes of conducting polymer film/coating- substrate structures under different testing conditions. An attempt is made to characterize and quantify the relationships between mechanical properties and microstructure features. In addition, the film cracking mechanism on the micro scale and some influencing factors that play a significant role in the service of the film-substrate structure are presented. These investigations cover the conducting polymer film/coating nucleation process, microstructure-fracture characterization, translation of brittle-ductile fractures, and cracking processes near the largest inherent macromolecule defects under thermal-mechanical loadings, and were carried out using in situ scanning electron microscopy (SEM) observations, as a novel method for evaluation of interface strength and critical failure stress. PMID:20054470

Three dimensional X-ray Diffraction Contrast Tomography Reconstruction of Polycrystalline Strontium Titanate during Sintering and Electron Backscatter Diffraction Validation

NASA Astrophysics Data System (ADS)

Syha, M.; Rheinheimer, W.; Loedermann, B.; Graff, A.; Trenkle, A.; Baeurer, M.; Weygand, D.; Ludwig, W.; Gumbsch, P.

The microstructural evolution of polycrystalline strontium titanate was investigated in three dimensions (3D) using X-ray diffraction contrast tomography (DCT) before and after ex-situ annealing at 1600°C. Post-annealing, the specimen was additionally subjected to phase contrast tomography (PCT) in order to finely resolve the porosities. The resulting microstructure reconstructions were studied with special emphasis on morphology and interface orientation during microstructure evolution. Subsequently, cross-sections of the specimen were studied using electron backscatter diffraction (EBSD). Corresponding cross-sections through the 3D reconstruction were identified and the quality of the reconstruction is validated with special emphasis on the spatial resolution at the grain boundaries, the size and location of pores contained in the material and the accuracy of the orientation determination.

Multi-Scale Modeling of Microstructural Evolution in Structural Metallic Systems

NASA Astrophysics Data System (ADS)

Zhao, Lei

Metallic alloys are a widely used class of structural materials, and the mechanical properties of these alloys are strongly dependent on the microstructure. Therefore, the scientific design of metallic materials with superior mechanical properties requires the understanding of the microstructural evolution. Computational models and simulations offer a number of advantages over experimental techniques in the prediction of microstructural evolution, because they can allow studies of microstructural evolution in situ, i.e., while the material is mechanically loaded (meso-scale simulations), and bring atomic-level insights into the microstructure (atomistic simulations). In this thesis, we applied a multi-scale modeling approach to study the microstructural evolution in several metallic systems, including polycrystalline materials and metallic glasses (MGs). Specifically, for polycrystalline materials, we developed a coupled finite element model that combines phase field method and crystal plasticity theory to study the plasticity effect on grain boundary (GB) migration. Our model is not only coupled strongly (i.e., we include plastic driving force on GB migration directly) and concurrently (i.e., coupled equations are solved simultaneously), but also it qualitatively captures such phenomena as the dislocation absorption by mobile GBs. The developed model provides a tool to study the microstructural evolution in plastically deformed metals and alloys. For MGs, we used molecular dynamics (MD) simulations to investigate the nucleation kinetics in the primary crystallization in Al-Sm system. We calculated the time-temperature-transformation curves for low Sm concentrations, from which the strong suppressing effect of Sm solute on Al nucleation and its influencing mechanism are revealed. Also, through the comparative analysis of both Al attachment and Al diffusion in MGs, it has been found that the nucleation kinetics is controlled by interfacial attachment of Al, and that the attachment behavior takes place collectively and heterogeneously, similarly to Al diffusion in MGs. Finally, we applied the MD technique to study the origin of five-fold twinning nucleation during the solidification of Al base alloys. We studied several model alloys and reported the observed nucleation pathway. We found that the key factors controlling the five-fold twinning are the twin boundary energy and the formation of pentagon structures, and the twin boundary energy plays the dominant role in the five-fold twinning in the model alloys studied.

The microstructure of capsule containing self-healing materials: A micro-computed tomography study

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

Van Stappen, Jeroen, E-mail: Jeroen.Vanstappen@uge

Autonomic self-healing materials are materials with built-in (micro-) capsules or vessels, which upon fracturing release healing agents in order to recover the material's physical and mechanical properties. In order to better understand and engineer these materials, a thorough characterization of the material's microstructural behavior is essential and often overlooked. In this context, micro-computed tomography (μCT) can be used to investigate the three dimensional distribution and (de)bonding of (micro-) capsules in their native state in a polymer system with self-healing properties. Furthermore, in-situ μCT experiments in a self-healing polymer and a self-healing concrete system can elucidate the breakage and leakage behaviormore » of (micro-) capsules at the micrometer scale. While challenges related to image resolution and contrast complicate the characterization in specific cases, non-destructive 3D imaging with μCT is shown to contribute to the understanding of the link between the microstructure and the self-healing behavior of these complex materials. - Highlights: • μCT imaging allows for the analysis of microcapsule distribution patterns in self-healing materials. • μCT allows for qualitative and quantitative measurements of healing agent release from carriers in self-healing materials. • Experimental set-ups can be optimized by changing chemical compounds in the system to ensure maximum quality imaging.« less

High cycle fatigue in the transmission electron microscope

DOE PAGES

Bufford, Daniel C.; Stauffer, Douglas; Mook, William M.; ...

2016-06-28

One of the most common causes of structural failure in metals is fatigue induced by cyclic loading. Historically, microstructure-level analysis of fatigue cracks has primarily been performed post mortem. However, such investigations do not directly reveal the internal structural processes at work near micro- and nanoscale fatigue cracks and thus do not provide direct evidence of active microstructural mechanisms. In this paper, the tension–tension fatigue behavior of nanocrystalline Cu was monitored in real time at the nanoscale by utilizing a new capability for quantitative cyclic mechanical loading performed in situ in a transmission electron microscope (TEM). Controllable loads were appliedmore » at frequencies from one to several hundred hertz, enabling accumulations of 10 6 cycles within 1 h. The nanometer-scale spatial resolution of the TEM allows quantitative fatigue crack growth studies at very slow crack growth rates, measured here at ~10 –12 m·cycle –1. This represents an incipient threshold regime that is well below the tensile yield stress and near the minimum conditions for fatigue crack growth. Evidence of localized deformation and grain growth within 150 nm of the crack tip was observed by both standard imaging and precession electron diffraction orientation mapping. Finally, these observations begin to reveal with unprecedented detail the local microstructural processes that govern damage accumulation, crack nucleation, and crack propagation during fatigue loading in nanocrystalline Cu.« less

Influence of CNTs decomposition during reactive friction-stir processing of an Al-Mg alloy on the correlation between microstructural characteristics and microtextural components.

PubMed

Khodabakhshi, F; Nosko, M; Gerlich, A P

2018-05-03

Multipass friction-stir processing was employed to uniformly disperse multiwalled carbon nanotubes (MW-CNTs) within an Al-Mg alloy metal matrix. Decomposition of MW-CNTs occurs in situ as a result of solid-state chemical reactions, forming fullerene (C60) and aluminium carbide (Al 4 C 3 ) phases during reactive high temperature severe plastic processing. The effects of this decomposition on the microstructural features, dynamic restoration mechanisms and crystallographic microtextural developments are studied for the first time by using electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) analysis. The formation of an equiaxed grain structure with an average size of ∼1.5 μm occurs within the stirred zone (SZ) under the influence of inclusions which hinder grain boundary migration via Zener-Smith pinning mechanisms during the discontinuous dynamic recrystallisation (DDRX). Formation of two strong Cubic and Brass microtextural components in the heat affected zone (HAZ) and thermomechanical affected zone (TMAZ) was noted as compared to the completely random and Cube components found in the base and SZ regions, respectively. The microstructural modification led to hardening and tensile strength improvement for the processed nanocomposite by ∼55% and 110%, respectively with respect to the annealed Al-Mg base alloy. © 2018 The Authors Journal of Microscopy © 2018 Royal Microscopical Society.

High cycle fatigue in the transmission electron microscope

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

Bufford, Daniel C.; Stauffer, Douglas; Mook, William M.

One of the most common causes of structural failure in metals is fatigue induced by cyclic loading. Historically, microstructure-level analysis of fatigue cracks has primarily been performed post mortem. However, such investigations do not directly reveal the internal structural processes at work near micro- and nanoscale fatigue cracks and thus do not provide direct evidence of active microstructural mechanisms. In this paper, the tension–tension fatigue behavior of nanocrystalline Cu was monitored in real time at the nanoscale by utilizing a new capability for quantitative cyclic mechanical loading performed in situ in a transmission electron microscope (TEM). Controllable loads were appliedmore » at frequencies from one to several hundred hertz, enabling accumulations of 10 6 cycles within 1 h. The nanometer-scale spatial resolution of the TEM allows quantitative fatigue crack growth studies at very slow crack growth rates, measured here at ~10 –12 m·cycle –1. This represents an incipient threshold regime that is well below the tensile yield stress and near the minimum conditions for fatigue crack growth. Evidence of localized deformation and grain growth within 150 nm of the crack tip was observed by both standard imaging and precession electron diffraction orientation mapping. Finally, these observations begin to reveal with unprecedented detail the local microstructural processes that govern damage accumulation, crack nucleation, and crack propagation during fatigue loading in nanocrystalline Cu.« less

Bridging Three Orders of Magnitude: Multiple Scattered Waves Sense Fractal Microscopic Structures via Dispersion

NASA Astrophysics Data System (ADS)

Lambert, Simon A.; Näsholm, Sven Peter; Nordsletten, David; Michler, Christian; Juge, Lauriane; Serfaty, Jean-Michel; Bilston, Lynne; Guzina, Bojan; Holm, Sverre; Sinkus, Ralph

2015-08-01

Wave scattering provides profound insight into the structure of matter. Typically, the ability to sense microstructure is determined by the ratio of scatterer size to probing wavelength. Here, we address the question of whether macroscopic waves can report back the presence and distribution of microscopic scatterers despite several orders of magnitude difference in scale between wavelength and scatterer size. In our analysis, monosized hard scatterers 5 μ m in radius are immersed in lossless gelatin phantoms to investigate the effect of multiple reflections on the propagation of shear waves with millimeter wavelength. Steady-state monochromatic waves are imaged in situ via magnetic resonance imaging, enabling quantification of the phase velocity at a voxel size big enough to contain thousands of individual scatterers, but small enough to resolve the wavelength. We show in theory, experiments, and simulations that the resulting coherent superposition of multiple reflections gives rise to power-law dispersion at the macroscopic scale if the scatterer distribution exhibits apparent fractality over an effective length scale that is comparable to the probing wavelength. Since apparent fractality is naturally present in any random medium, microstructure can thereby leave its fingerprint on the macroscopically quantifiable power-law exponent. Our results are generic to wave phenomena and carry great potential for sensing microstructure that exhibits intrinsic fractality, such as, for instance, vasculature.

Predictive characterization of aging and degradation of reactor materials in extreme environments. Final report, December 20, 2013 - September 20, 2017

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

Qu, Jianmin

Understanding of reactor material behavior in extreme environments is vital not only to the development of new materials for the next generation nuclear reactors, but also to the extension of the operating lifetimes of the current fleet of nuclear reactors. To this end, this project conducted a suite of unique experimental techniques, augmented by a mesoscale computational framework, to understand and predict the long-term effects of irradiation, temperature, and stress on material microstructures and their macroscopic behavior. The experimental techniques and computational tools were demonstrated on two distinctive types of reactor materials, namely, Zr alloys and high-Cr martensitic steels. Thesemore » materials are chosen as the test beds because they are the archetypes of high-performance reactor materials (cladding, wrappers, ducts, pressure vessel, piping, etc.). To fill the knowledge gaps, and to meet the technology needs, a suite of innovative in situ transmission electron microscopy (TEM) characterization techniques (heating, heavy ion irradiation, He implantation, quantitative small-scale mechanical testing, and various combinations thereof) were developed and used to elucidate and map the fundamental mechanisms of microstructure evolution in both Zr and Cr alloys for a wide range environmental boundary conditions in the thermal-mechanical-irradiation input space. Knowledge gained from the experimental observations of the active mechanisms and the role of local microstructural defects on the response of the material has been incorporated into a mathematically rigorous and comprehensive three-dimensional mesoscale framework capable of accounting for the compositional variation, microstructural evolution and localized deformation (radiation damage) to predict aging and degradation of key reactor materials operating in extreme environments. Predictions from this mesoscale framework were compared with the in situ TEM observations to validate the model.« less

Effect of heavy ion irradiation on microstructural evolution in CF8 cast austenitic stainless steel

DOE PAGES

Chen, Wei-Ying; Li, Meimei; Kirk, Marquis A.; ...

2015-08-21

The microstructural evolution in ferrite and austenitic in cast austenitic stainless steel (CASS) CF8, as received or thermally aged at 400 °C for 10,000 h, was followed under TEM with in situ irradiation of 1 MeV Kr ions at 300 and 350 °C to a fluence of 1.9 × 10 15 ions/cm 2 (~3 dpa) at the IVEM-Tandem Facility. For the unaged CF8, the irradiation-induced dislocation loops appeared at a much lower dose in the austenite than in the ferrite. At the end dose, the austenite formed a well-developed dislocation network microstructure, while the ferrite exhibited an extended dislocation structuremore » as line segments. Compared to the unaged CF8, the aged specimen appeared to have lower rate of damage accumulation. The rate of microstructural evolution under irradiation in the ferrite was significantly lower in the aged specimen than in the unaged. Finally, we attributed this difference to the different initial microstructures in the unaged and aged specimens, which implies that thermal aging and irradiation are not independent but interconnected damage processes.« less

Fast time-resolved aerosol collector: proof of concept

NASA Astrophysics Data System (ADS)

Yu, X.-Y.; Cowin, J. P.; Iedema, M. J.; Ali, H.

2010-10-01

Atmospheric particles can be collected in the field on substrates for subsequent laboratory analysis via chemically sensitive single particle methods such as scanning electron microscopy with energy dispersive x-ray analysis. With moving substrates time resolution of seconds to minutes can be achieved. In this paper, we demonstrate how to increase the time resolution when collecting particles on a substrate to a few milliseconds to provide real-time information. Our fast time-resolved aerosol collector ("Fast-TRAC") microscopically observes the particle collection on a substrate and records an on-line video. Particle arrivals are resolved to within a single frame (4-17 ms in this setup), and the spatial locations are matched to the subsequent single particle analysis. This approach also provides in-situ information on particle size and number concentration. Applications are expected in airborne studies of cloud microstructure, pollution plumes, and surface long-term monitoring.

Fast time-resolved aerosol collector: proof of concept

NASA Astrophysics Data System (ADS)

Yu, X.-Y.; Cowin, J. P.; Iedema, M. J.; Ali, H.

2010-06-01

Atmospheric particles can be collected in the field on substrates for subsequent laboratory analysis via chemically sensitive single particle methods such as scanning electron microscopy with energy dispersive x-ray analysis. With moving substrates time resolution of seconds to minutes can be achieved. In this paper, we demonstrate how to increase the time resolution when collecting particles on a substrate to a few milliseconds to provide real-time information. Our fast time-resolved aerosol collector ("Fast-TRAC") microscopically observes the particle collection on a substrate and records an on-line video. Particle arrivals are resolved to within a single frame (4-17 ms in this setup), and the spatial locations are matched to the subsequent single particle analysis. This approach also provides in-situ information on particle size and number concentration. Applications are expected in airborne studies of cloud microstructure, pollution plumes, and surface long-term monitoring.

Microscopy and microanalysis 1996

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

Bailey, G.W.; Corbett, J.M.; Dimlich, R.V.W.

1996-12-31

The Proceedings of this Annual Meeting contain paper of members from the three societies. These proceedings emphasizes the common research interests and attempts to eliminate some unwanted overlap. Topics covered are: microscopic analysis of animals with altered gene expression and in-situ gene and antibody localizations, high-resolution elemental mapping of nucleoprofein interactions, plant biology and pathology, quantitative HREM analysis of perfect and defected materials, computational methods for TEM image analysis, high-resolution FESM in materials research, frontiers in polymer microscopy and microanalysis, oxidation and corrosion, micro XRD and XRF, molecular microspectroscopy and spectral imaging, advances in confocal and multidimensional light microscopy, analyticalmore » electron microscopy in biology, correlative microscopy in biological sciences, grain-boundary microengineering, surfaces and interfaces, telepresence microscopy in education and research, MSA educational outreach, quantitative electron probe microanalysis, frontiers of analytical electron microscopy, critical issues in ceramic microstructures, dynamic organization of the cell, pathology, microbiology, high-resolution biological and cryo SEM, and scanning-probe microscopy.« less

In situ heavy ion irradiation studies of nanopore shrinkage and enhanced radiation tolerance of nanoporous Au

DOE PAGES

Li, Jin; Fan, Cuncai; Ding, Jie; ...

2017-01-03

High energy particle radiations induce severe microstructural damage in metallic materials. Nanoporous materials with a giant surface-to-volume ratio may alleviate radiation damage in irradiated metallic materials as free surface are defect sinks. We show, by using in situ Kr ion irradiation in a transmission electron microscope at room temperature, that nanoporous Au indeed has significantly improved radiation tolerance comparing with coarse-grained, fully dense Au. In situ studies show that nanopores can absorb and eliminate a large number of radiation-induced defect clusters. Meanwhile, nanopores shrink (self-heal) during radiation, and their shrinkage rate is pore size dependent. Furthermore, the in situ studiesmore » show dose-rate-dependent diffusivity of defect clusters. Our study sheds light on the design of radiation-tolerant nanoporous metallic materials for advanced nuclear reactor applications.« less

In Situ TEM Nanoindentation Studies on Stress-Induced Phase Transformations in Metallic Materials

DOE PAGES

Liu, Y.; Wang, H.; Zhang, X.

2015-11-30

Though abundant phase transformations are in general thermally driven processes, there are many examples wherein stresses can induce phase transformations. We applied numerous in situ techniques, such as in situ x-ray diffraction and neutron diffraction in order to reveal phase transformations. Recently, an in situ nanoindentation technique coupled with transmission electron microscopy demonstrated the capability to directly correlating stresses with phase transformations and microstructural evolutions at a submicron length scale. We briefly review in situ studies on stress-induced diffusional and diffusionless phase transformations in amorphous CuZrAl alloy and NiFeGa shape memory alloy. Moreover, in the amorphous CuZrAl, in situ nanoindentationmore » studies show that the nucleation of nanocrystals (a diffusional process) occurs at ultra-low stresses manifested by a prominent stress drop. In the NiFeGa shape memory alloy, two distinctive types of martensitic (diffusionless) phase transformations accompanied by stress plateaus are observed, including a reversible gradual phase transformation at low stress levels, and an irreversible abrupt phase transition at higher stress levels.« less

In situ ultrahigh-resolution optical coherence tomography characterization of eye bank corneal tissue processed for lamellar keratoplasty.

PubMed

Brown, Jamin S; Wang, Danling; Li, Xiaoli; Baluyot, Florence; Iliakis, Bernie; Lindquist, Thomas D; Shirakawa, Rika; Shen, Tueng T; Li, Xingde

2008-08-01

To use optical coherence tomography (OCT) as a noninvasive tool to perform in situ characterization of eye bank corneal tissue processed for lamellar keratoplasty. A custom-built ultrahigh-resolution OCT (UHR-OCT) was used to characterize donor corneal tissue that had been processed for lamellar keratoplasty. Twenty-seven donor corneas were analyzed. Four donor corneas were used as controls, whereas the rest were processed into donor corneal buttons for lamellar transplantation by using hand dissection, a microkeratome, or a femtosecond laser. UHR-OCT was also used to noninvasively characterize and monitor the viable corneal tissue immersed in storage medium over 3 weeks. The UHR-OCT captured high-resolution images of the donor corneal tissue in situ. This noninvasive technique showed the changes in donor corneal tissue morphology with time while in storage medium. The characteristics of the lamellar corneal tissue with each processing modality were clearly visible by UHR-OCT. The in situ characterization of the femtosecond laser-cut corneal tissue was noted to have more interface debris than shown by routine histology. The effects of the femtosecond laser microcavitation bubbles on the corneal tissue were well visualized at the edges of the lamellar flap while in storage medium. The results of our feasibility study show that UHR-OCT can provide superb, in situ microstructural characterization of eye bank corneal tissue noninvasively. The UHR-OCT interface findings and corneal endothelial disc thickness uniformity analysis are valuable information that may be used to optimize the modalities and parameters for lamellar tissue processing. The UHR-OCT is a powerful approach that will allow us to further evaluate the tissue response to different processing techniques for posterior lamellar keratoplasty. It may also provide information that can be used to correlate with postoperative clinical outcomes. UHR-OCT has the potential to become a routine part of tissue analysis for any eye bank or centers creating customized lamellar corneal tissue for transplantation.

Isothermal Time-Temperature-Precipitation Diagram for an Aluminum Alloy 6005A by In Situ DSC Experiments

PubMed Central

Milkereit, Benjamin; Giersberg, Lydia; Kessler, Olaf; Schick, Christoph

2014-01-01

Time-temperature-precipitation (TTP) diagrams deliver important material data, such as temperature and time ranges critical for precipitation during the quenching step of the age hardening procedure. Although the quenching step is continuous, isothermal TTP diagrams are often applied. Together with a so-called Quench Factor Analysis, they can be used to describe very different cooling paths. Typically, these diagrams are constructed based on mechanical properties or microstructures after an interrupted quenching, i.e., ex situ analyses. In recent years, an in situ calorimetric method to record continuous cooling precipitation diagrams of aluminum alloys has been developed to the application level by our group. This method has now been transferred to isothermal experiments, in which the whole heat treatment cycle was performed in a differential scanning calorimeter. The Al-Mg-Si-wrought alloy 6005A was investigated. Solution annealing at 540 °C and overcritical quenching to several temperatures between 450 °C and 250 °C were followed by isothermal soaking. Based on the heat flow curves during isothermal soaking, TTP diagrams were determined. An appropriate evaluation method has been developed. It was found that three different precipitation reactions in characteristic temperature intervals exist. Some of the low temperature reactions are not accessible in continuous cooling experiments and require isothermal studies. PMID:28788587

Preparation of a Strong Gelatin-Short Linear Glucan Nanocomposite Hydrogel by an in Situ Self-Assembly Process.

PubMed

Ge, Shengju; Li, Man; Ji, Na; Liu, Jing; Mul, Hongyan; Xiong, Liu; Sun, Qingjie

2018-01-10

Gelatin hydrogels exhibit excellent biocompatibility, nonimmunogenicity, and biodegradability, but they have limited applications in the food and medical industries because of their poor mechanical properties. Herein, we first developed an in situ self-assembly process for the preparation of gelatin-short linear glucan (SLG) nanocomposite hydrogels with enhanced mechanical strength. The microstructure, dynamic viscoelasticity, compression behavior, and thermal characteristics of the gelatin-SLG nanocomposite hydrogels were determined using scanning electron microscopy (SEM), dynamic rheological experiments, compression tests, and texture profile analysis tests. The SEM images revealed that nanoparticles were formed by the in situ self-assembly of SLG in the gelatin matrix and that the size of these nanoparticles ranged between 200 and 600 nm. The pores of the nanocomposite hydrogels were smaller than those of the pure gelatin hydrogels. Transmission electron microscopy images and X-ray diffraction further confirmed the presence of SLG nanoparticles with spherical shapes and B-type structures. Compared with pure gelatin hydrogels, the nanocomposite hydrogels exhibited improved mechanical behavior. Notably, the hardness and maximum values of the compressive stress of gelatin-SLG nanocomposites containing 5% SLG increased by about 2-fold and 3-fold, respectively, compared to the corresponding values of pure gelatin hydrogels.

Isothermal Time-Temperature-Precipitation Diagram for an Aluminum Alloy 6005A by In Situ DSC Experiments.

PubMed

Milkereit, Benjamin; Giersberg, Lydia; Kessler, Olaf; Schick, Christoph

2014-03-28

Time-temperature-precipitation (TTP) diagrams deliver important material data, such as temperature and time ranges critical for precipitation during the quenching step of the age hardening procedure. Although the quenching step is continuous, isothermal TTP diagrams are often applied. Together with a so-called Quench Factor Analysis, they can be used to describe very different cooling paths. Typically, these diagrams are constructed based on mechanical properties or microstructures after an interrupted quenching, i.e ., ex situ analyses. In recent years, an in situ calorimetric method to record continuous cooling precipitation diagrams of aluminum alloys has been developed to the application level by our group. This method has now been transferred to isothermal experiments, in which the whole heat treatment cycle was performed in a differential scanning calorimeter. The Al-Mg-Si-wrought alloy 6005A was investigated. Solution annealing at 540 °C and overcritical quenching to several temperatures between 450 °C and 250 °C were followed by isothermal soaking. Based on the heat flow curves during isothermal soaking, TTP diagrams were determined. An appropriate evaluation method has been developed. It was found that three different precipitation reactions in characteristic temperature intervals exist. Some of the low temperature reactions are not accessible in continuous cooling experiments and require isothermal studies.

Topograph for inspection of engine cylinder walls.

PubMed

Franz, S; Leonhardt, K; Windecker, R; Tiziani, H J

1999-12-20

The microstructural inspection of engine cylinder walls is an important task for quality management in the automotive industry. Until recently, mainly tactile methods were used for this purpose. We present an optical instrument based on microscopic fringe projection that permits fast, reliable, and nondestructive measurements of microstructure. The field of view is 0.8 mm x 1.2 mm, with a spatial sampling of 1100 x 700 pixels. In contrast to conventional tactile sensors, the optical method provides fast in situ three-dimensional surface characterizations that provide more information about the surface than do line profiles. Measurements are presented, and advantages of this instrument for characterization of a surface are discussed.

Hot-crack test for aluminium alloys welds using TIG process

NASA Astrophysics Data System (ADS)

Niel, A.; Deschaux-Beaume, F.; Bordreuil, C.; Fras, G.

2010-06-01

Hot cracking is a critical defect frequently observed during welding of aluminium alloys. In order to better understand the interaction between cracking phenomenon, process parameters, mechanical factors and microstructures resulting from solidification after welding, an original hot-cracking test during welding is developed. According to in-situ observations and post mortem analyses, hot cracking mechanisms are investigated, taking into account the interaction between microstructural parameters, depending on the thermal cycles, and mechanical parameters, depending on geometry and clamping conditions of the samples and on the thermal field on the sample. Finally, a process map indicating the limit between cracking and non-cracking zones according to welding parameters is presented.

Characterization of deformation mechanisms in zirconium alloys: effect of temperature and irradiation

NASA Astrophysics Data System (ADS)

Long, Fei

Zirconium alloys have been widely used in the CANDU (CANada Deuterium Uranium) reactor as core structural materials. Alloy such as Zircaloy-2 has been used for calandria tubes; fuel cladding; the pressure tube is manufactured from alloy Zr-2.5Nb. During in-reactor service, these alloys are exposed to a high flux of fast neutron at elevated temperatures. It is important to understand the effect of temperature and irradiation on the deformation mechanism of zirconium alloys. Aiming to provide experimental guidance for future modeling predictions on the properties of zirconium alloys this thesis describes the result of an investigation of the change of slip and twinning modes in Zircaloy-2 and Zr-2.5Nb as a function of temperature and irradiation. The aim is to provide scientific fundamentals and experimental evidences for future industry modeling in processing technique design, and in-reactor property change prediction of zirconium components. In situ neutron diffraction mechanical tests carried out on alloy Zircaloy-2 at three temperatures: 100¢ªC, 300¢ªC, and 500¢ªC, and described in Chapter 3. The evolution of the lattice strain of individual grain families in the loading and Poisson's directions during deformation, which probes the operation of slip and twinning modes at different stress levels, are described. By using the same type of in situ neutron diffraction technique, tests on Zr-2.5Nb pressure tube material samples, in either the fast-neutron irradiated or un-irradiated condition, are reported in Chapter 4. In Chapter 5, the measurement of dislocation density by means of line profile analysis of neutron diffraction patterns, as well as TEM observations of the dislocation microstructural evolution, is described. In Chapter 6 a hot-rolled Zr-2.5Nb with a larger grain size compared with the pressure tubing was used to study the development of dislocation microstructures with increasing plastic strain. In Chapter 7, in situ loading of heavy ion irradiated hot-rolled Zr-2.5Nb alloy is described, providing evidence for the interaction between moving dislocations and irradiation induced loops. Chapter 8 gives the effect on the dislocation structure of different levels of compressive strains along two directions in the hot-rolled Zr-2.5Nb alloy. By using high resolution neutron diffraction and TEM observations, the evolution of type and dislocation densities, as well as changes of dislocation microstructure with plastic strain were characterized.

In situ observation of fracture processes in high-strength concretes and limestone using high-speed X-ray phase-contrast imaging

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

Parab, Niranjan D.; Guo, Zherui; Hudspeth, Matthew

The mechanical properties and fracture mechanisms of geomaterials and construction materials such as concrete are reported to be dependent on the loading rates. However, the in situ cracking inside such specimens cannot be visualized using traditional optical imaging methods since the materials are opaque. In this study, the in situ sub-surface failure/damage mechanisms in Cor-Tuf (a reactive powder concrete), a high-strength concrete (HSC) and Indiana limestone under dynamic loading were investigated using high-speed synchrotron X-ray phase-contrast imaging. Dynamic compressive loading was applied using a modified Kolsky bar and fracture images were recorded using a synchronized high-speed synchrotron X-ray imaging set-up.more » Three-dimensional synchrotron X-ray tomography was also performed to record the microstructure of the specimens before dynamic loading. In the Cor-Tuf and HSC specimens, two different modes of cracking were observed: straight cracking or angular cracking with respect to the direction of loading. In limestone, cracks followed the grain boundaries and voids, ultimately fracturing the specimen. Cracks in HSC were more tortuous than the cracks in Cor-Tuf specimens. The effects of the microstructure on the observed cracking behaviour are discussed. This article is part of the themed issue ‘Experimental testing and modelling of brittle materials at high strain rates’.« less

Experimental studies of Micro- and Nano-grained UO 2: Grain Growth Behavior, Sufrace Morphology, and Fracture Toughness

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

Miao, Yinbin; Mo, Kun; Jamison, Laura M.

This activity is supported by the US Nuclear Energy Advanced Modeling and Simulation (NEAMS) Fuels Product Line (FPL) and aims at providing experimental data for the validation of the mesoscale simulation code MARMOT. MARMOT is a mesoscale multiphysics code that predicts the coevolution of microstructure and properties within reactor fuel during its lifetime in the reactor. It is an important component of the Moose-Bison-Marmot (MBM) code suite that has been developed by Idaho National Laboratory (INL) to enable next generation fuel performance modeling capability as part of the NEAMS Program FPL. In order to ensure the accuracy of the microstructure-basedmore » materials models being developed within the MARMOT code, extensive validation efforts must be carried out. In this report, we summarize the experimental efforts in FY16 including the following important experiments: (1) in-situ grain growth measurement of nano-grained UO 2; (2) investigation of surface morphology in micrograined UO 2; (3) Nano-indentation experiments on nano- and micro-grained UO 2. The highlight of this year is: we have successfully demonstrated our capability to in-situ measure grain size development while maintaining the stoichiometry of nano-grained UO 2 materials; the experiment is, for the first time, using synchrotron X-ray diffraction to in-situ measure grain growth behavior of UO 2.« less

In situ TEM probing of crystallization form-dependent sodiation behavior in ZnO nanowires for sodium-ion batteries

DOE PAGES

Xu, Feng; Li, Zhengrui; Wu, Lijun; ...

2016-09-13

Development of sodium-ion battery (SIB) electrode materials currently lags behind electrodes in commercial lithium-ion batteries (LIBs). However, in the long term, development of SIB components is a valuable goal. Their similar, but not identical, chemistries require careful identification of the underlying sodiation mechanism in SIBs. Here in this study, we utilize in situ transmission electron microscopy to explore quite different sodiation behaviors even in similar electrode materials through real-time visualization of microstructure and phase evolution. Upon electrochemical sodiation, single-crystalline ZnO nanowires (sc-ZNWs) are found to undergo a step-by-step electrochemical displacement reaction, forming crystalline NaZn 13 nanograins dispersed in a Namore » 2O matrix. This process is characterized by a slowly propagating reaction front and the formation of heterogeneous interfaces inside the ZNWs due to non-uniform sodiation amorphization. In contrast, poly-crystalline ZNWs (pc-ZNWs) exhibited an ultrafast sodiation process, which can partly be ascribed to the availability of unobstructed ionic transport pathways among ZnO nanograins. Thus the reaction front and heterogeneous interfaces disappear. The in situ TEM results, supported by calculation of the ion diffusion coefficient, provide breakthrough insights into the dependence of ion diffusion kinetics on crystallization form. This points toward a goal of optimizing the microstructure of electrode materials in order to develop high performance SIBs.« less

Microstructure and wear resistance of one-step in-situ synthesized TiN/Al composite coatings on Ti6Al4V alloy by a laser nitriding process

NASA Astrophysics Data System (ADS)

Fu, Yao; Zhang, Xian-Cheng; Sui, Jian-Feng; Tu, Shan-Tung; Xuan, Fu-Zhen; Wang, Zheng-Dong

2015-04-01

The aim of this paper was to develop a one-step in situ method to synthesize the TiN reinforced Al metallic matrix composite coatings on Ti6Al4V alloy. In this method, the Al powder and nitrogen gas were simultaneously fed into feeding nozzle during a laser nitriding process. The microstructure, microhardness and sliding wear resistance of TiN/Al coatings synthesized at different laser powers in laser nitriding were investigated. Results showed that the crack- and pore-free coatings can be made through the proposed method. However, the morphologies and distribution of TiN dendrites and wear resistance of coatings were strongly dependent on laser power used in nitriding. With increasing the laser power, the amount and density of massive TiN dendritic structure in the coating decreased and the elongated and narrow dendrites increased, leading to the increment of wear resistance of coating. When the laser power is high, the convectional flow pattern of the melt pool can be seen near the bottom of pool.

Lithium electrodeposition dynamics in aprotic electrolyte observed in situ via transmission electron microscopy

DOE PAGES

Leenheer, Andrew Jay; Jungjohann, Katherine Leigh; Zavadil, Kevin Robert; ...

2015-03-18

Electrodeposited metallic lithium is an ideal negative battery electrode, but nonuniform microstructure evolution during cycling leads to degradation and safety issues. A better understanding of the Li plating and stripping processes is needed to enable practical Li-metal batteries. Here we use a custom microfabricated, sealed liquid cell for in situ scanning transmission electron microscopy (STEM) to image the first few cycles of lithium electrodeposition/dissolution in liquid aprotic electrolyte at submicron resolution. Cycling at current densities from 1 to 25 mA/cm 2 leads to variations in grain structure, with higher current densities giving a more needle-like, higher surface area deposit. Themore » effect of the electron beam was explored, and it was found that, even with minimal beam exposure, beam-induced surface film formation could alter the Li microstructure. The electrochemical dissolution was seen to initiate from isolated points on grains rather than uniformly across the Li surface, due to the stabilizing solid electrolyte interphase surface film. As a result, we discuss the implications for operando STEM liquid-cell imaging and Li-battery applications.« less

Microstructure characteristics and properties of in-situ formed TiC/Ni based alloy composite coating by laser cladding

NASA Astrophysics Data System (ADS)

Yang, Sen; Liu, Wenjin; Zhong, Minlin

2003-03-01

Different weight ratio of nickel based alloy, titanium and graphite powders were mixed and then laser cladded onto carbon steel substrate to produce a surface metal matrix composite layer. The experimental results showed that the coating was uniform, continuous and free of cracks. An excellent bonding between the coating and the carbon steel substrate was ensured by the strong metallurgical interface. The microstructures of the coating were mainly composed of γ-Ni dendrite, M23C6, a small amount of CrB, and dispersed TiC particles, and the in-situ generated TiCp/matrix interfaces were clean and free from deleterious surface reaction. The morphologies of TiC particles changed from the global, cluster to flower-like shape, the volume fraction of TiCp and the microhardness gradually increased from the bottom to the top of the coating layer, and the maximum microhardness of the coating was about HV0.2850, 3 times larger than that of steel substrate. The volume fraction of TiC particles increased with increasing of volume fraction of Ti and C too.

Stress and Strain Distributions during Machining of Ti-6Al-4V at Ambient and Cryogenic Temperatures

NASA Astrophysics Data System (ADS)

Rahman, Md. Fahim

Dry and liquid nitrogen pre-cooled Ti-6Al-4V samples were machined at a cutting speed of 43.2 m/min and at low (0.1 mm/rev) to high (0.4 mm/rev) feed rates for understanding the effects of temperature and strain rate on chip microstructures. During cryogenic machining, it was observed that between feed rates of 0.10 and 0.30 mm/rev, a 25% pressure reduction on tool occurred. Smaller number of chips and low tool/chip contact time and temperature were observed (compared to dry machining under ambient conditions). An in-situ set-up that consisted of a microscope and a lathe was constructed and helped to propose a novel serrated chip formation mechanism when microstructures (strain localization) and surface roughness were considered. Dimpled fracture surfaces observed in high-speed-machined chips were formed due to stable crack propagation that was also recorded during in-situ machining. An instability criterion was developed that showed easier strain localization within the 0.10-0.30mm/rev feed rate range.

Instant polysaccharide-based emulsions: impact of microstructure on lipolysis.

PubMed

Torcello-Gómez, Amelia; Foster, Timothy J

2017-06-21

The development of emulsion-based products through optimisation of ingredients, reduction in energy-input during manufacture, while fulfilling healthy attributes, are major objectives within the food industry. Instant emulsions can meet these features, but comprehensive studies are necessary to investigate the effect of the initial formulation on the final microstructure and, in turn, on the in vitro lipolysis, comprising the double aim of this work. The instant emulsion is formed within 1.5-3 min after pouring the aqueous phase into the oil phase which contains a mixture of emulsifier (Tween 20), swelling particles (Sephadex) and thickeners (hydroxypropylmethylcellulose, HPMC, and guar gum, GG) under mild shearing (180 rpm). The creation of oil-in-water emulsions is monitored in situ by viscosity analysis, the final microstructure visualised by microscopy and the release of free fatty acids under simulated intestinal conditions quantified by titration. Increasing the concentration and molecular weight (M w ) of GG leads to smaller emulsion droplets due to increased bulk viscosity upon shearing. This droplet size reduction is magnified when increasing the M w of HPMC or swelling capacity of viscosifying particles. In addition, in the absence of the emulsifier Tween 20, the sole use of high-Mw HPMC is effective in emulsification due to combined increased bulk viscosity and interfacial activity. Hence, optimisation of the ingredient choice and usage level is possible when designing microstructures. Finally, emulsions with larger droplet size (>20 μm) display a slower rate and lower extent of lipolysis, while finer emulsions (droplet size ≤20 μm) exhibit maximum rate and extent profiles. This correlates with the extent of emulsion destabilisation observed under intestinal conditions.

Preparation and Characterization of New Geopolymer-Epoxy Resin Hybrid Mortars

PubMed Central

Colangelo, Francesco; Roviello, Giuseppina; Ricciotti, Laura; Ferone, Claudio; Cioffi, Raffaele

2013-01-01

The preparation and characterization of metakaolin-based geopolymer mortars containing an organic epoxy resin are presented here for the first time. The specimens have been prepared by means of an innovative in situ co-reticulation process, in mild conditions, of commercial epoxy based organic resins and geopolymeric slurry. In this way, geopolymer based hybrid mortars characterized by a different content of normalized sand (up to 66% in weight) and by a homogeneous dispersion of the organic resin have been obtained. Once hardened, these new materials show improved compressive strength and toughness in respect to both the neat geopolymer and the hybrid pastes since the organic polymer provides a more cohesive microstructure, with a reduced amount of microcracks. The microstructural characterization allows to point out the presence of an Interfacial Transition Zone similar to that observed in cement based mortars and concretes. A correlation between microstructural features and mechanical properties has been studied too. PMID:28811418

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

NASA Astrophysics Data System (ADS)

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

2017-04-01

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

Single-source-precursor synthesis of dense SiC/HfC(x)N(1-x)-based ultrahigh-temperature ceramic nanocomposites.

PubMed

Wen, Qingbo; Xu, Yeping; Xu, Binbin; Fasel, Claudia; Guillon, Olivier; Buntkowsky, Gerd; Yu, Zhaoju; Riedel, Ralf; Ionescu, Emanuel

2014-11-21

A novel single-source precursor was synthesized by the reaction of an allyl hydrido polycarbosilane (SMP10) and tetrakis(dimethylamido)hafnium(iv) (TDMAH) for the purpose of preparing dense monolithic SiC/HfC(x)N(1-x)-based ultrahigh temperature ceramic nanocomposites. The materials obtained at different stages of the synthesis process were characterized via Fourier transform infrared (FT-IR) as well as nuclear magnetic resonance (NMR) spectroscopy. The polymer-to-ceramic transformation was investigated by means of MAS NMR and FT-IR spectroscopy as well as thermogravimetric analysis (TGA) coupled with in situ mass spectrometry. Moreover, the microstructural evolution of the synthesized SiHfCN-based ceramics annealed at different temperatures ranging from 1300 °C to 1800 °C was characterized by elemental analysis, X-ray diffraction, Raman spectroscopy and transmission electron microscopy (TEM). Based on its high temperature behavior, the amorphous SiHfCN-based ceramic powder was used to prepare monolithic SiC/HfC(x)N(1-x)-based nanocomposites using the spark plasma sintering (SPS) technique. The results showed that dense monolithic SiC/HfC(x)N(1-x)-based nanocomposites with low open porosity (0.74 vol%) can be prepared successfully from single-source precursors. The average grain size of both HfC0.83N0.17 and SiC phases was found to be less than 100 nm after SPS processing owing to a unique microstructure: HfC0.83N0.17 grains were embedded homogeneously in a β-SiC matrix and encapsulated by in situ formed carbon layers which acted as a diffusion barrier to suppress grain growth. The segregated Hf-carbonitride grains significantly influenced the electrical conductivity of the SPS processed monolithic samples. While Hf-free polymer-derived SiC showed an electrical conductivity of ca. 1.8 S cm(-1), the electrical conductivity of the Hf-containing material was analyzed to be ca. 136.2 S cm(-1).

Microstructure and fracture in SiC whisker reinforced 2124 aluminum composite

NASA Technical Reports Server (NTRS)

Nieh, T. G.; Raninen, R. A.; Chellman, D. J.

1985-01-01

The microstructures of extruded and hot-rolled 2124 Al-15 percent (by weight) SiC whisker composites have been investigated, experimentally. Among the specific factors studied were: the strength of the whisker-matrix interfaces; (2) the presence of oxides; (3) the presence of defective whiskers; (4) and the presence of distribution of intermetallic compounds, impurities in the SiC(w) powder, and microstructural inhomogeneities. Modifications in the microstructure of the SiC/AL composites due to hot rolling and extrusion are illustrated in a series of microphotographs. It was found that hot rolling along the axis of extrusion was associated with some types of whisker damage, while the whiskers still retain their original orientation. Hot-rolling perpendicular to the axis of extrusion, however, tended to rotate the whiskers and produced a nearly isotropic material. Whisker free zones were virtually eliminated or reduced in size by hot rolling. In situ Auger fractography of the composite showed that the interfacial bonding between the SiC and the Al matrix was good and that Al2O2 had no significant influence on the fracture mechanics of the composite.

New Development in Selective Laser Melting of Ti-6Al-4V: A Wider Processing Window for the Achievement of Fully Lamellar α + β Microstructures

NASA Astrophysics Data System (ADS)

Lui, E. W.; Xu, W.; Pateras, A.; Qian, M.; Brandt, M.

2017-12-01

Recent progress has shown that Ti-6Al-4V fabricated by selective laser melting (SLM) can achieve a fully lamellar α + β microstructure using 60 µm layer thickness in the as-built state via in situ martensite decomposition by manipulating the processing parameters. The potential to broaden the processing window was explored in this study by increasing the layer thickness to the less commonly used 90 µm. Fully lamellar α + β microstructures were produced in the as-built state using inter-layer times in the range of 1-12 s. Microstructural features such as the α-lath thickness and morphology were sensitive to both build height and inter-layer time. The α-laths produced using the inter-layer time of 1 s were much coarser than those produced with the inter-layer time of 12 s. The fine fully lamellar α + β structure resulted in tensile ductility of 11% and yield strength of 980 MPa. The tensile properties can be further improved by minimizing the presence of process-induced defects.

Impurity incorporation, deposition kinetics, and microstructural evolution in sputtered Ta films

NASA Astrophysics Data System (ADS)

Whitacre, Jay Fredric

There is an increasing need to control the microstructure in thin sputtered Ta films for application as high-temperature coatings or diffusion barriers in microelectronic interconnect structures. To this end, the relationship between impurity incorporation, deposition kinetics, and microstructural evolution was examined for room-temperature low growth rate DC magnetron sputtered Ta films. Impurity levels present during deposition were controlled by pumping the chamber to various base pressures before growth. Ar pressures ranging from 2 to 20 mTorr were used to create contrasting kinetic environments in the sputter gas. This affected both the distribution of adatom kinetic energies at the substrate as well as the rate of impurity desorption from the chamber walls: at higher Ar pressures adatoms has lower kinetic energies, and there was an increase in impurity concentration. X-ray diffraction, high-resolution transmission electron microscopy (HREM), transmission electron diffraction (TED), scanning electron microscopy (SEM), secondary ion mass spectrometry (SIMS), and x-ray photoelectron. spectroscopy (XPS) were used to examine film crystallography, microstructure, and composition. A novel laboratory-based in-situ x-ray diffractometer was constructed. This new set-up allowed for the direct observation of microstructural evolution during growth. Films deposited at increasingly higher Ar pressures displayed a systematic decrease in grain size and degree of texturing, while surface morphology was found to vary from a nearly flat surface to a rough surface with several length scales of organization. In-situ x-ray results showed that the rate of texture evolution was found to be much higher in films grown using lower Ar pressures. These effects were studied in films less than 200 A thick using high resolution x-ray diffraction in conjunction with a synchrotron light source (SSRL B.L. 7-2). Films grown using higher Ar pressures (above 10 mTorr) with a pre-growth base pressure of 1 x 10--6 Torr had grains less than 10 nm in diameter and significant amorphous content Calculated radial distribution functions show a significant increase in average inter-atomic spacing in films grown using higher base pressures and Ar pressures. The amorphous content in the films was determined via comparison between ideal crystalline diffraction patterns and actual data. Thinner films grown at higher Ar pressures had relatively greater amorphous content. Real-time process control using the in-situ diffractometer was also demonstrated. The effects observed are discussed in the context of previous theories and experiments that document room-temperature sputter film growth. The changes in film microstructure observed were impurity mediated. Specifically, oxygen desorbed from the chamber walls during growth were incorporated into the film and subsequently limited grain development and texturing. A second phase consisting of amorphous Ta2O5 formed between the grain nuclei. Adatom kinetics played a role in determining surface morphology: at low Ar pressures (2 mTorr) significant adatom kinetic energies served to flattened the film surface, though impurity levels dominated grain development even in these conditions.

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

Li, Jin; Fan, Cuncai; Ding, Jie

High energy particle radiations induce severe microstructural damage in metallic materials. Nanoporous materials with a giant surface-to-volume ratio may alleviate radiation damage in irradiated metallic materials as free surface are defect sinks. We show, by using in situ Kr ion irradiation in a transmission electron microscope at room temperature, that nanoporous Au indeed has significantly improved radiation tolerance comparing with coarse-grained, fully dense Au. In situ studies show that nanopores can absorb and eliminate a large number of radiation-induced defect clusters. Meanwhile, nanopores shrink (self-heal) during radiation, and their shrinkage rate is pore size dependent. Furthermore, the in situ studiesmore » show dose-rate-dependent diffusivity of defect clusters. Our study sheds light on the design of radiation-tolerant nanoporous metallic materials for advanced nuclear reactor applications.« less

Mechanisms and mechanics of shape loss during supersolidus liquid-phase sintering

NASA Astrophysics Data System (ADS)

Lal, Anand

Rapid sinter densification of relatively coarse prealloyed powders is possible by exceeding the solidus temperature in an approach termed supersolidus liquid phase sintering (SLPS). However, narrow processing windows for densification without distortion often limit this process. The liquid films at the grain boundaries that are responsible for densification also reduce the structural rigidity of components. Hence, components tend to slump under their own weight. Thus, the present study investigates shape loss during SLPS and rationalizes the processing and material factors with regard to separating densification from distortion. Experiments are performed on various prealloyed powders, including bronze, 316L stainless steel, and T15 tool steel. Differential thermal analysis, dilatometry, and in situ video imaging of sintering compacts are used to follow melting, densification, and distortion, respectively. Further, density and dimensional measurements are performed on sintered compacts. Results indicate a dependence of distortion on the sintering temperature and time, compact size, and melting behavior of the alloy. It is shown that the sintering temperature window, where high-density, precise components are obtained, can be widened for 316L stainless steel by boron addition. For the first time, a beam bending technique is used to measure the macroscopic apparent viscosity of semisolid bronze. The viscosity drops with temperature above the solidus and lies in the range of 108 to 106 Pa-s. Additionally, the in situ transverse rupture strength of bronze is measured to demonstrate the softening above the solidus temperature. Further, microstructural measurements are performed to enable correlation with the slumping behavior and viscosity. A model combining the deformation mechanisms, driving forces, and microstructural characteristics is developed to predict the conditions for densification and distortion onset. The microstructure is also correlated with the magnitude of shape loss and viscosity of a semisolid aggregate. A mechanistic model, based on the semisolid rheological characteristics, is developed to predict the magnitude and nature of shape loss. The model shows good correlation with experimental data for bronze. This study offers critical insight into SLPS and provides processing strategies for fabrication of high-density components without shape loss.

Shocked monazite chronometry: integrating microstructural and in situ isotopic age data for determining precise impact ages

NASA Astrophysics Data System (ADS)

Erickson, Timmons M.; Timms, Nicholas E.; Kirkland, Christopher L.; Tohver, Eric; Cavosie, Aaron J.; Pearce, Mark A.; Reddy, Steven M.

2017-03-01

Monazite is a robust geochronometer and occurs in a wide range of rock types. Monazite also records shock deformation from meteorite impact but the effects of impact-related microstructures on the U-Th-Pb systematics remain poorly constrained. We have, therefore, analyzed shock-deformed monazite grains from the central uplift of the Vredefort impact structure, South Africa, and impact melt from the Araguainha impact structure, Brazil, using electron backscatter diffraction, electron microprobe elemental mapping, and secondary ion mass spectrometry (SIMS). Crystallographic orientation mapping of monazite grains from both impact structures reveals a similar combination of crystal-plastic deformation features, including shock twins, planar deformation bands and neoblasts. Shock twins were documented in up to four different orientations within individual monazite grains, occurring as compound and/or type one twins in (001), (100), ( 10bar{1} ), {110}, { 212 }, and type two (irrational) twin planes with rational shear directions in [0bar{1}bar{1}] and [bar{1}bar{1}0]. SIMS U-Th-Pb analyses of the plastically deformed parent domains reveal discordant age arrays, where discordance scales with increasing plastic strain. The correlation between discordance and strain is likely a result of the formation of fast diffusion pathways during the shock event. Neoblasts in granular monazite domains are strain-free, having grown during the impact events via consumption of strained parent grains. Neoblastic monazite from the Inlandsee leucogranofels at Vredefort records a 207Pb/206Pb age of 2010 ± 15 Ma (2 σ, n = 9), consistent with previous impact age estimates of 2020 Ma. Neoblastic monazite from Araguainha impact melt yield a Concordia age of 259 ± 5 Ma (2 σ, n = 7), which is consistent with previous impact age estimates of 255 ± 3 Ma. Our results demonstrate that targeting discrete microstructural domains in shocked monazite, as identified through orientation mapping, for in situ U-Th-Pb analysis can date impact-related deformation. Monazite is, therefore, one of the few high-temperature geochronometers that can be used for accurate and precise dating of meteorite impacts.

Review on Microstructure Analysis of Metals and Alloys Using Image Analysis Techniques

NASA Astrophysics Data System (ADS)

Rekha, Suganthini; Bupesh Raja, V. K.

2017-05-01

The metals and alloys find vast application in engineering and domestic sectors. The mechanical properties of the metals and alloys are influenced by their microstructure. Hence the microstructural investigation is very critical. Traditionally the microstructure is studied using optical microscope with suitable metallurgical preparation. The past few decades the computers are applied in the capture and analysis of the optical micrographs. The advent of computer softwares like digital image processing and computer vision technologies are a boon to the analysis of the microstructure. In this paper the literature study of the various developments in the microstructural analysis, is done. The conventional optical microscope is complemented by the use of Scanning Electron Microscope (SEM) and other high end equipments.

User-independent EBSD parameters to study the progress of recovery and recrystallization in Cu-Zn alloy during in situ heating.

PubMed

Sharma, N K; Shekhar, S

2016-12-01

Microstructural evolution of cold-rolled Cu-5%Zn alloy during in situ heating inside field-emission scanning electron microscope was utilized to obtain user-independent parameters in order to trace the progress of static recovery and recrystallization. Electron back-scattered diffraction (EBSD)-based orientation imaging microscopy was used to obtain micrographs at various stages of in situ heating. It is shown that unlike the pre-existing methods, additional EBSD-based parameter can be used to trace the progress of recovery and recrystallization, which is not dependent on user input and hence less prone to error. True strain of 0.3 was imposed during cold rolling of alloy sample. Rolled sample was subjected to in situ heating from room temperature to 500°C (∼0.58 Tm) with soaking time of 10 min, at each of the intermediate temperatures viz. 100, 200, 300, 400 and 450°C. After reaching 500°C, the sample was kept at this temperature for a maximum duration of around 15 h. The sample showed clear signs of recovery for temperature up to 450°C, and at 500°C, recrystallization started to take place. Recrystallization kinetics was moderate, and full recrystallization was achieved in approximately 120 min. We found that EBSD parameter, namely, band contrast intensity can be used as an extra handle to map out the progress of recrystallization occurring in the sample. By contrast, mean angular deviation can be used to understand the evolution of recovery in samples. The parameters mentioned in the current study, unlike other pre-existing methods, can also be used for mapping local microstructural transformations due to recovery and recrystallization. We discuss the benefits and limitations in using these additional handles in understanding the changes taking place in the material during in situ heating. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

Microstructure and conductivity of in-situ polymerized poly(3,4-ethylenedioxythiophene) (PEDOT) crystals

NASA Astrophysics Data System (ADS)

Liu, Jinglin; Ouyang, Liangqi; Wu, Jinghang; Kuo, Chin-Chen; Wei, Bin; Martin, David

2013-03-01

Conjugated polymers are widely used in organic solar cells, biomedical devices, and chemical sensors. Both chemical and electrochemical methods have been developed for preparing conducting polymers, but the extent of crystalline order is usually modest. Here we synthesized highly-ordered brominated (3,4-ethylenedioxythiophene) (EDOT-Br) monomer crystals via electrochemical methods. The kinetics of the synthesis was studied with a Quartz Crystal Microbalance (QCM) and Cyclic Voltammetry (CV). The chemical structure of the EDOT-Br monomer has been confirmed by Nuclear Magnetic Resonance (NMR), Ultraviolet-Visible Spectroscopy (UV-Vis), Fourier Transform Infrared Spectroscopy (FTIR), and Mass Spectrometry (MS). The EDOT-Br monomer crystals can be in-situ polymerized into highly ordered PEDOT conjugated polymer crystals by annealing at temperatures below the EDOT-Br melting point. The crystalline structure was studied by optical microscopy, electron microscopy and X-Ray analysis. The conductivity and electrochemical properties of both the EDOT-Br monomer and corresponding PEDOT polymer crystals were examined with electrochemical impedance spectroscopy (EIS) and CV. This work was supported by NSF, DMR- 1103027.

In situ TEM study of electron-beam radiation induced boron diffusion and effects on phase and microstructure evolution in nanostructured CoFeB/SiO2 thin film

NASA Astrophysics Data System (ADS)

Liu, B. H.; Teo, H. W.; Mo, Z. H.; Mai, Z. H.; Lam, J.; Xue, J. M.; Zhao, Y. Z.; Tan, P. K.

2017-01-01

Using in situ transmission electron microscopy (TEM), we studied boron diffusion and segregation in CoFeB/SiO2 nanostructured thin film stacks. We also investigated how these phenomena affected the phase and microstructure of CoFeB thin films under electron beam irradiation at 300 kV. A unique phase transformation was observed in CoFeB thin films under high-dose electron irradiation, from a polycrystalline Co3Fe to a unilateral amorphous phase of Co3Fe and nanocrystalline FexCo23-xB6. The unilateral amorphization of the Co3Fe film showed an electron-dose-rate sensitivity with a threshold dose rate. Detailed in situ TEM studies revealed that the unilateral amorphization of the Co3Fe film arose from boron segregation at the bottom of the Co3Fe thin film induced by radiation-enhanced diffusion of boron atoms that were displaced by electron knock-on effects. The radiation-induced nanocrystallization of FexCo23-xB6 was also found to be dose-rate sensitive with a higher electron beam current leading to earlier nucleation and more rapid grain growth. The nanocrystallization of FexCo23-xB6 occurred preferentially at the CoFeB/SiO2 interface. Kinetic studies by in situ TEM revealed the surface crystallization and diffusion-controlled nucleation and grain growth mechanisms. The radiation-enhanced atomic diffusivity and high-concentration of radiation-induced point defects at the Co3Fe/SiO2 interface enhanced the local short-range ordering of Fe, Co, and B atoms, favoring nucleation and grain growth of FexCo23-xB6 at the interface.

Recent Developments in Ultra High Temperature Ceramics at NASA Ames

NASA Technical Reports Server (NTRS)

Johnson, Sylvia M.; Gasch, Matt; Lawson, John W.; Gusman, Michael I.; Stackpole, Margaret M.

2009-01-01

NASA Ames is pursuing a variety of approaches to modify and control the microstructure of UHTCs with the goal of improving fracture toughness, oxidation resistance and controlling thermal conductivity. The overall goal is to produce materials that can perform reliably as sharp leading edges or nose tips in hypersonic reentry vehicles. Processing approaches include the use of preceramic polymers as the SiC source (as opposed to powder techniques), the addition of third phases to control grain growth and oxidation, and the use of processing techniques to produce high purity materials. Both hot pressing and field assisted sintering have been used to make UHTCs. Characterization of the mechanical and thermal properties of these materials is ongoing, as is arcjet testing to evaluate performance under simulated reentry conditions. The preceramic polymer approach has generated a microstructure in which elongated SiC grains grow in the form of an in-situ composite. This microstructure has the advantage of improving fracture toughness while potentially improving oxidation resistance by reducing the amount and interconnectivity of SiC in the material. Addition of third phases, such as Ir, results in a very fine-grained microstructure, even in hot-pressed samples. The results of processing and compositional changes on microstructure and properties are reported, along with selected arcjet results.

Growth of carbon nanotubes in arc plasma treated graphite disc: microstructural characterization and electrical conductivity study

NASA Astrophysics Data System (ADS)

Nayak, B. B.; Sahu, R. K.; Dash, T.; Pradhan, S.

2018-03-01

Circular graphite discs were treated in arc plasma by varying arcing time. Analysis of the plasma treated discs by field emission scanning electron microscope revealed globular grain morphologies on the surfaces, but when the same were observed at higher magnification and higher resolution under transmission electron microscope, growth of multiwall carbon nanotubes of around 2 nm diameter was clearly seen. In situ growth of carbon nanotube bundles/bunches consisting of around 0.7 nm tube diameter was marked in the case of 6 min treated disc surface. Both the untreated and the plasma treated graphite discs were characterized by X-ray diffraction, energy dispersive spectra of X-ray, X-ray photoelectron spectroscopy, transmission electron microscopy, micro Raman spectroscopy and BET surface area measurement. From Raman spectra, BET surface area and microstructure observed in transmission electron microscope, growth of several layers of graphene was identified. Four-point probe measurements for electrical resistivity/conductivity of the graphite discs treated under different plasma conditions showed significant increase in conductivity values over that of untreated graphite conductivity value and the best result, i.e., around eightfold increase in conductivity, was observed in the case of 6 min plasma treated sample exhibiting carbon nanotube bundles/bunches grown on disc surface. By comparing the microstructures of the untreated and plasma treated graphite discs, the electrical conductivity increase in graphite disc is attributed to carbon nanotubes (including bundles/bunches) growth on disc surface by plasma treatment.

Osteoblast Cell Response on the Ti6Al4V Alloy Heat-Treated

PubMed Central

Chávez-Díaz, Mercedes Paulina; Escudero-Rincón, María Lorenza; Arce-Estrada, Elsa Miriam; Cabrera-Sierra, Román

2017-01-01

In an effort to examine the effect of the microstructural changes of the Ti6Al4V alloy, two heat treatments were carried out below (Ti6Al4V800) and above (Ti6Al4V1050) its β-phase transformation temperature. After each treatment, globular and lamellar microstructures were obtained. Saos-2 pre-osteoblast human osteosarcoma cells were seeded onto Ti6Al4V alloy disks and immersed in cell culture for 7 days. Electrochemical assays in situ were performed using OCP and EIS measurements. Impedance data show a passive behavior for the three Ti6Al4V alloys; additionally, enhanced impedance values were recorded for Ti6Al4V800 and Ti6Al4V1050 alloys. This passive behavior in culture medium is mostly due to the formation of TiO2 during their sterilization. Biocompatibility and cell adhesion were characterized using the SEM technique; Ti6Al4V as received and Ti6Al4V800 alloys exhibited polygonal and elongated morphology, whereas Ti6Al4V1050 alloy displayed a spherical morphology. Ti and O elements were identified by EDX analysis due to the TiO2 and signals of C, N and O, related to the formation of organic compounds from extracellular matrix. These results suggest that cell adhesion is more likely to occur on TiO2 formed in discrete α-phase regions (hcp) depending on its microstructure (grains). PMID:28772804

Center for Cement Composite Materials

DTIC Science & Technology

1990-01-31

metal-oxygen structures G. Kordas MSE-Ceramics Electron paramagnetic resonance W. M. Kriven MSE-Ceramics Electron microscopy Microstructural...SPONSORING iSb. OFFICE SYMBOL 9. PROWIREMENT INSTRUMENT IDENTIFICATION NUMBER ORGANIZATION (If applicable) C S(2is _ _ _- r_,__’ Contract F49620-87-C...novel in-situ technique involving nuclear magnetic resonance . Fiber- matrix interactions in MDF laminates were also studied. Characterization of DSP

Support for the Armor Ceramics symposium at the 40th International Conference on Advanced Ceramics and Composites

DTIC Science & Technology

2016-05-09

WW-P069-2016. In situ HT -ESEM study of MO2 (M=Ce, Th, U) microspheres sintering: From neck elaboration to microstructure design G.I. Nkou Bouala...PERCENT_SUPPORTEDNAME FTE Equivalent: Total Number: Sub Contractors (DD882) Names of Faculty Supported Names of Under Graduate students supported Names of

XPS and biocompatibility studies of titania film on anodized NiTi shape memory alloy.

PubMed

Chu, C L; Wang, R M; Hu, T; Yin, L H; Pu, Y P; Lin, P H; Dong, Y S; Guo, C; Chung, C Y; Yeung, K W K; Chu, Paul K

2009-01-01

A dense titania film is fabricated in situ on NiTi shape memory alloy (SMA) by anodic oxidation in a Na(2)SO(4) electrolyte. The microstructure of the titania film and its influence on the biocompatibility of NiTi SMA are investigated by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), inductively coupled plasma mass spectrometry (ICPMS), hemolysis analysis, and platelet adhesion test. The results indicate that the titania film has a Ni-free zone near the surface and can effectively block the release of harmful Ni ions from the NiTi substrate in simulated body fluids. Moreover, the wettability, hemolysis resistance, and thromboresistance of the NiTi sample are improved by this anodic oxidation method.

Dynamic 3D strain measurements with embedded micro-structured optical fiber Bragg grating sensors during impact on a CFRP coupon

NASA Astrophysics Data System (ADS)

Goossens, Sidney; Geernaert, Thomas; De Pauw, Ben; Lamberti, Alfredo; Vanlanduit, Steve; Luyckx, Geert; Chiesura, Gabriele; Thienpont, Hugo; Berghmans, Francis

2017-04-01

Composite materials are increasingly used in aerospace applications, owing to their high strength-to-mass ratio. Such materials are nevertheless vulnerable to impact damage. It is therefore important to investigate the effects of impacts on composites. Here we embed specialty microstructured optical fiber Bragg grating based sensors inside a carbon fiber reinforced polymer, providing access to the 3D strain evolution within the composite during impact. We measured a maximum strain of -655 μɛ along the direction of impact, and substantially lower values in the two in-plane directions. Such in-situ characterization can trigger insight in the development of impact damage in composites.

Microstructural Aspects of Localized Corrosion Behavior of Mg Alloys

NASA Astrophysics Data System (ADS)

Chu, Peng-Wei

Combining high specific strength and unique electrochemical properties, magnesium (Mg) alloys are promising lightweight materials for various applications from automotive, consumer electronics, biomedical body implant, to battery electrodes. Engineering solutions such as coatings have enabled the use of Mg alloys, despite their intrinsic low corrosion resistance. Consequently, the fundamental mechanisms responsible for the unique localized corrosion behavior of bare Mg alloys, the associated abnormal hydrogen evolution response, and the relationships between corrosion behavior and alloy microstructure are still unsolved. This thesis aims to uncover the specificities of Mg corrosion and the roles of alloy chemistry and microstructure. To this end, multiscale site-specific microstructure characterization techniques, including in situ optical microscopy, scanning electron microscopy with focused ion beam milling, and transmission electron microscopy, combined with electrochemical analysis and hydrogen evolution rate monitoring, were performed on pure Mg and selected Mg alloys under free corrosion and anodic polarization, revealing key new information on the propagation mode of localized corrosion and the role of alloy microstructures, thereby confirming or disproving the validity of previously proposed corrosion models. Uniform surface corrosion film on Mg alloys immersed in NaCl solution consisted a bi-layered structure, with a porous Mg(OH)2 outer layer on top of a MgO inner layer. Presence of fine scale precipitates in Mg alloys interacted with the corrosion reaction front, reducing the corrosion rate and surface corrosion film thickness. Protruding hemispherical dome-like corrosion products, accompanied by growing hydrogen bubbles, formed on top of the impurity particles in Mg alloys by deposition of Mg(OH)2 via a microgalvanic effect. Localized corrosion on Mg alloys under both free immersion and anodic polarization was found to be governed by a common mechanism, with the corrosion front propagating laterally a few mum inside the alloy and underneath the surface corrosion film, with finger-like features aligned with (0001) Mg basal planes at the localized corrosion/alloy interface. Rising streams of hydrogen bubbles were found to follow the anodic dissolution of Mg and formation of Mg(OH)2 corrosion products at the propagating localized corrosion fronts. Alloying elements segregation to the grain boundaries showed the ability to stop localized corrosion propagation momentarily. By revealing the microstructure of corrosion features on Mg alloys, a descriptive model was proposed. Relationships between the corrosion behavior and alloy microstructures were also identified. This microscopic information can serve as a guideline for future development of Mg alloys by tailoring the microstructure to achieve proper corrosion responses for applications under different environments.

Realistic micromechanical modeling and simulation of two-phase heterogeneous materials

NASA Astrophysics Data System (ADS)

Sreeranganathan, Arun

This dissertation research focuses on micromechanical modeling and simulations of two-phase heterogeneous materials exhibiting anisotropic and non-uniform microstructures with long-range spatial correlations. Completed work involves development of methodologies for realistic micromechanical analyses of materials using a combination of stereological techniques, two- and three-dimensional digital image processing, and finite element based modeling tools. The methodologies are developed via its applications to two technologically important material systems, namely, discontinuously reinforced aluminum composites containing silicon carbide particles as reinforcement, and boron modified titanium alloys containing in situ formed titanium boride whiskers. Microstructural attributes such as the shape, size, volume fraction, and spatial distribution of the reinforcement phase in these materials were incorporated in the models without any simplifying assumptions. Instrumented indentation was used to determine the constitutive properties of individual microstructural phases. Micromechanical analyses were performed using realistic 2D and 3D models and the results were compared with experimental data. Results indicated that 2D models fail to capture the deformation behavior of these materials and 3D analyses are required for realistic simulations. The effect of clustering of silicon carbide particles and associated porosity on the mechanical response of discontinuously reinforced aluminum composites was investigated using 3D models. Parametric studies were carried out using computer simulated microstructures incorporating realistic microstructural attributes. The intrinsic merit of this research is the development and integration of the required enabling techniques and methodologies for representation, modeling, and simulations of complex geometry of microstructures in two- and three-dimensional space facilitating better understanding of the effects of microstructural geometry on the mechanical behavior of materials.

Stability of surface plastic flow in large strain deformation of metals

NASA Astrophysics Data System (ADS)

Viswanathan, Koushik; Udapa, Anirduh; Sagapuram, Dinakar; Mann, James; Chandrasekar, Srinivasan

We examine large-strain unconstrained simple shear deformation in metals using a model two-dimensional cutting system and high-speed in situ imaging. The nature of the deformation mode is shown to be a function of the initial microstructure state of the metal and the deformation geometry. For annealed metals, which exhibit large ductility and strain hardening capacity, the commonly assumed laminar flow mode is inherently unstable. Instead, the imposed shear is accommodated by a highly rotational flow-sinuous flow-with vortex-like components and large-amplitude folding on the mesoscale. Sinuous flow is triggered by a plastic instability on the material surface ahead of the primary region of shear. On the other hand, when the material is extensively strain-hardened prior to shear, laminar flow again becomes unstable giving way to shear banding. The existence of these flow modes is established by stability analysis of laminar flow. The role of the initial microstructure state in determining the change in stability from laminar to sinuous / shear-banded flows in metals is elucidated. The implications for cutting, forming and wear processes for metals, and to surface plasticity phenomena such as mechanochemical Rehbinder effects are discussed.

In situ elaboration of a binary Ti-26Nb alloy by selective laser melting of elemental titanium and niobium mixed powders.

PubMed

Fischer, M; Joguet, D; Robin, G; Peltier, L; Laheurte, P

2016-05-01

Ti-Nb alloys are excellent candidates for biomedical applications such as implantology and joint replacement because of their very low elastic modulus, their excellent biocompatibility and their high strength. A low elastic modulus, close to that of the cortical bone minimizes the stress shielding effect that appears subsequent to the insertion of an implant. The objective of this study is to investigate the microstructural and mechanical properties of a Ti-Nb alloy elaborated by selective laser melting on powder bed of a mixture of Ti and Nb elemental powders (26 at.%). The influence of operating parameters on porosity of manufactured samples and on efficacy of dissolving Nb particles in Ti was studied. The results obtained by optical microscopy, SEM analysis and X-ray microtomography show that the laser energy has a significant effect on the compactness and homogeneity of the manufactured parts. Homogeneous and compact samples were obtained for high energy levels. Microstructure of these samples has been further characterized. Their mechanical properties were assessed by ultrasonic measures and the Young's modulus found is close to that of classically elaborated Ti-26 Nbingot. Copyright © 2016 Elsevier B.V. All rights reserved.

Structure deformation of indium oxide from nanoparticles into nanostructured polycrystalline films by in situ thermal radiation treatment

PubMed Central

2013-01-01

A microstructure deformation of indium oxide (In2O3) nanoparticles by an in situ thermal radiation treatment in nitrous oxide plasma was investigated. The In2O3 nanoparticles were completely transformed into nanostructured In2O3 films upon 10 min of treatment time. The treated In2O3 nanoparticle sample showed improvement in crystallinity while maintaining a large surface area of nanostructure morphology. The direct transition optical absorption at higher photon energy and the electrical conductivity of the In2O3 nanoparticles were significantly enhanced by the treatment. PMID:24134646

Al-TiC composites in situ-processed by ingot metallurgy and rapid solidification technology. Part 2: Mechanical behavior

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

Tong, X.C.; Fang, H.S.

1998-03-01

In Part 2 of this article, the high-strength Al-Si/TiC composite and the elevated-temperature-resistant Al-Fe(-V-Si)/TiC composite, developed on the basis of the in situ Al-TiC composites (Part 1 of the article), have been evaluated for their room- and elevated-temperature mechanical behavior. The microstructural characteristics of ingot metallurgy (IM) or rapid solidification (RS) Al-Si/TiC and Al-Fe(-V-Si)/TiC composites could be thought of as a combination of the related alloy matrix microstructures and the IM or RS Al/TiC composites. The IM Al/TiC and the Al-Si/TiC composites show superior strength and ductility to the relevant aluminum-based composites. The RS Al/TiC and the Al-Fe-V-Si/TiC exhibit highmore » Young`s moduli and substantial improvements in room- and elevated-temperature tensile properties compared to those of rapidly solidified alloys and conventional composites. The Young`s modulus values of RS Al/TiC and Al-Fe-V-Si/TiC composites are well within Hashin-Shtrikman (H-S) limits, in keeping with the strong interfacial bonding. In the micromechanics approach, the principal strengthening mechanisms for the present dispersed, particle-hardened RS in situ Al-TiC composites would include Orowan strengthening, grain-size and substructure strengthening, and solid-solution strengthening.« less

Carbon spheres-assisted strategy to prepare mesoporous manganese dioxide for supercapacitor applications

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

Li Siheng; Graduate University of Chinese Academy of Sciences, Beijing 100039; Qi Li, E-mail: qil@ciac.jl.cn

Mesoporous MnO{sub 2} microstructures with large specific surface area have been successfully synthesized by an in-situ redox precipitation method in the presence of colloidal carbon spheres. The samples of them had much higher specific surface area, pore size and pore volume than those obtained via routes without carbon spheres. The morphology, chemical compositions and porous nature of products were fully characterized. Electrochemical measurements showed that these mesoporous MnO{sub 2} could function well when used as positive electrode materials for supercapacitor. Ideal electrochemical capacitive performances and cyclic stability after 2000 galvanostatic charge-discharge cycles could be observed in 1 M neutral Na{submore » 2}SO{sub 4} aqueous electrolyte with a working voltage of 1.7 V. - Graphical Abstract: Mesoporous MnO{sub 2} microstructures with large S{sub BET} were successfully synthesized by in-situ redox precipitation method in the presence of colloidal carbon spheres. Electrochemical measurements showed that these mesoporous MnO{sub 2} could be well used as electrode materials for supercapacitor. Highlights: Black-Right-Pointing-Pointer Mesoporous MnO{sub 2} was prepared by in-situ redox method assisted by carbon spheres. Black-Right-Pointing-Pointer S{sub BET}, pore size and volume were higher than MnO{sub 2} obtained without carbon spheres. Black-Right-Pointing-Pointer They could function well when used as electrode materials for supercapacitor. Black-Right-Pointing-Pointer Ideal capacitive behaviors and long cycling life showed after 2000 charge-discharge.« less

A Novel Method for In Situ Electromechanical Characterization of Nanoscale Specimens

PubMed Central

Reid, Russell C.; Piqué, Alberto; Kang, Wonmo

2017-01-01

Electrically assisted deformation (EAD) is increasingly being used to improve the formability of metals during processes such as sheet metal rolling and forging. Adoption of this technique is proceeding despite disagreement concerning the underlying mechanism responsible for EAD. The experimental procedure described herein enables a more explicit study compared to previous EAD research by removing thermal effects, which are responsible for disagreement in interpreting previous EAD results. Furthermore, as the procedure described here enables EAD observation in situ and in real time in a transmission electron microscope (TEM), it is superior to existing post-mortem methods that observe EAD effects post-test. Test samples consist of a single crystal copper (SCC) foil having a free-standing tensile test section of nanoscale thickness, fabricated using a combination of laser and ion beam milling. The SCC is mounted to an etched silicon base that provides mechanical support and electrical isolation while serving as a heat sink. Using this geometry, even at high current density (~3,500 A/mm2), the test section experiences a negligible temperature increase (<0.02 °C), thus eliminating Joule heating effects. Monitoring material deformation and identifying the corresponding changes to microstructures, e.g. dislocations, are accomplished by acquiring and analyzing a series of TEM images. Our sample preparation and in situ experiment procedures are robust and versatile as they can be readily utilized to test materials with different microstructures, e.g., single and polycrystalline copper. PMID:28605394

TEM in situ micropillar compression tests of ion irradiated oxide dispersion strengthened alloy

NASA Astrophysics Data System (ADS)

Yano, K. H.; Swenson, M. J.; Wu, Y.; Wharry, J. P.

2017-01-01

The growing role of charged particle irradiation in the evaluation of nuclear reactor candidate materials requires the development of novel methods to assess mechanical properties in near-surface irradiation damage layers just a few micrometers thick. In situ transmission electron microscopic (TEM) mechanical testing is one such promising method. In this work, microcompression pillars are fabricated from a Fe2+ ion irradiated bulk specimen of a model Fe-9%Cr oxide dispersion strengthened (ODS) alloy. Yield strengths measured directly from TEM in situ compression tests are within expected values, and are consistent with predictions based on the irradiated microstructure. Measured elastic modulus values, once adjusted for the amount of deformation and deflection in the base material, are also within the expected range. A pillar size effect is only observed in samples with minimum dimension ≤100 nm due to the low inter-obstacle spacing in the as received and irradiated material. TEM in situ micropillar compression tests hold great promise for quantitatively determining mechanical properties of shallow ion-irradiated layers.

[Laser Raman Spectroscopy and Its Application in Gas Hydrate Studies].

PubMed

Fu, Juan; Wu, Neng-you; Lu, Hai-long; Wu, Dai-dai; Su, Qiu-cheng

2015-11-01

Gas hydrates are important potential energy resources. Microstructural characterization of gas hydrate can provide information to study the mechanism of gas hydrate formation and to support the exploitation and application of gas hydrate technology. This article systemly introduces the basic principle of laser Raman spectroscopy and summarizes its application in gas hydrate studies. Based on Raman results, not only can the information about gas composition and structural type be deduced, but also the occupancies of large and small cages and even hydration number can be calculated from the relative intensities of Raman peaks. By using the in-situ analytical technology, laser Raman specstropy can be applied to characterize the formation and decomposition processes of gas hydrate at microscale, for example the enclathration and leaving of gas molecules into/from its cages, to monitor the changes in gas concentration and gas solubility during hydrate formation and decomposition, and to identify phase changes in the study system. Laser Raman in-situ analytical technology has also been used in determination of hydrate structure and understanding its changing process under the conditions of ultra high pressure. Deep-sea in-situ Raman spectrometer can be employed for the in-situ analysis of the structures of natural gas hydrate and their formation environment. Raman imaging technology can be applied to specify the characteristics of crystallization and gas distribution over hydrate surface. With the development of laser Raman technology and its combination with other instruments, it will become more powerful and play a more significant role in the microscopic study of gas hydrate.

Advances and Achievements in In Situ Analysis of Corrosion and Structure–Property Relationship in Mg Alloys

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

Orlov, D.; Joshi, V.

Every year, TMS Magnesium Committee carefully selects a special topic in magnesium (Mg) related research and development not only having the hottest subject from both academic and industrial perspectives but also demonstrating major achievements within this subject. Following last year’s topic on Mg microallying [1], this year’s focus is on in-situ methods and associated techniques in their broad definition spanning from laboratory- to large- scale facilities to process monitoring. The applications of in-situ techniques have a wide spectrum from the analysis of melts and liquid-solid transitions to solid-state phenomena during thermo-mechanical processing and heat treatments to surface interactions with variousmore » environments. Therefore, such works are of significant interest to scientists working in the area of Mg alloy development as well as to a much broader audience from both academia and industry. This interest is primarily caused by challenges in the analysis of structure-property relationship in Mg alloys, and even cursory glance of literature reveals sharp increase of publications relevant to this topic recently. For instance, very high reactivity of Mg as well as its well-known propensity to substantially alter structure upon unloading in mechanical testing makes it difficult to understand and thus to simulate correlation between microstructures observed in post-mortem analysis and physical processes during testing or fabrication. However, recent advances in in-situ analysis based on large-scale research facilities such as neutron scattering and synchrotron radiation sources as well as microscopy-based, acoustic emission, and other more traditional techniques allowed significant achievements. Apart from apparent development of relevant experimental techniques, a significant part of this success should also be attributed to increasing accessibility of the facilities and simplification of their use from a user perspective. The selection of articles in this special topic is quite far from comprehensive review covering all aspects of in-situ methods available for metallic materials development. However, this was not the purpose in any case. Instead, this selection is intended to present several studies on Mg alloys and Mg-based composites with the use of in-situ techniques. In addition, it overviews two techniques, ‘Acoustic Emission’ (AE) and ‘Ambient-Pressure X-ray Photoelectron Spectroscopy’ (AP-XPS), that are rather novel to the Mg community. These studies are supposed to give readers representative examples of such techniques potential and to help in navigating the spectrum of modern state-of-the-art analytical methods facilitating the development of Mg alloys. These articles are organized in the order corresponding to typical Mg alloy lifecycle from material preparation and solidification to thermo-mechanical processing and product fabrication to degradation.« less

Crystal structure and texture changes during thermal cycling of TATB

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

Vogel, Sven C.; Yeager, John David

2015-02-20

Goals: Understand crystal structure and micro-structure changes during thermal cycling, understand reasons for ratcheting of TATB during thermal cycling, and Support of B61 LEP. Deliverables achieved: Completed in situ thermal cycling of loose powder and pressed pellet TATB on HIPPO, Quantified preferred orientation of pressed pellet, and quantified relative change of each of the six lattic parameters.

Bacterial Paleontology and Studies of Carbonaceous Chondrites

NASA Technical Reports Server (NTRS)

Gerasimenko, L. M.; Hoover, Richard B.; Rozanov, Alexei Y.; Zhegallo, E. A.; Zhmur, S. I.

1999-01-01

The study of the fossilization processes of modern cyanobacteria provides insights needed to recognize bacterial microfossils. The fossilization of cyanobacteria is discussed and images of recent and fossil bacteria and cyanobacteria from the Early Proterozoic to Neogene carbonaceous rocks (kerites, shungites, and black shales) and phosphorites are provided. These are compared with biomorphic microstructures and possible microfossils encountered in-situ in carbonaceous meteorites.

Development of ultrafine Ti-Fe-Sn in-situ composite with enhanced plasticity

NASA Astrophysics Data System (ADS)

Mondal, B.; Samal, S.; Biswas, K.; Govind

2012-01-01

The present investigation is aimed at developing ultrafine eutectic/dendrite Ti-Fe-Sn in-situ composite with balanced combination of strength and plasticity. It also studies the microstructure evolution in the series of hypereutectic Ti-Fe-Sn ternary alloys. Sn concentration of these alloys has been varied from 0 - 10 atom% in the binary alloy (Ti71Fe29) keeping the Ti concentration fixed. These alloys have been prepared by arc melting under an Ar atmosphere on a water-cooled Cu hearth, which are subsequently suction cast in a split Cu-mold under an Ar atmosphere. Detailed X-ray diffraction (XRD) study shows the presence of TiFe, β-Ti, and Ti3Sn phases. The SEM micrographs reveal that the microstructures consist of fine scale eutectic matrix (β-Ti and TiFe) with primary dendrite phases (TiFe and/or Ti3Sn) depending on concentration of Sn. α -Ti forms as a eutectoid reaction product of β-Ti. The room temperature uniaxial compressive test reveals simultaneous improvement in the strength (1942 MPa) and plasticity (13.1 %) for Ti71Fe26Sn3 ternary alloy. The fracture surface indicates a ductile mode of fracture for the alloy.

Fabrication of the Ti5Si3/Ti composite inoculants and its refining mechanism on pure titanium

NASA Astrophysics Data System (ADS)

Li, Nuo; Cui, Chunxiang; Liu, Shaungjin; Zhao, Long; Liu, Shuiqing

2017-03-01

The in situ Ti5Si3/Ti inoculants were successfully prepared by vacuum arc-melting and melt-spinning method. An efficient route by adding a small quantity of Ti5Si3/Ti inoculants to Ti melt has been first proposed to modify the coarse grains of as cast microstructure of pure titanium in this paper. It was found that the microstructure of ribbon inoculants was cellular structure that composed of Ti5Si3 and α-Ti phases. The grain refining effect of the inoculants was significantly improved with the adding ratio range from 0.2% to 0.5% in weight. With the increase of addition amount of inoculants on Ti melt, the tensile strength, yield strength and microhardness of pure titanium are significantly improved except elongation. The excellent grain refining effect can be attributed to the heterogeneous nucleation of the titanium grain on the precipitated Ti5Si3 phases in the Si-rich regions and the constitutional supercooling of Si in the Si-poverty regions. It is suggested that the in situ Ti5Si3/Ti inoculants is a promising inoculants for titanium alloys.

Novel symmetrical coralloid Cu 3D superstructures: Solid-state synthesis from a Cu-carboxylate MOF and their in-situ thermal conversion

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

Chen Lingyun, E-mail: lychen@cqu.edu.c; Shen Yongming; Bai Junfeng, E-mail: bjunfeng@nju.edu.c

2009-08-15

We describe here a one-step solid-state process for the synthesis of metal three-dimensional (3D) superstructures from a metal-organic framework (MOF). Novel symmetrical coralloid Cu 3D superstructures with surface interspersed with clusters of Cu nanoparticles were successfully synthesized by thermolysis of the [Cu{sub 3}(btc){sub 2}] (btc=benzene-1,3,5-tricarboxylato) MOF in a one-end closed horizontal tube furnace (OCTF). The obtained products were characterized by TGA, FT-IR, XRD, EDX, SEM, TEM, HRTEM and SAED. Different reaction conditions were discussed. Furthermore, the synthesized Cu samples were converted into CuO microstructures by in-situ calcination in the air. In addition, the possible formation mechanism was also proposed. Thismore » method is a simple and facile route, which builds a direct linkage between metal-carboxylate MOF crystals and metal nano- or microstructures and also opens a new application field of MOFs. - Graphical abstract: Novel symmetrical coralloid Cu 3D superstructures were synthesized by thermolysis of the [Cu{sub 3}(btc){sub 2}] (btc=benzene-1,3,5-tricarboxylato) MOF microcrystals in a one-end closed horizontal tube furnace (OCTF).« less

Effects of plastic deformation on microstructure and superplasticity of the in situ Al3Ti/2024Al composites

NASA Astrophysics Data System (ADS)

Jiao, Lei; Yang, Yonggang; Li, Hui; Zhao, Yutao; Wang, Xiaolu

2018-05-01

In this study, the in situ Al3Ti/2024Al composites were successfully fabricated by direct melt reaction method and subjected to forging and friction stir processing (FSP) to achieve superplasticity. Then, the microstructure and superplastic tensile behavior of the composites were investigated. The results show that the reinforcement particles are broken and grains are fine after plastic processing. Particularly, the size of reinforcement particles ranges from 0.2 μm to 5 μm and the average size of fine equiaxed grains is 5 μm after FSP processing. And the superplasticity of the composites was improved apparently. The maximum elongation of 642% was obtained at 0.15 s‑1 and 510 °C for the FSP specimen, with a strain rate sensitive parameter (m) of 0.58, indicating the FSP specimen has obtained excellent high strain rate superplasticity. The strain rate sensitivity parameter, m, ranges from 0.23 to 0.58, and the activation energy was calculated to be 135.24 kJ mol‑1. All results indicated that the main superplastic deformation mechanism was grain boundary sliding (GBS) for the FSP Al3Ti/2024Al composites.

Effect of pulsed laser parameters on in-situ TiC synthesis in laser surface treatment

NASA Astrophysics Data System (ADS)

Hamedi, M. J.; Torkamany, M. J.; Sabbaghzadeh, J.

2011-04-01

Commercial titanium sheets pre-coated with 300-μm thick graphite layer were treated by employing a pulsed Nd:YAG laser in order to enhance surface properties such as wear and erosion resistance. Laser in-situ alloying method produced a composite layer by melting the titanium substrate and dissolution of graphite in the melt pool. Correlations between pulsed laser parameters, microstructure and microhardness of the synthesized composite coatings were investigated. Effects of pulse duration and overlapping factor on the microstructure and hardness of the alloyed layer were deduced from Vickers micro-indentation tests, XRD, SEM and metallographic analyses of cross sections of the generated layer. Results show that the composite cladding layer was constituted with TiC intermetallic phase between the titanium matrix in particle and dendrite forms. The dendritic morphology of composite layer was changed to cellular grain structure by increasing laser pulse duration and irradiated energy. High values of the measured hardness indicate that deposited titanium carbide increases in the conditions with more pulse duration and low process speed. This occurs due to more dissolution of carbon into liquid Ti by heat input increasing and positive influence of the Marangoni flow in the melted zone.

Deformation-Induced Microstructural Banding in TRIP Steels

NASA Astrophysics Data System (ADS)

Celotto, S.; Ghadbeigi, H.; Pinna, C.; Shollock, B. A.; Efthymiadis, P.

2018-05-01

Microstructure inhomogeneities can strongly influence the mechanical properties of advanced high-strength steels in a detrimental manner. This study of a transformation-induced plasticity (TRIP) steel investigates the effect of pre-existing contiguous grain boundary networks (CGBNs) of hard second-phases and shows how these develop into bands during tensile testing using in situ observations in conjunction with digital image correlation (DIC). The bands form by the lateral contraction of the soft ferrite matrix, which rotates and displaces the CGBNs of second-phases and the individual features within them to become aligned with the loading direction. The more extensive pre-existing CGBNs that were before the deformation already aligned with the loading direction are the most critical microstructural feature for damage initiation and propagation. They induce micro-void formation between the hard second-phases along them, which coalesce and develop into long macroscopic fissures. The hard phases, retained austenite and martensite, were not differentiated as it was found that the individual phases do not play a role in the formation of these bands. It is suggested that minimizing the presence of CGBNs of hard second-phases in the initial microstructure will increase the formability.

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

Chen, Aiying; Liu, Jiabin; Wang, Hongtao

Gradient materials often have attractive mechanical properties that outperform uniform microstructure counterparts. It remains a difficult task to investigate and compare the performance of various gradient microstructures due to the difficulty of fabrication, the wide range of length scales involved, and their respective volume percentage variations. We have investigated four types of gradient microstructures in 304 stainless steels that utilize submicrotwins, nanotwins, nanocrystalline-, ultrafine- and coarse-grains as building blocks. Tensile tests reveal that the gradient microstructure consisting of submicrotwins and nanotwins has a persistent and stable work hardening rate and yields an impressive combination of high strength and high ductility,more » leading to a toughness that is nearly 50% higher than that of the coarse-grained counterpart. Ex- and in-situ transmission electron microscopy indicates that nanoscale and submicroscale twins help to suppress and limit martensitic phase transformation via the confinement of martensite within the twin lamellar. Twinning and detwinning remain active during tensile deformation and contribute to the work hardening behavior. We discuss the advantageous properties of using submicrotwins as the main load carrier and nanotwins as the strengthening layers over those coarse and nanocrystalline grains. Furthermore, our work uncovers a new gradient design strategy to help metals and alloys achieve high strength and high ductility.« less

Multi-modal porous microstructure for high temperature fuel cell application

NASA Astrophysics Data System (ADS)

Wejrzanowski, T.; Haj Ibrahim, S.; Cwieka, K.; Loeffler, M.; Milewski, J.; Zschech, E.; Lee, C.-G.

2018-01-01

In this study, the effect of microstructure of porous nickel electrode on the performance of high temperature fuel cell is investigated and presented based on a molten carbonate fuel cell (MCFC) cathode. The cathode materials are fabricated from slurry consisting of nickel powder and polymeric binder/solvent mixture, using the tape casting method. The final pore structure is shaped through modifying the slurry composition - with or without the addition of porogen(s). The manufactured materials are extensively characterized by various techniques involving: micro-computed tomography (micro-XCT), scanning electron microscopy (SEM), mercury porosimetry, BET and Archimedes method. Tomographic images are also analyzed and quantified to reveal the evolution of pore space due to nickel in situ oxidation to NiO, and infiltration by the electrolyte. Single-cell performance tests are carried out under MCFC operation conditions to estimate the performance of the manufactured materials. It is found that the multi-modal microstructure of MCFC cathode results in a significant enhancement of the power density generated by the reference cell. To give greater insight into the understanding of the effect of microstructure on the properties of the cathode, a model based on 3D tomography image transformation is proposed.

Effect of Alloying Elements on Nb-Rich Portion of Nb-Si-X Ternary Systems and In Situ Crack Observation of Nb-Si-Based Alloys

NASA Astrophysics Data System (ADS)

Miura, Seiji; Hatabata, Toru; Okawa, Takuya; Mohri, Tetsuo

2014-03-01

To find a new route for microstructure control and to find additive elements beneficial for improving high-temperature strength, a systematic investigation is performed on hypoeutectic Nb-15 at. pct Si-X ternary alloys containing a transition element, Fe, Co, Ni, Cu, Ru, Rh, Pd, Re, Os, Ir, Pt, or Au. Information on phase equilibrium is classified in terms of phase stability of silicide phases, α Nb5Si3, Nb4SiX, and Nb3Si, and the relationship between microstructure and mechanical properties both at room temperature and high temperature is investigated. All the additive elements are found to stabilize either α Nb5Si3 or Nb4SiX but destabilize Nb3Si. A microstructure of Nbss/α Nb5Si3 alloy composed of spheroidized α Nb5Si3 phase embedded in the Nbss matrix is effective for toughening, regardless of the initial as-cast microstructure. Also the plastic deformation of Nbss dendrites may effectively suppress the propagation of longer cracks. High-temperature strength of alloys is governed by the deformation of Nbss phase and increases with higher melting point additives.

Microstructural evolution and deformation behavior of Al-Cu alloys: A Transmission X-ray Microscopy (TXM) and micropillar compression study

DOE PAGES

Kaira, C. Shashank; Kantzos, Christopher; Williams, Jason J.; ...

2017-11-07

In this paper, a unique approach to correlating an evolving 3D microstructure in an Al-Cu alloy and its micro-scale mechanical properties has been introduced. Using these nanoscale three-dimensional microstructures derived from Transmission X-ray Microscopy (TXM), individual contributions from different strengthening mechanisms were quantified. The spatial distribution and morphology of the individual θ' and θ phases were seen to play an important role in influencing dislocation storage. Uniaxial micro-compression experiments were used to quantify the stress-strain response of the alloy at different aging times. Transmission electron microscopy (TEM) aided in discerning dislocation activity at these precipitates. A model is proposed tomore » accurately predict the variation in yield stress by using appropriate morphological parameters from the 3D microstructure and its validity has been corroborated using experimental measurements. Distributions of 2D and 3D inter-precipitate spacing were seen to provide crucial insights on influencing deformation in such precipitation-strengthened alloys. In conclusion, the transition in deformation behavior and origin of numerous strain bursts were investigated using in situ micropillar compression testing.« less

The Microstructural Evolution and Mechanical Properties of Zr-Based Metallic Glass under Different Strain Rate Compressions

PubMed Central

Chen, Tao-Hsing; Tsai, Chih-Kai

2015-01-01

In this study, the high strain rate deformation behavior and the microstructure evolution of Zr-Cu-Al-Ni metallic glasses under various strain rates were investigated. The influence of strain and strain rate on the mechanical properties and fracture behavior, as well as microstructural properties was also investigated. Before mechanical testing, the structure and thermal stability of the Zr-Cu-Al-Ni metallic glasses were studied with X-ray diffraction (XRD) and differential scanning calorimeter. The mechanical property experiments and microstructural observations of Zr-Cu-Al-Ni metallic glasses under different strain rates ranging from 10−3 to 5.1 × 103 s−1 and at temperatures of 25 °C were investigated using compressive split-Hopkinson bar (SHPB) and an MTS tester. An in situ transmission electron microscope (TEM) nanoindenter was used to carry out compression tests and investigate the deformation behavior arising at nanopillars of the Zr-based metallic glass. The formation and interaction of shear band during the plastic deformation were investigated. Moreover, it was clearly apparent that the mechanical strength and ductility could be enhanced by impeding the penetration of shear bands with reinforced particles. PMID:28788034

Deformation-Induced Microstructural Banding in TRIP Steels

NASA Astrophysics Data System (ADS)

Celotto, S.; Ghadbeigi, H.; Pinna, C.; Shollock, B. A.; Efthymiadis, P.

2018-07-01

Microstructure inhomogeneities can strongly influence the mechanical properties of advanced high-strength steels in a detrimental manner. This study of a transformation-induced plasticity (TRIP) steel investigates the effect of pre-existing contiguous grain boundary networks (CGBNs) of hard second-phases and shows how these develop into bands during tensile testing using in situ observations in conjunction with digital image correlation (DIC). The bands form by the lateral contraction of the soft ferrite matrix, which rotates and displaces the CGBNs of second-phases and the individual features within them to become aligned with the loading direction. The more extensive pre-existing CGBNs that were before the deformation already aligned with the loading direction are the most critical microstructural feature for damage initiation and propagation. They induce micro-void formation between the hard second-phases along them, which coalesce and develop into long macroscopic fissures. The hard phases, retained austenite and martensite, were not differentiated as it was found that the individual phases do not play a role in the formation of these bands. It is suggested that minimizing the presence of CGBNs of hard second-phases in the initial microstructure will increase the formability.

Microstructural evolution and deformation behavior of Al-Cu alloys: A Transmission X-ray Microscopy (TXM) and micropillar compression study

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

Kaira, C. Shashank; Kantzos, Christopher; Williams, Jason J.

In this paper, a unique approach to correlating an evolving 3D microstructure in an Al-Cu alloy and its micro-scale mechanical properties has been introduced. Using these nanoscale three-dimensional microstructures derived from Transmission X-ray Microscopy (TXM), individual contributions from different strengthening mechanisms were quantified. The spatial distribution and morphology of the individual θ' and θ phases were seen to play an important role in influencing dislocation storage. Uniaxial micro-compression experiments were used to quantify the stress-strain response of the alloy at different aging times. Transmission electron microscopy (TEM) aided in discerning dislocation activity at these precipitates. A model is proposed tomore » accurately predict the variation in yield stress by using appropriate morphological parameters from the 3D microstructure and its validity has been corroborated using experimental measurements. Distributions of 2D and 3D inter-precipitate spacing were seen to provide crucial insights on influencing deformation in such precipitation-strengthened alloys. In conclusion, the transition in deformation behavior and origin of numerous strain bursts were investigated using in situ micropillar compression testing.« less

Three-dimensional Optical Coherence Tomography for Optical Biopsy of Lymph Nodes and Assessment of Metastatic Disease

PubMed Central

John, Renu; Adie, Steven G.; Chaney, Eric J.; Marjanovic, Marina; Tangella, Krishnarao V.; Boppart, Stephen A.

2013-01-01

Background Numerous techniques have been developed for localizing lymph nodes before surgical resection and for their histological assessment. Nondestructive high-resolution transcapsule optical imaging of lymph nodes offers the potential for in situ assessment of metastatic involvement, potentially during surgical procedures. Methods Three-dimensional optical coherence tomography (3-D OCT) was used for imaging and assessing resected popliteal lymph nodes from a preclinical rat metastatic tumor model over a 9-day time-course study after tumor induction. The spectral-domain OCT system utilized a center wavelength of 800 nm, provided axial and transverse resolutions of 3 and 12 µm, respectively, and performed imaging at 10,000 axial scans per second. Results OCT is capable of providing high-resolution labelfree images of intact lymph node microstructure based on intrinsic optical scattering properties with penetration depths of ~1–2 mm. The results demonstrate that OCT is capable of differentiating normal, reactive, and metastatic lymph nodes based on microstructural changes. The optical scattering and structural changes revealed by OCT from day 3 to day 9 after the injection of tumor cells into the lymphatic system correlate with inflammatory and immunological changes observed in the capsule, precortical regions, follicles, and germination centers found during histopathology. Conclusions We report for the first time a longitudinal study of 3-D transcapsule OCT imaging of intact lymph nodes demonstrating microstructural changes during metastatic infiltration. These results demonstrate the potential of OCT as a technique for intraoperative, real-time in situ 3-D optical biopsy of lymph nodes for the intraoperative staging of cancer. PMID:22688663

Microfluidic processing of concentrated surfactant mixtures: online SAXS, microscopy and rheology.

PubMed

Martin, Hazel P; Brooks, Nicholas J; Seddon, John M; Luckham, Paul F; Terrill, Nick J; Kowalski, Adam J; Cabral, João T

2016-02-14

We investigate the effect of microfluidic flow on the microstructure and dynamics of a model surfactant mixture, combining synchrotron Small Angle X-ray Scattering (SAXS), microscopy and rheology. A system comprising a single-chain cationic surfactant, hexadecyl trimethyl ammonium chloride (C16TAC), a short-chain alcohol (1-pentanol) and water was selected for the study due to its flow responsiveness and industrial relevance. Model flow fields, including sequential contraction-expansion (extensional) and rotational flows, were investigated and the fluid response in terms of the lamellar d-spacing, orientation and birefringence was monitored in situ, as well as the recovery processes after cessation of flow. Extensional flows are found to result in considerable d-spacing increase (from approx 59 Å to 65 Å). However, under continuous flow, swelling decreases with increasing flow velocity, eventually approaching the equilibrium values at velocities ≃2 cm s(-1). Through individual constrictions we observe the alignment of lamellae along the flow velocity, accompanied by increasing birefringence, followed by an orientation flip whereby lamellae exit perpendicularly to the flow direction. The resulting microstructures are mapped quantitatively onto the flow field in 2D with 200 μm spatial resolution. Rotational flows alone do not result in appreciable changes in lamellar spacing and flow type and magnitude evidently impact the fluid microstructure under flow, as well as upon relaxation. The findings are correlated with rheological properties measured ex situ to provide a mechanistic understanding of the effect of flow imposed by tubular processing units in the phase behavior and performance of a model surfactant system with ubiquitous applications in personal care and coating industries.

Imaging pancreatobiliary ductal system with optical coherence tomography: A review

PubMed Central

Mahmud, Mohammad S; May, Gray R; Kamal, Mohammad M; Khwaja, Ahmed S; Sun, Carry; Vitkin, Alex; Yang, Victor XD

2013-01-01

An accurate, noninvasive and cost-effective method of in situ tissue evaluation during endoscopy would be highly advantageous for the detection of dysplasia or early cancer and for identifying different disease stages. Optical coherence tomography (OCT) is a noninvasive, high-resolution (1-10 μm) emerging optical imaging method with potential for identifying microscopic subsurface features in the pancreatic and biliary ductal system. Tissue microstructure of pancreaticobiliary ductal system has been successfully imaged by inserting an OCT probe through a standard endoscope operative channel. High-resolution OCT images and the technique’s endoscopic compatibility have allowed for the microstructural diagnostic of the pancreatobiliary diseases. In this review, we discussed currently available pancreaticobiliary ductal imaging systems to assess the pancreatobiliary tissue microstructure and to evaluate varieties of pancreaticobiliary disorders and diseases. Results show that OCT can improve the quality of images of pancreatobiliary system during endoscopic retrograde cholangiopancheatography procedure, which may be important in distinguishing between the neoplastic and non-neoplastic lesions. PMID:24255746

Microstructures and properties of ceramic particle-reinforced metal matrix composite layers produced by laser cladding

NASA Astrophysics Data System (ADS)

Zhang, Qingmao; He, Jingjiang; Liu, Wenjin; Zhong, Minlin

2005-01-01

Different weight ratio of titanium, zirconium, WC and Fe-based alloy powders were mixed, and cladded onto a medium carbon steel substrate using a 3kW continuous wave CO2 laser, aiming at producing Ceramic particles- reinforced metal matrix composites (MMCs) layers. The microstructures of the layers are typical hypoeutectic, and the major phases are Ni3Si2, TiSi2, Fe3C, FeNi, MC, Fe7Mo3, Fe3B, γ(residual austenite) and M(martensite). The microstructure morphologies of MMCs layers are dendrites/cells. The MC-type reinforcements are in situ synthesis Carbides which main compositions consist of transition elements Zr, Ti, W. The MC-type particles distributed within dendrite and interdendritic regions with different volume fractions for single and overlapping clad layers. The MMCs layers are dense and free of cracks with a good metallurgical bonding between the layer and substrate. The addition ratio of WC in the mixtures has the remarkable effect on the microhardness of clad layers.

Directional Solidification and Mechanical Properties of NiAl-NiAlTa Alloys

NASA Technical Reports Server (NTRS)

Johnson, D. R.; Chen, X. F.; Oliver, B. F.; Noebe, R. D.; Whittenberger, J. D.

1995-01-01

Directional solidification of eutectic alloys is a promising technique for producing in-situ composite materials exhibiting a balance of properties. Consequently, the microstructure, creep strength and fracture toughness of directionally solidified NiAl-NiAlTa alloys were investigated. Directional solidification was performed by containerless processing techniques to minimize alloy contamination. The eutectic composition was found to be NiAl-15.5 at% Ta and well-aligned microstructures were produced at this composition. A near-eutectic alloy of NiAl-14.5Ta was also investigated. Directional solidification of the near-eutectic composition resulted in microstructures consisting of NiAl dendrites surrounded by aligned eutectic regions. The off-eutectic alloy exhibited promising compressive creep strengths compared to other NiAl-based intermetallics, while preliminary testing indicated that the eutectic alloy was competitive with Ni-base single crystal superalloys. The room temperature toughness of these two-phase alloys was similar to that of polycrystalline NiAl even with the presence of the brittle Laves phase NiAlTa.

Microfluidic devices with permeable polymer barriers for capture and transport of biomolecules and cells.

PubMed

Lee, Ho Suk; Chu, Wai Keung; Zhang, Kun; Huang, Xiaohua

2013-09-07

We report a method for fabricating permeable polymer microstructure barriers in polydimethylsiloxane (PDMS) microfluidic devices and the use of the devices to capture and transport DNA and cells. The polymer microstructure in a desired location in a fluidic channel is formed in situ by the polymerization of acrylamide and polyethylene diacrylate cross-linker (PEG-DA) monomer in a solution which is trapped in the location using a pair of PDMS valves. The porous polymer microstructure provides a mechanical barrier to convective fluid flow in the channel or between two microfluidic chambers while it still conducts ions or small charged species under an electric field, allowing for the rapid capture and transport of biomolecules and cells by electrophoresis. We have demonstrated the application of the devices for the rapid capture and efficient release of bacteriophage λ genomic DNA, solution exchange and for the transport and capture of HeLa cells. Our devices will enable the multi-step processing of biomolecules and cells or individual cells within a single microfluidic chamber.

Interpreting U-Pb data from primary and secondary features in lunar zircon

NASA Astrophysics Data System (ADS)

Grange, M. L.; Pidgeon, R. T.; Nemchin, A. A.; Timms, N. E.; Meyer, C.

2013-01-01

In this paper, we describe primary and secondary microstructures and textural characteristics found in lunar zircon and discuss the relationships between these features and the zircon U-Pb isotopic systems and the significance of these features for understanding lunar processes. Lunar zircons can be classified according to: (i) textural relationships between zircon and surrounding minerals in the host breccias, (ii) the internal microstructures of the zircon grains as identified by optical microscopy, cathodoluminescence (CL) imaging and electron backscattered diffraction (EBSD) mapping and (iii) results of in situ ion microprobe analyses of the Th-U-Pb isotopic systems. Primary zircon can occur as part of a cogenetic mineral assemblage (lithic clast) or as an individual mineral clast and is unzoned, or has sector and/or oscillatory zoning. The age of primary zircon is obtained when multiple ion microprobe analyses across the polished surface of the grain give reproducible and essentially concordant data. A secondary set of microstructures, superimposed on primary zircon, include localised recrystallised domains, localised amorphous domains, crystal-plastic deformation, planar deformation features and fractures, and are associated with impact processes. The first two secondary microstructures often yield internally consistent and close to concordant U-Pb ages that we interpret as dating impact events. Others secondary microstructures such as planar deformation features, crystal-plastic deformation and micro-fractures can provide channels for Pb diffusion and result in partial resetting of the U-Pb isotopic systems.

A 4-D dataset for validation of crystal growth in a complex three-phase material, ice cream

NASA Astrophysics Data System (ADS)

Rockett, P.; Karagadde, S.; Guo, E.; Bent, J.; Hazekamp, J.; Kingsley, M.; Vila-Comamala, J.; Lee, P. D.

2015-06-01

Four dimensional (4D, or 3D plus time) X-ray tomographic imaging of phase changes in materials is quickly becoming an accepted tool for quantifying the development of microstructures to both inform and validate models. However, most of the systems studied have been relatively simple binary compositions with only two phases. In this study we present a quantitative dataset of the phase evolution in a complex three-phase material, ice cream. The microstructure of ice cream is an important parameter in terms of sensorial perception, and therefore quantification and modelling of the evolution of the microstructure with time and temperature is key to understanding its fabrication and storage. The microstructure consists of three phases, air cells, ice crystals, and unfrozen matrix. We perform in situ synchrotron X-ray imaging of ice cream samples using in-line phase contrast tomography, housed within a purpose built cold-stage (-40 to +20oC) with finely controlled variation in specimen temperature. The size and distribution of ice crystals and air cells during programmed temperature cycling are determined using 3D quantification. The microstructural evolution of three-phase materials has many other important applications ranging from biological to structural and functional material, hence this dataset can act as a validation case for numerical investigations on faceted and non-faceted crystal growth in a range of materials.

SCC Initiation Behavior of Alloy 182 in PWR Primary Water

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

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

SCC initiation behavior of 15% cold forged specimens cut from four different alloy 182 weldments was investigated in 360°C simulated PWR primary water under constant load at the yield stress using direct current potential drop to perform in-situ monitoring of SCC initiation time. Within each weldment, one or more specimens underwent SCC initiation within 24 hours of reaching full load while some specimens had much longer initiation times, in a few cases exceeding 2500 hours. Detailed examinations were conducted on these specimens with a focus on different microstructural features such as preexisting defects, grain orientation and second phases, highlighting anmore » important role of microstructure in crack initiation of alloy 182.« less

A study of the effects of rare-earth elements on the microstructural evolution and deformation behavior of magnesium alloys at temperatures up to 523K

NASA Astrophysics Data System (ADS)

Chakkedath, Ajith

Due to their high specific strength, lightweight magnesium (Mg) alloys are being increasingly used for applications, such as the automotive industry, where weight savings are critical. In order to develop new alloys and processing methods to achieve higher strength and better formability to compete with currently used metal alloys, it is important to understand the effects of alloying elements, processing, and temperature on the microstructure, mechanical properties, and the deformation behavior. In this dissertation, a systematic investigation on the effects of Nd additions (0-1wt.%) and temperature (298-523K) on the microstructure and the activity of different deformation modes in as-cast and cast-then-extruded Mg-1Mn (wt.%) alloys were performed. For this study, an in-situ testing technique which combines tension and compression testing inside a scanning electron microscope (SEM) with electron backscatter diffraction (EBSD) analysis was employed. The main findings of this work were that the microstructure, strength, and the distribution of the deformation modes varied significantly as a function of Nd content, temperature, and processing. An increase in the Nd content resulted in a weaker texture after extrusion in Mg-1Mn alloys. A combination of slip and twinning mechanisms controlled the tensile deformation in the extruded alloys at ambient temperatures. With an increase in temperature, the twinning activity decreased, and slip mechanisms dominated the deformation. In the extruded Nd-containing alloys, basal slip dominated the deformation, especially at elevated temperatures, suggesting that Nd additions strengthen basal slip. This resulted in excellent elevated-temperature strength retention in extruded Mg-1Mn-1Nd alloy, and a decrease in the Nd content to 0-0.3wt.% resulted in a decrease in the tensile strength at elevated temperatures. In extruded Mg-1Mn, contraction twinning dominated the tensile deformation and this alloy exhibited a lower elongation-to-failure (epsilon f) than the other alloys at 323K. With an increase in strain, these twins evolved into {101¯1} - {101¯2} double twins. Crystal plasticity modeling and simulation of the contraction twins and double twins showed that the activity of these twin modes is detrimental to the epsilon f of Mg alloys due to the strain localization that happens within the twinned volume due to the enhanced activity of basal slip. This agreed with the experimental observations. Compared to the extruded materials, the as-cast alloys exhibited significantly larger grain sizes and lower tensile strengths. The deformation in the as-cast alloys was dominated by a combination of basal slip and extension twinning at all test temperatures. A novel methodology which combines in-situ annealing inside a SEM with EBSD analysis was developed and employed to understand the effects of dilute Ce additions (0.2-0.6wt.%) on the recrystallization behavior in Mg-2Zn (wt.%) alloys. Texture weakening in these alloys resulted from the formation of an enhanced number of grain boundaries with rotation axis during recrystallization. The developed testing methodology will be valuable for future recrystallization studies on Mg and other alloy systems. Overall, the insights gained from this dissertation will have a broad impact on understanding the deformation behavior and microstructural evolution of RE-containing Mg alloys, and such insights can serve as guidance for the development of new alloys and processes. The information and data provided in this dissertation can also serve as inputs for the development of accurate crystal plasticity models.

The physical and mechanical metallurgy of advanced O+BCC titanium alloys

NASA Astrophysics Data System (ADS)

Cowen, Christopher John

This thesis comprises a systematic study of the microstructural evolution, phase transformation behavior, elevated-temperature creep behavior, room-temperature and elevated-temperature tensile behavior, and room-temperature fatigue behavior of advanced titanium-aluminum-niobium (Ti-Al-Nb) alloys with and without boron additions. The specific alloys studied were: Ti-5A1-45Nb (at%), Ti-15Al-33Nb (at%), Ti-15Al-33Nb-0.5B (at%), Ti-15Al-33Nb-5B (at%), Ti-21Al-29Nb (at%), Ti-22Al-26Nb (at%), and Ti-22Al-26Nb-5B (at%). The only alloy composition that had been previously studied before this thesis work began was Ti-22Al-26Nb (at%). Publication in peer-reviewed material science journals of the work performed in this thesis has made data available in the scientific literature that was previously non-existent. The knowledge gap for Ti-Al-Nb phase equilibria over the compositional range of Ti-23Al-27Nb (at%) to Ti-12Al-38Nb (at%) that existed before this work began was successfully filled. The addition of 5 at% boron to the Ti-15Al-33Nb alloy produced 5-9 volume percent boride phase needles within the microstructure. The chemical composition of the boride phase measured by electron microprobe was determined to be approximately B 2TiNb. The lattice parameters of the boride phase were simulated through density functional theory calculations by collaborators at the Air Force Research Laboratory based on the measured composition. Using the simulated lattice parameters, electron backscatter diffraction kikuchi patterns and selected area electron diffraction patterns obtained from the boride phase were successfully indexed according to the space group and site occupancies of the B27 orthorhombic crystal structure. This suggests that half the Ti (c) Wyckoff positions are occupied by Ti atoms and the other half are occupied by Nb atoms in the boride phase lattice. Creep deformation behavior is the main focus of this thesis and in particular understanding the dominant creep deformation mechanisms as a function of stress, temperature, and strain rate. Microstructure-creep relationships for Ti-Al-Nb-xB alloys were developed with the understanding gained. A rule-of-mixtures empirical model based on constituent phase volume fractions and strain rates was developed to predict the minimum creep rates of two-phase O+BCC microstructures. The most innovative results of this thesis were produced through the development of an in-situ creep testing methodology. The creep deformation evolution was chronicled in-situ during high temperature creep experiments, while creep displacement versus time data was simultaneously obtained. The in-situ experiments revealed that prior-BCC grain boundaries were the locus of damage accumulation during creep deformation. A methodology that allows in-situ observation of surface creep deformation as a function of creep displacement has yet to be presented in the literature.

Spatially resolved, in situ potential measurements through porous electrodes as applied to fuel cells.

PubMed

Hess, Katherine C; Epting, William K; Litster, Shawn

2011-12-15

We report the development and use of a microstructured electrode scaffold (MES) to make spatially resolved, in situ, electrolyte potential measurements through the thickness of a polymer electrolyte fuel cell (PEFC) electrode. This new approach uses a microfabricated apparatus to analyze the coupled transport and electrochemical phenomena in porous electrodes at the microscale. In this study, the MES allows the fuel cell to run under near-standard operating conditions, while providing electrolyte potential measurements at discrete distances through the electrode's thickness. Here we use spatial distributions of electrolyte potential to evaluate the effects of Ohmic and mass transport resistances on the through-plane reaction distribution for various operating conditions. Additionally, we use the potential distributions to estimate the ionic conductivity of the electrode. Our results indicate the in situ conductivity is higher than typically estimated for PEFC electrodes based on bulk polymer electrolyte membrane (PEM) conductivity.

In situ synthesis of semiconducting single-walled carbon nanotubes by modified arc discharging method

NASA Astrophysics Data System (ADS)

Zhao, Tingkai; Ji, Xianglin; Jin, Wenbo; Yang, Wenbo; Zhao, Xing; Dang, Alei; Li, Hao; Li, Tiehu

2017-02-01

Semiconducting single-walled carbon nanotubes (s-SWCNTs) were in situ synthesized by a temperature-controlled arc discharging furnace with DC electric field using Co-Ni alloy powder as catalyst in helium gas. The microstructures of s-SWCNTs were characterized using high-resolution transmission electron microscopy, electron diffraction, and Raman spectrometry apparatus. The experimental results indicated that the best voltage value in DC electric field is 54 V, and the environmental temperature of the reaction chamber is 600 °C. The mean diameter of s-SWCNTs was estimated about 1.3 nm. The chiral vector ( n, m) of s-SWCNTs was calculated to be (10, 10) type according to the electron diffraction patterns.

In-situ neutron diffraction study of martensitic variant redistribution in polycrystalline Ni-Mn-Ga alloy under cyclic thermo-mechanical treatment

NASA Astrophysics Data System (ADS)

Li, Zongbin; Zhang, Yudong; Esling, Claude; Gan, Weimin; Zou, Naifu; Zhao, Xiang; Zuo, Liang

2014-07-01

The influences of uniaxial compressive stress on martensitic transformation were studied on a polycrystalline Ni-Mn-Ga bulk alloy prepared by directional solidification. Based upon the integrated in-situ neutron diffraction measurements, direct experimental evidence was obtained on the variant redistribution of seven-layered modulated (7M) martensite, triggered by external uniaxial compression during martensitic transformation. Large anisotropic lattice strain, induced by the cyclic thermo-mechanical treatment, has led to the microstructure modification by forming martensitic variants with a strong ⟨0 1 0⟩7M preferential orientation along the loading axis. As a result, the saturation of magnetization became easier to be reached.

In-situ neutron diffraction study of martensitic variant redistribution in polycrystalline Ni-Mn-Ga alloy under cyclic thermo-mechanical treatment

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

Li, Zongbin; Zou, Naifu; Zhao, Xiang

2014-07-14

The influences of uniaxial compressive stress on martensitic transformation were studied on a polycrystalline Ni-Mn-Ga bulk alloy prepared by directional solidification. Based upon the integrated in-situ neutron diffraction measurements, direct experimental evidence was obtained on the variant redistribution of seven-layered modulated (7M) martensite, triggered by external uniaxial compression during martensitic transformation. Large anisotropic lattice strain, induced by the cyclic thermo-mechanical treatment, has led to the microstructure modification by forming martensitic variants with a strong 〈0 1 0〉{sub 7M} preferential orientation along the loading axis. As a result, the saturation of magnetization became easier to be reached.

Experimental investigation on in-situ microwave casting of copper

NASA Astrophysics Data System (ADS)

Raman Mishra, Radha; Sharma, Apurbba Kumar

2018-04-01

The in-situ microwave casting of metallic materials is a recently developed casting process. The process works on the principles of hybrid microwave heating and is accomplished inside the applicator cavity. The process involves – melting of the charge, in-situ pouring and solidification of the melt. The electromagnetic and thermal properties of the charge affects microwave-material interaction and hence melting of the charge. On the other hand, cooling conditions inside the applicator controls solidification process. The present work reports on in-situ casting of copper developed inside a multimode cavity at 2.45 GHz using 1400 W. The molten metal was allowed to get poured in-situ inside a graphite mold and solidification was carried out in the same mold inside the applicator cavity. The interaction of microwave with the charge during exposure was studied and the role of oxide layer during meltingthe copper blocks has been presented. The developed in-situ cast was characterized to access the cast quality. Microstructural study revealed the homogeneous and dense structure of the cast. The X-ray diffraction pattern indicated presence of copper in different orientations with (1 1 1) as the dominant orientation. The average micro indentation hardness of the casts was found 93±20 HV.

Feasibility of in situ controlled heat treatment (ISHT) of Inconel 718 during electron beam melting additive manufacturing

DOE PAGES

Sames, William J.; Unocic, Kinga A.; Helmreich, Grant W.; ...

2016-10-07

A novel technique was developed to control the microstructure evolution in Alloy 718 processed using Electron Beam Melting (EBM). In situ solution treatment and aging of Alloy 718 was performed by heating the top surface of the build after build completion scanning an electron beam to act as a planar heat source during the cool down process. Results demonstrate that the measured hardness (478 ± 7 HV) of the material processed using in situ heat treatment similar to that of peak-aged Inconel 718. Large solidification grains and cracks formed, which are identified as the likely mechanism leading to failure ofmore » tensile tests of the in situ heat treatment material under loading. Despite poor tensile performance, the technique proposed was shown to successively age Alloy 718 (increase precipitate size and hardness) without removing the sample from the process chamber, which can reduce the number of process steps in producing a part. Lastly, tighter controls on processing temperature during layer melting to lower process temperature and selective heating during in situ heat treatment to reduce over-sintering are proposed as methods for improving the process.« less

Functional pitch of a liver: fatty liver disease diagnosis with photoacoustic spectrum analysis

NASA Astrophysics Data System (ADS)

Xu, Guan; Meng, Zhuoxian; Lin, Jiandie; Carson, Paul; Wang, Xueding

2014-03-01

To provide more information for classification and assessment of biological tissues, photoacoustic spectrum analysis (PASA) moves beyond the quantification of the intensities of the photoacoustic (PA) signals by the use of the frequency-domain power distribution, namely power spectrum, of broadband PA signals. The method of PASA quantifies the linear-fit to the power spectrum of the PA signals from a biological tissue with 3 parameters, including intercept, midband-fit and slope. Intercept and midband-fit reflect the total optical absorption of the tissues whereas slope reflects the heterogeneity of the tissue structure. Taking advantage of the optical absorption contrasts contributed by lipid and blood at 1200 and 532 nm, respectively and the heterogeneous tissue microstructure in fatty liver due to the lipid infiltration, we investigate the capability of PASA in identifying histological changes of fatty livers in mouse model. 6 and 9 pairs of normal and fatty liver tissues from rat models were examined by ex vivo experiment with a conventional rotational PA measurement system. One pair of rat models with normal and fatty livers was examined non-invasively and in situ with our recently developed ultrasound and PA parallel imaging system. The results support our hypotheses that the spectrum analysis of PA signals can provide quantitative measures of the differences between the normal and fatty liver tissues and that part of the PA power spectrum can suffice for characterization of microstructures in biological tissues. Experimental results also indicate that the vibrational absorption peak of lipid at 1200nm could facilitate fatty liver diagnosis.

Additive Manufacturing of Reactive In Situ Zr Based Ultra-High Temperature Ceramic Composites

NASA Astrophysics Data System (ADS)

Sahasrabudhe, Himanshu; Bandyopadhyay, Amit

2016-03-01

Reactive in situ multi-material additive manufacturing of ZrB2-based ultra-high-temperature ceramics in a Zr metal matrix was demonstrated using LENS™. Sound metallurgical bonding was achieved between the Zr metal and Zr-BN composites with Ti6Al4V substrate. Though the feedstock Zr power had α phase, LENS™ processing of the Zr powder and Zr-BN premix powder mixture led to the formation of some β phase of Zr. Microstructure of the Zr-BN composite showed primary grains of zirconium diboride phase in zirconium metal matrix. The presence of ZrB2 ceramic phase was confirmed by X-ray diffraction (XRD) analysis. Hardness of pure Zr was measured as 280 ± 12 HV and, by increasing the BN content in the feedstock, the hardness was found to increase. In Zr-5%BN composite, the hardness was 421 ± 10 HV and the same for Zr-10%BN composite was 562 ± 10 HV. It is envisioned that such multi-materials additive manufacturing will enable products in the future that cannot be manufactured using traditional approaches particularly in the areas of high-temperature metal-ceramic composites with compositional and functional gradation.

Crystallization Kinetics in Fluorochloroziroconate Glass-Ceramics

NASA Astrophysics Data System (ADS)

Alvarez, Carlos J.

Annealing fluorochlorozirconate (FCZ) glasses nucleates BaCl2 nanocrystals in the glass matrix, resulting in a nanocomposite glass-ceramic that has optical properties suitable for use as a medical X-ray imaging plate. Understanding the way in which the BaCl¬2 nanocrystal nucleation, growth and phase transformation processes proceed is critical to controlling the optical behavior. However, there is a very limited amount of information about the formation, morphology, and distribution of the nanocrystalline particles in FCZ glass-ceramics. In this thesis, the correlation between the microstructure and the crystallization kinetics of FCZ glass-ceramics, are studied in detail. In situ X-ray diffraction and transmission electron microscopy annealing experiments are used to analyze the crystal structure, size and distribution of BaCl 2 nanocrystals in FCZ glass-ceramics as a function of annealing rate and temperature. Microstructural analysis of the early stages on nucleation identified the formation of both BaCl2 and BaF2 nanocrystals. Annealing FCZ glass-ceramics above 280°C can cause the formation of additional glass matrix phase crystals, their microstructure and the annealing parameters required for their growth are identified. As the crystalline phases grow directly from the glass, small variations in processing of the glass can have a profound influence on the crystallization process. The information obtained from these experiments improves the understanding of the nucleation, growth and phase transformation process of the BaCl¬2 nanocrystals and additional crystalline phases that form in FCZ glass-ceramics, and may help expedite the implementation of FCZ glass-ceramics as next-generation X-ray detectors. Lastly, as these glass-ceramics may one day be commercialized, an investigation into their degradation in different environmental conditions was also performed. The effects of direct contact with water or prolonged exposure to humid environments on the microstructure and the optical properties for FCZ glasses and glass-ceramics was explored.

The Investigation of Strain-Induced Martensite Reverse Transformation in AISI 304 Austenitic Stainless Steel

NASA Astrophysics Data System (ADS)

Cios, G.; Tokarski, T.; Żywczak, A.; Dziurka, R.; Stępień, M.; Gondek, Ł.; Marciszko, M.; Pawłowski, B.; Wieczerzak, K.; Bała, P.

2017-10-01

This paper presents a comprehensive study on the strain-induced martensitic transformation and reversion transformation of the strain-induced martensite in AISI 304 stainless steel using a number of complementary techniques such as dilatometry, calorimetry, magnetometry, and in-situ X-ray diffraction, coupled with high-resolution microstructural transmission Kikuchi diffraction analysis. Tensile deformation was applied at temperatures between room temperature and 213 K (-60 °C) in order to obtain a different volume fraction of strain-induced martensite (up to 70 pct). The volume fraction of the strain-induced martensite, measured by the magnetometric method, was correlated with the total elongation, hardness, and linear thermal expansion coefficient. The thermal expansion coefficient, as well as the hardness of the strain-induced martensitic phase was evaluated. The in-situ thermal treatment experiments showed unusual changes in the kinetics of the reverse transformation (α' → γ). The X-ray diffraction analysis revealed that the reverse transformation may be stress assisted—strains inherited from the martensitic transformation may increase its kinetics at the lower annealing temperature range. More importantly, the transmission Kikuchi diffraction measurements showed that the reverse transformation of the strain-induced martensite proceeds through a displacive, diffusionless mechanism, maintaining the Kurdjumov-Sachs crystallographic relationship between the martensite and the reverted austenite. This finding is in contradiction to the results reported by other researchers for a similar alloy composition.

In-situ studies on the micro-structure evolution of A2W2O7 (A=Li, Na, K) during melting by high temperature Raman spectroscopy and density functional theory.

PubMed

Wang, Jian; You, Jinglin; Wang, Min; Lu, Liming; Wan, Songming; Sobol, A A

2017-10-05

In-situ high temperature Raman spectroscopic (HTRS) technique in combination with density functional theory (DFT) analysis has been adopted to investigate the micro-structure of solid and molten A 2 W 2 O 7 (A=Li, Na, K). The [WO 6 ] octahedra were found to be connected to each other by corner and edge sharing in the crystalline Li 2 W 2 O 7 and K 2 W 2 O 7 compounds. In the crystal lattice of Na 2 W 2 O 7 , on the other hand, the [WO 4 ] tetrahedra and [WO 6 ] octahedra were found to coexist and paired by corner sharing. Although the structural diversity has clearly led to distinct Raman spectra of the crystalline A 2 W 2 O 7 compounds, the spectra of their melts tended to be analogous, showing the typical vibration modes of (W 2 O 7 ) 2- dimer. A mechanism was then proposed to explain the structure evolution occurring during the melting process of A 2 W 2 O 7 . The effect of A + cation on the Raman bands of (W 2 O 7 ) 2- dimer in molten A 2 W 2 O 7 has also been investigated. Both the wavenumber and full width at half-height (FWHH) of the characteristic band assigned to the symmetrical stretching vibration mode of WO nb (non-bridging oxygen) in (W 2 O 7 ) 2- were found to decrease in the sequence of Li + , Na + and K + , indicating the cation effect on the mean bond length and its distribution range of WO nb . In addition, the relative intensity of this band was also influenced by the cation and it was increased in the order of Li 2 W 2 O 7 , Na 2 W 2 O 7 and K 2 W 2 O 7 , which has been explained by the charge transfer process and confirmed by Mulliken overlap population analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

BUNDLE: A Novel Furnace for Performing Controlled Directional Solidification Experiments in a Microgravity Environment

NASA Technical Reports Server (NTRS)

Carrasquillo, Edgar J.; Griffin, Mark R.; Hammond, Monica S.; Johnson, Martin L.; Grugel, R. N.

2000-01-01

NASA Marshall Space Flight Center has developed a novel directional solidification furnace prototype for processing metals and alloys experiments in a microgravity environment. The BUNDLE (Bridgman Unidirectional Dendrite in Liquid Experiment) furnace is intended to accommodate the science requirements of Flight Definition Principle Investigators studying cellular/dendritic growth in aluminum and lead alloys at processing temperatures up to 1200 C. The furnace implements a number of innovative features to achieve high thermal gradients and quench rates in a low-power, light-weight design. These include a pyrolytic boron nitride/graphite composite heating element surrounded by layers of self-supporting refractory metal shielding, and a graphite fiber enhanced cold zone allowing high levels of heat extraction from the sample crucible. Novel to the BUNDLE design is an in-situ helium gas quench capability that ensures rapid freezing of the solidifying region (mushy zone) of the metal sample within the furnace without sample disturbance prior to quenching; this is a stringent requirement for subsequent analysis and understanding of microstructural development. The experiment hardware concept features multiple furnaces that may be "bundled" together so many samples, currently up to eight, can be processed at one time. The design of BUNDLE is flexible enough to be implemented on the Shuttle and Space Station in a number of locations (SpaceHab, Express Rack, MPESS, ISPR, etc). BUNDLE prototype furnaces have directionally solidified and quenched 1cm diameter lead - 5.8 weight percent antimony and aluminum - 4 weight percent copper alloys. Quenching of the mushy zone, as recorded by in-situ thermocouples, occurred on the order of 0.5 seconds or less, a rate within the PI's requirements. Subsequent metallographic examination revealed the solidified microstructure to be, as expected, unidirectional. Both the dendrite tips and the eutectic reaction were planar in nature indicating uniform axial heat flow. Delineation between the growing dendrites and eutectic structure with the "quenched-in" liquid was sharp, attesting to the efficacy of the helium quench. BUNDLE's conception, development, capability, and adaptability are presented (in view of Flight PI's needs and science requirements) through viewgraphs depicting actual hardware, generated thermal analysis, and micrographs prepared from BUNDLE processed, flight-like samples.

BUNDLE - A Novel Furnace for Performing Controlled Directional Solidification Experiments in a Microgravity Environment

NASA Technical Reports Server (NTRS)

Carrasquillo, Edgar J.; Griffin, Mark R.; Hammond, Monica S.; Johnson, Martin L.; Grugel, R. N.

2001-01-01

NASA Marshall Space Flight Center has developed a novel directional solidification furnace prototype for processing metals and alloys experiments in a microgravity environment. The BUNDLE (Bridgman Unidirectional Dendrite in Liquid Experiment) furnace is intended to accommodate the science requirements of Flight Definition Principle Investigators studying cellular/dendritic growth in aluminum and lead alloys at processing temperatures up to 1200 C. The furnace implements a number of innovative features to achieve high thermal gradients and quench rates in a low-power, light-weight design. These include a pyrolytic boron nitride/graphite composite heating element surrounded by layers of self-supporting refractory metal shielding, and a graphite fiber enhanced cold zone allowing high levels of heat extraction from the sample crucible. Novel to the BUNDLE design is an in-situ helium gas quench capability that ensures rapid freezing of the solidifying region (mushy zone) of the metal sample within the furnace without sample disturbance prior to quenching; this is a stringent requirement for subsequent analysis and understanding of microstructural development. The experiment hardware concept features multiple furnaces that may be "bundled" together so many samples, currently up to eight, can be processed at one time. The design of BUNDLE is flexible enough to be implemented on the Shuttle and Space Station in a number of locations (SpaceHab, Express Rack, MPESS, ISPR, etc). BUNDLE prototype furnaces have directionally solidified and quenched 1cm diameter lead - 5.8 weight percent antimony and aluminum - 4 weight percent copper alloys. Quenching of the mushy zone, as recorded by in-situ thermocouples, occurred on the order of 0.5 seconds or less, a rate within the PI's requirements. Subsequent metallographic examination revealed the solidified microstructure to be, as expected, unidirectional. Both the dendrite tips and the eutectic reaction were planar in nature indicating uniform axial heat flow. Delineation between the growing dendrites and eutectic structure with the "quenched-in" liquid was sharp, attesting to the efficacy of the helium quench. BUNDLE's conception, development, capability, and adaptability are presented (in view of Flight PI's needs and science requirements) through viewgraphs depicting actual hardware, generated thermal analysis, and micrographs prepared from BUNDLE processed, flight-like samples.

Reduction Expansion Synthesis as Strategy to Control Nitrogen Doping Level and Surface Area in Graphene

PubMed Central

Canty, Russell; Gonzalez, Edwin; MacDonald, Caleb; Osswald, Sebastian; Zea, Hugo; Luhrs, Claudia C.

2015-01-01

Graphene sheets doped with nitrogen were produced by the reduction-expansion (RES) method utilizing graphite oxide (GO) and urea as precursor materials. The simultaneous graphene generation and nitrogen insertion reactions are based on the fact that urea decomposes upon heating to release reducing gases. The volatile byproducts perform two primary functions: (i) promoting the reduction of the GO and (ii) providing the nitrogen to be inserted in situ as the graphene structure is created. Samples with diverse urea/GO mass ratios were treated at 800 °C in inert atmosphere to generate graphene with diverse microstructural characteristics and levels of nitrogen doping. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to study the microstructural features of the products. The effects of doping on the samples structure and surface area were studied by X-ray diffraction (XRD), Raman Spectroscopy, and Brunauer Emmet Teller (BET). The GO and urea decomposition-reduction process as well as nitrogen-doped graphene stability were studied by thermogravimetric analysis (TGA) coupled with mass spectroscopy (MS) analysis of the evolved gases. Results show that the proposed method offers a high level of control over the amount of nitrogen inserted in the graphene and may be used alternatively to control its surface area. To demonstrate the practical relevance of these findings, as-produced samples were used as electrodes in supercapacitor and battery devices and compared with conventional, thermally exfoliated graphene. PMID:28793618

In Situ Optical Observation of High-Temperature Geological Processes With the Moissanite Cell

NASA Astrophysics Data System (ADS)

Walte, N.; Keppler, H.

2005-12-01

A major drawback of existing techniques in experimental earth and material sciences is the inability to observe ongoing high-temperature processes in situ during an experiment. Examples for important time-dependent processes include the textural development of rocks and oxide systems during melting and crystallization, solid-state and melt-present recrystallization and Ostwald ripening, and bubble nucleation and growth during degassing of glasses and melts. The investigation of these processes by post-mortem analysis of a quenched microstructure is time consuming and often unsatisfactory. Here, we introduce the moissanite cell that allows optical in situ observation of long-term experiments at high temperatures. Moissanite is a transparent gem-quality type of SiC that is characterized by its hardness and superior chemical and thermal resistance. Two moissanite windows with a thickness and diameter of several millimeters are placed into sockets of fired pyrophyllite and fixed onto two opposite metal plates. The sockets are wrapped with heating wire and each window is connected to a thermocouple for temperature control. The sample is placed directly between the moissanite windows and the cell is assembled similarly to a large diamond anvil cell. In situ observation of the sample is done with a microscope through observation windows and movies are recorded with an attached digital camera. Our experiments with the new cell show that temperatures above 1200°C can be maintained and observed in a sample for several days without damaging the cell nor the windows. Time-lapse movies of melting and crystallizing natural and synthetic rocks and of degassing glasses and melts will be presented to show the potential of the new technique for experimental earth and material science.

Measuring twinning and slip in shock-compressed Ta from in-situ x-ray diffraction

NASA Astrophysics Data System (ADS)

Wehrenberg, Christopher; McGonegle, David; Sliwa, Marcin; Suggit, Matt; Wark, Justin; Lee, Hae Ja; Nagler, Bob; Tavella, Franz; Remington, Bruce; Rudd, Rob; Lazicki, Amy; Park, Hye-Sook; Swift, Damian; Zepeda-Ruiz, Louis; Higginbotham, Andrew; Bolme, Cindy

2017-06-01

A fundamental understanding of high-pressure and high-strain-rate deformation rests on grasping the underlying microstructural processes, such as twinning and dislocation generation and transport (slip), yet simulations and ex-post-facto recovery experiments provide conflicting answers to these basic issues. Here, we report direct, in-situ observation of twinning and slip in shock compressed Ta using in-situ x-ray diffraction. A series of shock experiments were performed on the Matter in Extreme Conditions end station at LCLS. Direct laser ablation was used to drive a shock, ranging in pressure from 10-300 GPa, into a Ta sample with an initial (110) fiber texture. The subsequent changes in texture were observed in-situ by examining the azimuthal distribution of the diffraction intensity and found to match twinning and lattice rotation. Measurements of the twin fraction and lattice rotation were used to calculate the equivalent plastic strain from twinning and slip. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract No. DE-AC52-07NA27344.

Predicting neutron damage using TEM with in situ ion irradiation and computer modeling

NASA Astrophysics Data System (ADS)

Kirk, Marquis A.; Li, Meimei; Xu, Donghua; Wirth, Brian D.

2018-01-01

We have constructed a computer model of irradiation defect production closely coordinated with TEM and in situ ion irradiation of Molybdenum at 80 °C over a range of dose, dose rate and foil thickness. We have reexamined our previous ion irradiation data to assign appropriate error and uncertainty based on more recent work. The spatially dependent cascade cluster dynamics model is updated with recent Molecular Dynamics results for cascades in Mo. After a careful assignment of both ion and neutron irradiation dose values in dpa, TEM data are compared for both ion and neutron irradiated Mo from the same source material. Using the computer model of defect formation and evolution based on the in situ ion irradiation of thin foils, the defect microstructure, consisting of densities and sizes of dislocation loops, is predicted for neutron irradiation of bulk material at 80 °C and compared with experiment. Reasonable agreement between model prediction and experimental data demonstrates a promising direction in understanding and predicting neutron damage using a closely coordinated program of in situ ion irradiation experiment and computer simulation.

Deformation behavior and mechanical analysis of vertically aligned carbon nanotube (VACNT) bundles

NASA Astrophysics Data System (ADS)

Hutchens, Shelby B.

Vertically aligned carbon nanotubes (VACNTs) serve as integral components in a variety of applications including MEMS devices, energy absorbing materials, dry adhesives, light absorbing coatings, and electron emitters, all of which require structural robustness. It is only through an understanding of VACNT's structural mechanical response and local constitutive stress-strain relationship that future advancements through rational design may take place. Even for applications in which the structural response is not central to device performance, VACNTs must be sufficiently robust and therefore knowledge of their microstructure-property relationship is essential. This thesis first describes the results of in situ uniaxial compression experiments of 50 micron diameter cylindrical bundles of these complex, hierarchical materials as they undergo unusual deformation behavior. Most notably they deform via a series of localized folding events, originating near the bundle base, which propagate laterally and collapse sequentially from bottom to top. This deformation mechanism accompanies an overall foam-like stress-strain response having elastic, plateau, and densification regimes with the addition of undulations in the stress throughout the plateau regime that correspond to the sequential folding events. Microstructural observations indicate the presence of a strength gradient, due to a gradient in both tube density and alignment along the bundle height, which is found to play a key role in both the sequential deformation process and the overall stress-strain response. Using the complicated structural response as both motivation and confirmation, a finite element model based on a viscoplastic solid is proposed. This model is characterized by a flow stress relation that contains an initial peak followed by strong softening and successive hardening. Analysis of this constitutive relation results in capture of the sequential buckling phenomenon and a strength gradient effect. This combination of experimental and modeling approaches motivates discussion of the particular microstructural mechanisms and local material behavior that govern the non-trivial energy absorption via sequential, localized buckle formation in the VACNT bundles.

Fundamental Investigations and Rational Design of Durable High-Performance SOFC Cathodes

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

Chen, Yu; Ding, Dong; Wei, Tao

The main objective of this project is to unravel the degradation mechanism of LSCF cathodes under realistic operating conditions with different types of contaminants, aiming towards the rational design of cathodes with high-performance and enhanced durability by combining a porous backbone (such as LSCF) with a thin catalyst coating. The mechanistic understanding will help us to optimize the composition and morphology of the catalyst layer and microstructure of the LSCF backbone for better performance and durability. More specifically, the technical objectives include: (1) to unravel the degradation mechanism of LSCF cathodes under realistic operating conditions with different types of contaminantsmore » using in situ and ex situ measurements performed on specially-designed cathodes; (2) to examine the microstructural and compositional evolution of LSCF cathodes as well as the cathode/electrolyte interfaces under realistic operating conditions; (3) to correlate the fuel cell performance instability and degradation with the microstructural and morphological evolution and surface chemistry change of the cathode under realistic operating conditions; (4) to explore new catalyst materials and electrode structures to enhance the stability of the LSCF cathode under realistic operating conditions; and (5) to validate the long term stability of the modified LSCF cathode in commercially available cells under realistic operating conditions. We have systematically evaluated LSCF cathodes in symmetrical cells and anode supported cells under realistic conditions with different types of contaminants such as humidity, CO 2, and Cr. Electrochemical models for the design of test cells and understanding of mechanisms have been developed for the exploration of fundamental properties of electrode materials. It is demonstrated that the activity and stability of LSCF cathodes can be degraded by the introduction of contaminants. The microstructural and compositional evolution of LSCF cathodes as well as the cathode/electrolyte interfaces under realistic operating conditions has been studied. It is found that SrO readily segregated/enriched on the LSCF surface. More severe contamination conditions cause more SrO on surface. Novel catalyst coatings through particle depositions (PrOx) or continuous thin films (PNM) were successfully developed to improve the activity and stability of LSCF cathodes. Finally, we have demonstrated enhanced activity and stability of LSCF cathodes over longer periods of time in homemade and commercially available cells by an optimized PNM (dense film and particles) infiltration process, under clean air and realistic operating conditions (3% H 2O, 5% CO 2 and direct Crofer contact). Both performance and durability of single cells with PNM coating has been enhanced compared with those without coating. Raman analysis of cathodes surface indicated that the intensity of SrCrO 4 was significantly decreased.« less

Fabrication and characterization of microstructure of stainless steel matrix composites containing up to 25 vol% NbC

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

Kan, Wen Hao, E-mail: wkan6795@uni.sydney.edu.au

AISI 440 stainless steels reinforced with various volume fractions of niobium carbide (NbC) particles of up to 25 vol% were fabricated in-situ using an argon arc furnace and then heat-treated to produce a martensitic matrix. Optical and scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and electron back-scatter diffraction (EBSD) techniques were used to analyze the microstructure, phases and composition of these composites. Interestingly, it was found that Chinese-script NbC could nucleate on existing primary NbC particles creating NbC clusters with complex microstructures. Additionally, hardness tests were used to evaluate viability in mining and mineral processing applications. The increasemore » in NbC content resulted in an overall increase in the hardness of the composites while causing a marginal decrease in the amount of Cr in solid solution with the matrix, which could be a concern for corrosion resistance. The latter was due to the fact that the NbC lattice could dissolve a minor amount of Cr. Thermodynamic simulations also attributed this to a slight increase in M{sub 7}C{sub 3} precipitation. Nonetheless, these novel composites show great promise for applications in wear and corrosive environments. - Highlights: •Stainless steels reinforced with NbC particles of up to 25 vol% were fabricated. •NbC was formed in-situ in the steels using an arc melter. •Martensitic transformation of the matrix of each sample was achieved. •NbC reinforcements increased the bulk hardness values of the steels. •Dissolved Cr in the matrix of each sample was sufficient for passivity in theory.« less

Gradient twinned 304 stainless steels for high strength and high ductility

DOE PAGES

Chen, Aiying; Liu, Jiabin; Wang, Hongtao; ...

2016-04-23

Gradient materials often have attractive mechanical properties that outperform uniform microstructure counterparts. It remains a difficult task to investigate and compare the performance of various gradient microstructures due to the difficulty of fabrication, the wide range of length scales involved, and their respective volume percentage variations. We have investigated four types of gradient microstructures in 304 stainless steels that utilize submicrotwins, nanotwins, nanocrystalline-, ultrafine- and coarse-grains as building blocks. Tensile tests reveal that the gradient microstructure consisting of submicrotwins and nanotwins has a persistent and stable work hardening rate and yields an impressive combination of high strength and high ductility,more » leading to a toughness that is nearly 50% higher than that of the coarse-grained counterpart. Ex- and in-situ transmission electron microscopy indicates that nanoscale and submicroscale twins help to suppress and limit martensitic phase transformation via the confinement of martensite within the twin lamellar. Twinning and detwinning remain active during tensile deformation and contribute to the work hardening behavior. We discuss the advantageous properties of using submicrotwins as the main load carrier and nanotwins as the strengthening layers over those coarse and nanocrystalline grains. Furthermore, our work uncovers a new gradient design strategy to help metals and alloys achieve high strength and high ductility.« less

A quantitative and non-contact technique to characterise microstructural variations of skin tissues during photo-damaging process based on Mueller matrix polarimetry.

PubMed

Dong, Yang; He, Honghui; Sheng, Wei; Wu, Jian; Ma, Hui

2017-10-31

Skin tissue consists of collagen and elastic fibres, which are highly susceptible to damage when exposed to ultraviolet radiation (UVR), leading to skin aging and cancer. However, a lack of non-invasive detection methods makes determining the degree of UVR damage to skin in real time difficult. As one of the fundamental features of light, polarization can be used to develop imaging techniques capable of providing structural information about tissues. In particular, Mueller matrix polarimetry is suitable for detecting changes in collagen and elastic fibres. Here, we demonstrate a novel, quantitative, non-contact and in situ technique based on Mueller matrix polarimetry for monitoring the microstructural changes of skin tissues during UVR-induced photo-damaging. We measured the Mueller matrices of nude mouse skin samples, then analysed the transformed parameters to characterise microstructural changes during the skin photo-damaging and self-repairing processes. Comparisons between samples with and without the application of a sunscreen showed that the Mueller matrix-derived parameters are potential indicators for fibrous microstructure in skin tissues. Histological examination and Monte Carlo simulations confirmed the relationship between the Mueller matrix parameters and changes to fibrous structures. This technique paves the way for non-contact evaluation of skin structure in cosmetics and dermatological health.

A method to generate conformal finite-element meshes from 3D measurements of microstructurally small fatigue-crack propagation [A method to generate conformal finite-element meshes from 3D measurements of microstructurally small fatigue-crack propagation: 3D Meshes of Microstructurally Small Crack Growth

DOE PAGES

Spear, Ashley D.; Hochhalter, Jacob D.; Cerrone, Albert R.; ...

2016-04-27

In an effort to reproduce computationally the observed evolution of microstructurally small fatigue cracks (MSFCs), a method is presented for generating conformal, finite-element (FE), volume meshes from 3D measurements of MSFC propagation. The resulting volume meshes contain traction-free surfaces that conform to incrementally measured 3D crack shapes. Grain morphologies measured using near-field high-energy X-ray diffraction microscopy are also represented within the FE volume meshes. Proof-of-concept simulations are performed to demonstrate the utility of the mesh-generation method. The proof-of-concept simulations employ a crystal-plasticity constitutive model and are performed using the conformal FE meshes corresponding to successive crack-growth increments. Although the simulationsmore » for each crack increment are currently independent of one another, they need not be, and transfer of material-state information among successive crack-increment meshes is discussed. The mesh-generation method was developed using post-mortem measurements, yet it is general enough that it can be applied to in-situ measurements of 3D MSFC propagation.« less

A method to generate conformal finite-element meshes from 3D measurements of microstructurally small fatigue-crack propagation [A method to generate conformal finite-element meshes from 3D measurements of microstructurally small fatigue-crack propagation: 3D Meshes of Microstructurally Small Crack Growth

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

Spear, Ashley D.; Hochhalter, Jacob D.; Cerrone, Albert R.

In an effort to reproduce computationally the observed evolution of microstructurally small fatigue cracks (MSFCs), a method is presented for generating conformal, finite-element (FE), volume meshes from 3D measurements of MSFC propagation. The resulting volume meshes contain traction-free surfaces that conform to incrementally measured 3D crack shapes. Grain morphologies measured using near-field high-energy X-ray diffraction microscopy are also represented within the FE volume meshes. Proof-of-concept simulations are performed to demonstrate the utility of the mesh-generation method. The proof-of-concept simulations employ a crystal-plasticity constitutive model and are performed using the conformal FE meshes corresponding to successive crack-growth increments. Although the simulationsmore » for each crack increment are currently independent of one another, they need not be, and transfer of material-state information among successive crack-increment meshes is discussed. The mesh-generation method was developed using post-mortem measurements, yet it is general enough that it can be applied to in-situ measurements of 3D MSFC propagation.« less

LA-ICP-MS-derived U-concentrations and microstructural domains within biogenic aragonite of Arctica islandica shell.

PubMed

Helama, Samuli; Heikkilä, Pasi; Rinne, Katja; Nielsen, Jan Kresten; Nielsen, Jesper Kresten

2015-05-01

Understanding of the uranium uptake processes (both in vivo and post-mortem) into the skeletal structures of marine calcifiers is a subject of multi-disciplinary interest. U-concentration changes within the molluscan shell may serve as a paleoceanographic proxy of the pH history. A proxy of this type is needed to track the effects of fossil fuel emissions to ocean acidification. Moreover, attaining reliable U-series dates using shell materials would be a geochronological breakthrough. Picturing the high-resolution changes of U-concentrations in shell profiles is now possible by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS). Here, we analyzed in situ U-concentration variations in sub-fossilized shells of ocean quahog (Arctica islandica), a commonly studied bivalve species in Quaternary geoscience, using LA-ICP-MS. Microstructural details of the shell profiles were achieved by the scanning electron microscopy (SEM). Comparison of the shell aragonite microstructure with the changes in U-concentration revealed that uranium of possibly secondary origin is concentrated into the porous granular layers of the shell. Our results reinforce the hypothesis that U-concentration variations can be linked with microstructural differences within the shell. A combination of LA-ICP-MS and SEM analyses is recommended as an interesting approach for understanding the U-concentration variations in similar materials.

Correlating thermoelectric properties with microstructure in Bi 0.8 Sb 0.2 thin films

DOE PAGES

Siegal, M. P.; Lima-Sharma, A. L.; Sharma, P. A.; ...

2017-04-03

The room temperature electronic transport properties of 100 nm-thick thermoelectric Bi 0.8Sb 0.2 films, sputter-deposited onto quartz substrates and post-annealed in an ex-situ furnace, systematically correlate with the overall microstructural quality, improving with increasing annealing temperature until close to the melting point for the alloy composition. Furthermore, the optimized films have high crystalline quality with ~99% of the grains oriented with the trigonal axis perpendicular to the substrate surface. Film resistivities and Seebeck coefficients are accurately measured by preventing deleterious surface oxide formation via a SiN capping layer and using Nd-doped Al for contacts. Our resulting values are similar tomore » single crystals and significantly better than previous reports from films and polycrystalline bulk alloys.« less

Mechanical Properties of Organized Microcomposites Fabricated by Interference Lithography

NASA Astrophysics Data System (ADS)

Singamaneni, Srikanth; Chang, Sehoon; Jang, Ji-Hyun; Davis, Whitney; Thomas, Edwin; Tsukruk, Vladimir

2009-03-01

We demonstrate that organized, porous, polymer microstructures with continuous open nanoscale pores and sub-micron spacings obtained via interference lithography can be successfully utilized in a highly non-traditional field of ordered microcomposites. Organized microcomposite structures are fabricated by employing two independent strategies, namely, capillary infiltration and in situ polymerization of the rubbery component into the porous glassy microframes. The mechanical properties and ultimate fracture behavior of the single and bicomponent microframes are investigated at different length scales. The ordered single and bi-component microstructures with high degree of control over the microscopic organization of the polymeric phases result in excellent mechanical properties. Combining hard and soft polymer components provides multifunctional materials and coatings with synergetic properties and is frequently utilized for design of advanced polymeric composites.

The Crystal Hotel: A Microfluidic Approach to Biomimetic Crystallization.

PubMed

Gong, Xiuqing; Wang, Yun-Wei; Ihli, Johannes; Kim, Yi-Yeoun; Li, Shunbo; Walshaw, Richard; Chen, Li; Meldrum, Fiona C

2015-12-02

A "crystal hotel" microfluidic device that allows crystal growth in confined volumes to be studied in situ is used to produce large calcite single crystals with predefined crystallographic orientation, microstructure, and shape by control of the detailed physical environment, flow, and surface chemistry. This general approach can be extended to form technologically important, nanopatterned single crystals. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Adaption of an In-Situ Microscale Tension Technique to Enable Fatigue Testing (PREPRINT)

DTIC Science & Technology

2012-08-01

mechanical properties , including fatigue performance, are strongly related to the crystallographic texture of these alloys.[5-7] With the combined use...effects, exploration of deformation micromechanisms, and measurement of the local properties in a bulk material (e.g., variations in the local...Approved for public release; distribution unlimited 9 microstructure of this material , would be expected to exhibit a reduction in mechanical properties

Acoustic Scattering Models of Zooplankton and Microstructure

DTIC Science & Technology

1999-09-30

1998, a remotely operated vehicle was used to deploy acoustic transducers so that the acoustic scattering by siphonophores , a gas-bearing animal, could...their high frequency acoustics systems. 4) In addition, we have identified two types of zooplankton ( siphonophores and pteropods) that have high...Benfield, P.H. Wiebe, and D. Chu, 1999. “In situ measurements of acoustic target strengths of siphonophores ,” Proceedings of the 2nd EAA

In situ synthesis of Fe-based alloy clad coatings containing TiB2-TiN-(h-BN)

NASA Astrophysics Data System (ADS)

Jiang, Shao-qun; Wang, Gang; Ren, Qing-wen; Yang, Chuan-duo; Wang, Ze-hua; Zhou, Ze-hua

2015-06-01

Fe-based alloy coatings containing TiB2-TiN-(h-BN) were synthesized in situ on Q235 steel substrates by a plasma cladding process using the powders of Fe901 alloy, Ti, and h-BN as raw materials. The effects of Ti/h-BN mass ratio on interfacial bonds between the coating and substrate along with the microstructures and microhardnesses of the coatings were investigated. The results show that the Ti/h-BN mass ratio is a vital factor in the formation of the coatings. Free h-BN can be introduced into the coatings by adding an excess amount of h-BN into the precursor. Decreases in the Ti/h-BN mass ratio improve the microstructural uniformity and compactness and enhance the interfacial bonds of the coatings. At a Ti/h-BN mass ratio of 10/20, the coating is free of cracks and micropores, and mainly consists of Fe-Cr, Fe3B, TiB2, TiN, Ti2N, TiB, FeN, FeB, Fe2B, and h-BN phases. Its average microhardness in the zone between 0.1-2.8 mm from the coating surface is about Hv0.2 551.5.

Process-Property Relationship for Air Plasma-Sprayed Gadolinium Zirconate Coatings

NASA Astrophysics Data System (ADS)

Dwivedi, Gopal; Tan, Yang; Viswanathan, Vaishak; Sampath, Sanjay

2015-02-01

The continuous need of elevating operating temperature of gas turbine engines has introduced several challenges with the current state-of-the-art yttria-stabilized zirconia (YSZ)-based thermal barrier coatings (TBCs), requiring examination of new TBC material with high temperature phase stability, lower thermal conductivity, and resistance to environmental ash particles. Gadolinium zirconate (Gd2Zr2O7) (GDZ) has been shown to meet many of these requirements, and has, in fact, been successfully implemented in to engine components. However, several fundamental issues related to the process-ability, toughness, and microstructural differences for GDZ when compared to equivalent YSZ coating. This study seeks to critically address the process-structure-property correlations for plasma-sprayed GDZ coating subjected to controlled parametric exploration. Use of in-flight diagnostics coupled with in situ and ex situ coating property monitoring allows examination and comparison of the process-property interplay and the resultant differences between the two TBC compositions. The results indicate that it is feasible to retain material chemistry and fabricate relevant microstructures of interest with GDZ with concomitant performance advantages such as low conductivity, mechanical compliance, sintering resistance, and suppression of environmentally induced damage from ash particles. This study provides a framework for optimal design and manufacturing of emergent multi-layer and multi-material TBCs.

In-Situ Synthetic TiB2 Particulate Reinforced Metal Matrix Composite Coating on AA2024 Aluminum Alloy by Laser Cladding Technology

NASA Astrophysics Data System (ADS)

Xu, Jiang; Kan, Yide; Liu, Wenjin

In order to improve the wear resistance of aluminum alloy, in-situ synthesized TiB2 and Ti3B4 peritectic composite particulate reinforced metal matrix composite, formed on a 2024 aluminum alloy by laser cladding with a powder mixture of Fe-coated Boron, Ti and Al, was successfully achieved using 3-KW CW CO2 laser. The chemical composition, microstructure and phase structure of the composite clad coating were analyzed by energy dispersive X-ray spectroscopy (EDX), SEM, AFM and XRD. The typical microstructure of the composite coating is composed of TiB2, Ti3B4, Al3Ti, Al3Fe and α-Al. The surface hardness of cladding coating increases with the amount of added Fe-coated B and Ti powder which determines the amount of TiB2 and Ti3B4 peritectic composite particulate. The nanohardness and the elastic modulus at the interface of the TiB2 and Ti3B4 peritectic composite particulate/matrix were investigated using the nanoindentation technique. The results showed that the nanohardness and the reduced elastic modulus from the peritectic composite particulate to the matrix is a gradient distribution.

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

Microstructural characterization of multiphase chocolate using X-ray microtomography.

PubMed

Frisullo, Pierangelo; Licciardello, Fabio; Muratore, Giuseppe; Del Nobile, Matteo Alessandro

2010-09-01

In this study, X-ray microtomography (μCT) was used for the image analysis of the microstructure of 12 types of Italian aerated chocolate chosen to exhibit variability in terms of cocoa mass content. Appropriate quantitative 3-dimensional parameters describing the microstructure were calculated, for example, the structure thickness (ST), object structure volume ratio (OSVR), and the percentage object volume (POV). Chemical analysis was also performed to correlate the microstructural data to the chemical composition of the samples. Correlation between the μCT parameters acquired for the pore microstructure evaluation and the chemical analysis revealed that the sugar crystals content does not influence the pore structure and content. On the other hand, it revealed that there is a strong correlation between the POV and the sugar content obtained by chemical analysis. The results from this study show that μCT is a suitable technique for the microstructural analysis of confectionary products such as chocolates and not only does it provide an accurate analysis of the pores and microstructure but the data obtained could also be used to aid in the assessment of its composition and consistency with label specifications. X-ray microtomography (μCT) is a noninvasive and nondestructive 3-D imaging technique that has several advantages over other methods, including the ability to image low-moisture materials. Given the enormous success of μCT in medical applications, material science, chemical engineering, geology, and biology, it is not surprising that in recent years much attention has been focused on extending this imaging technique to food science as a useful technique to aid in the study of food microstructure. X-ray microtomography provides in-depth information on the microstructure of the food product being tested; therefore, a better understanding of the physical structure of the product and from an engineering perspective, knowledge about the microstructure of foods can be used to identify the important processing parameters that affect the quality of a product.

The Effect of Li Additions on Wear Properties of Al-Mg2Si Cast In-situ Composites

NASA Astrophysics Data System (ADS)

Ghorbani, M. R.; Emamy, M.; Ghiasinejad, J.; Malekan, A.

2010-06-01

Wear rate of a modified Al-Mg2Si composite was studied by the use of a conventional pin-on-disc technique. In-situ Al-Mg2Si composites (15, 20, 25 wt.%) were cast in a simple cylindrical mold. 0.3 wt.% Li was added into the molten composite to modify its microstructure. It has been found that Li addition decreases the mean size of primary Mg2Si particles. The wear behavior of different composites at different rates revealed that Li addition increases the wear properties of Al-15%Mg2Si to some extent but it did not have any significant influence on wear properties of two other composites.

Thermographic Microstructure Monitoring in Electron Beam Additive Manufacturing.

PubMed

Raplee, J; Plotkowski, A; Kirka, M M; Dinwiddie, R; Okello, A; Dehoff, R R; Babu, S S

2017-03-03

To reduce the uncertainty of build performance in metal additive manufacturing, robust process monitoring systems that can detect imperfections and improve repeatability are desired. One of the most promising methods for in situ monitoring is thermographic imaging. However, there is a challenge in using this technology due to the difference in surface emittance between the metal powder and solidified part being observed that affects the accuracy of the temperature data collected. The purpose of the present study was to develop a method for properly calibrating temperature profiles from thermographic data to account for this emittance change and to determine important characteristics of the build through additional processing. The thermographic data was analyzed to identify the transition of material from metal powder to a solid as-printed part. A corrected temperature profile was then assembled for each point using calibrations for these surface conditions. Using this data, the thermal gradient and solid-liquid interface velocity were approximated and correlated to experimentally observed microstructural variation within the part. This work shows that by using a method of process monitoring, repeatability of a build could be monitored specifically in relation to microstructure control.

Influence of adding strong-carbide-formation elements multiply on particle-reinforced Fe-matrix composite layer produced by laser cladding

NASA Astrophysics Data System (ADS)

Ma, Mingxing; Liu, Wenjin; Zhong, Minlin; Zhang, Hongjun; Zhang, Weiming

2005-01-01

In the research hotspot of particle reinforced metal-matrix composite layer produced by laser cladding, in-situ reinforced particles obtained by adding strong-carbide-formation elements into cladding power have been attracting more attention for their unique advantage. The research has demonstrated that when adding strong-carbide-formation elements-Ti into the cladding powder of the Fe-C-Si-B separately, by optimizing the composition, better cladding coating with the characters of better strength and toughness, higher wear resistance and free of cracks. When the microstructure of cladding coating is hypoeutectic microstructure, its comprehensive performance is best. The research discovered that, compositely adding the strong-carbide-formation elements like Ti+V, Ti+Zr or V+Zr into the cladding coating is able to improve its comprehensive capability. All the cladding coatings obtained are hypoeutectic microstructure. The cladding coatings have a great deal of particulates, and its average microhardness reaches HV0.2700-1400. The research also discovered that the cladding coating obtained is of less cracking after adding the Ti+Zr.

Thermographic Microstructure Monitoring in Electron Beam Additive Manufacturing

DOE PAGES

Raplee, Jake B.; Plotkowski, Alex J.; Kirka, Michael M.; ...

2017-03-03

To reduce the uncertainty of build performance in metal additive manufacturing, robust process monitoring systems that can detect imperfections and improve repeatability are desired. One of the most promising methods for in-situ monitoring is thermographic imaging. However, there is a challenge in using this technology due to the difference in surface emittance between the metal powder and solidified part being observed that affects the accuracy of the temperature data collected. This developed a method for properly calibrating temperature profiles from thermographic data and then determining important characteristics of the build through additional processing. The thermographic data was analyzed to determinemore » the transition of material from metal powder to a solid as-printed part. A corrected temperature profile was then assembled for each point using calibrations for these surface conditions. Using this data, we calculated the thermal gradient and solid-liquid interface velocity and correlated it to microstructural variation within the part experimentally. This work shows that by using a method of process monitoring, repeatability of a build could be monitored specifically in relation to microstructure control.« less

Removing Biofilms from Microstructured Titanium Ex Vivo: A Novel Approach Using Atmospheric Plasma Technology

PubMed Central

Rupf, Stefan; Idlibi, Ahmad Nour; Marrawi, Fuad Al; Hannig, Matthias; Schubert, Andreas; von Mueller, Lutz; Spitzer, Wolfgang; Holtmann, Henrik; Lehmann, Antje; Rueppell, Andre; Schindler, Axel

2011-01-01

The removal of biofilms from microstructured titanium used for dental implants is a still unresolved challenge. This experimental study investigated disinfection and removal of in situ formed biofilms from microstructured titanium using cold atmospheric plasma in combination with air/water spray. Titanium discs (roughness (Ra): 1.96 µm) were exposed to human oral cavities for 24 and 72 hours (n = 149 each) to produce biofilms. Biofilm thickness was determined using confocal laser scanning microscopy (n = 5 each). Plasma treatment of biofilms was carried out ex vivo using a microwave-driven pulsed plasma source working at temperatures from 39 to 43°C. Following plasma treatment, one group was air/water spray treated before re-treatment by second plasma pulses. Vital microorganisms on the titanium surfaces were identified by contact culture (Rodac agar plates). Biofilm presence and bacterial viability were quantified by fluorescence microscopy. Morphology of titanium surfaces and attached biofilms was visualized by scanning electron microscopy (SEM). Total protein amounts of biofilms were colorimetrically quantified. Untreated and air/water treated biofilms served as controls. Cold plasma treatment of native biofilms with a mean thickness of 19 µm (24 h) to 91 µm (72 h) covering the microstructure of the titanium surface caused inactivation of biofilm bacteria and significant reduction of protein amounts. Total removal of biofilms, however, required additional application of air/water spray, and a second series of plasma treatment. Importantly, the microstructure of the titanium discs was not altered by plasma treatment. The combination of atmospheric plasma and non-abrasive air/water spray is applicable for complete elimination of oral biofilms from microstructured titanium used for dental implants and may enable new routes for the therapy of periimplant disease. PMID:22016784

Image-Based Macro-Micro Finite Element Models of a Canine Femur with Implant Design Implications

NASA Astrophysics Data System (ADS)

Ghosh, Somnath; Krishnan, Ganapathi; Dyce, Jonathan

2006-06-01

In this paper, a comprehensive model of a bone-cement-implant assembly is developed for a canine cemented femoral prosthesis system. Various steps in this development entail profiling the canine femur contours by computed tomography (CT) scanning, computer aided design (CAD) reconstruction of the canine femur from CT images, CAD modeling of the implant from implant blue prints and CAD modeling of the interface cement. Finite element analysis of the macroscopic assembly is conducted for stress analysis in individual components of the system, accounting for variation in density and material properties in the porous bone material. A sensitivity analysis is conducted with the macroscopic model to investigate the effect of implant design variables on the stress distribution in the assembly. Subsequently, rigorous microstructural analysis of the bone incorporating the morphological intricacies is conducted. Various steps in this development include acquisition of the bone microstructural data from histological serial sectioning, stacking of sections to obtain 3D renderings of void distributions, microstructural characterization and determination of properties and, finally, microstructural stress analysis using a 3D Voronoi cell finite element method. Generation of the simulated microstructure and analysis by the 3D Voronoi cell finite element model provides a new way of modeling complex microstructures and correlating to morphological characteristics. An inverse calculation of the material parameters of bone by combining macroscopic experiments with microstructural characterization and analysis provides a new approach to evaluating properties without having to do experiments at this scale. Finally, the microstructural stresses in the femur are computed using the 3D VCFEM to study the stress distribution at the scale of the bone porosity. Significant difference is observed between the macroscopic stresses and the peak microscopic stresses at different locations.

Real-time Analysis of the Enzymatic Biodegradation of Polyhydroxyalkanoate Thin Films Using Microfabricated Polymer Microstructures

NASA Astrophysics Data System (ADS)

Delfaus, Stephen; Latuga, Brian M.; Morse, Clinton; McCarney, Evan R.; Rossini, Connie J.; Augustine, Brian H.; Flythe, Michael D.; Rowe, Sean; Baron, Stephen F.; Dennis, Douglas E.

2003-11-01

In-situ atomic force microscopy (AFM) allows for the real-time acquisition and analysis of materials undergoing biological and chemical alterations. A co-polymer blend of poly 3-hydroxybutyrate / poly 3-hydroxyvalerate P(3HB-3HV) were spun-cast onto glass slides to create thin films with film thickness of 40 nm. This polymer is naturally biodegradable by a variety of bacterially produced enzymes. In this study, these materials were degraded by an untyped and concentrated Strptomyces sp. enzyme produced from soil. Using liquid-cell AFM in contact mode, we were able to observe biodegradation uniformly across the surface of the P(3HB-3HV) films beginning within 2 min of introduction of the enzyme. Height standards have been developed using microcontact printing of self assembled monolayers and selective dewetting to produce P(3HB-3HV) structures with dimensions as small as 10 mm. We will discuss the use of microfabricated height standards to measure biodegradation kinetics in these polymers.

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

DOE PAGES

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

2015-06-24

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

Application of Image Analysis for Characterization of Spatial Arrangements of Features in Microstructure

NASA Technical Reports Server (NTRS)

Louis, Pascal; Gokhale, Arun M.

1995-01-01

A number of microstructural processes are sensitive to the spatial arrangements of features in microstructure. However, very little attention has been given in the past to the experimental measurements of the descriptors of microstructural distance distributions due to the lack of practically feasible methods. We present a digital image analysis procedure to estimate the micro-structural distance distributions. The application of the technique is demonstrated via estimation of K function, radial distribution function, and nearest-neighbor distribution function of hollow spherical carbon particulates in a polymer matrix composite, observed in a metallographic section.

Flexible bipolar nanofibrous membranes for improving gradient microstructure in tendon-to-bone healing.

PubMed

Li, Xiaoxi; Cheng, Ruoyu; Sun, Zhiyong; Su, Wei; Pan, Guoqing; Zhao, Song; Zhao, Jinzhong; Cui, Wenguo

2017-10-01

Enthesis is a specialized tissue interface between the tendon and bone. Enthesis structure is very complex because of gradient changes in its composition and structure. There is currently no strategy to create a suitable environment and to regenerate the gradual-changing enthesis because of the modular complexities between two tissue types. Herein, a dual-layer organic/inorganic flexible bipolar fibrous membrane (BFM) was successfully fabricated by electrospinning to generate biomimetic non-mineralized fibrocartilage and mineralized fibrocartilage in tendon-to-bone integration of enthesis. The growth of the in situ apatite nanoparticle layer was induced on the nano hydroxyapatite-poly-l-lactic acid (nHA-PLLA) fibrous layer in simulated body solution, and the poly-l-lactic acid (PLLA) fibrous layer retained its original properties to induce tendon regeneration. The in vivo results showed that BFM significantly increased the area of glycosaminoglycan staining at the tendon-bone interface and improved collagen organization when compared to the simplex fibrous membrane (SFM) of PLLA. Implanting the bipolar membrane also induced bone formation and fibrillogenesis as assessed by micro-CT and histological analysis. Biomechanical testing showed that the BFM group had a greater ultimate load-to-failure and stiffness than the SFM group at 12weeks after surgery. Therefore, this flexible bipolar nanofibrous membrane improves the healing and regeneration process of the enthesis in rotator cuff repair. In this study, we generated a biomimetic dual-layer organic/inorganic flexible bipolar fibrous membrane by sequential electrospinning and in situ biomineralization, producing integrated bipolar fibrous membranes of PLLA fibrous membrane as the upper layer and nHA-PLLA fibrous membrane as the lower layer to mimic non-mineralized fibrocartilage and mineralized fibrocartilage in tendon-to-bone integration of enthesis. Flexible bipolar nanofibrous membranes could be easily fabricated with gradient microstructure for enthesis regeneration in rotator cuff tears. Copyright © 2017 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Microstructure-property relationships of chemically vapor deposited zirconia fiber coating for environmentally durable silicon carbide/silicon carbide composites

NASA Astrophysics Data System (ADS)

Li, Hao

In SiC/SiC ceramic matrix composites, toughness is obtained by adding a fiber coating, which provides a weak interface for crack deflection and debonding between the fiber and the matrix. However, the most commonly used fiber coatings, carbon and boron nitride, are unstable in oxidative environments. In the present study, the feasibility of using a chemically vapor deposited zirconia (CVD-ZrO2) fiber coating as an oxidation-resistant interphase for SiC/SiC composites was investigated. A study of morphological evolution in the CVD-ZrO2 coating suggested that a size-controlled displacive phase transformation from tetragonal ZrO2 ( t-ZrO2) to monoclinic ZrO2 (m-ZrO 2) was the key mechanism responsible for the weak interface behavior exhibited by the ZrO2 coating. It appeared that a low oxygen partial pressure in the CVD reactor chamber was essential for the nucleation of t-ZrO2 and therefore was responsible for the delamination behavior. With this understanding of the weak interface mechanism, minicomposite specimens containing various ZrO2 fiber coating morphologies were fabricated and tested. A fractographic analysis showed that in-situ fiber strength and minicomposite failure loads were strongly dependent on the phase contents and microstructure of the ZrO2 coating. We determined that an optimum microstructure of the ZrO2 coating should contain a predelaminated interface surrounded by a dense outer layer. The outer layer was needed to protect the fiber from degradation during the subsequent SiC matrix infiltration procedure. A preliminary tensile stress-rupture study indicated that the ZrO2 coating exhibited promising performance in terms of providing the weak interface behavior and maintaining the thermal and oxidative stability at elevated temperatures.

Deformation Behavior of Ultra-Strong and Ductile Mg-Gd-Y-Zn-Zr Alloy with Bimodal Microstructure

NASA Astrophysics Data System (ADS)

Xu, C.; Fan, G. H.; Nakata, T.; Liang, X.; Chi, Y. Q.; Qiao, X. G.; Cao, G. J.; Zhang, T. T.; Huang, M.; Miao, K. S.; Zheng, M. Y.; Kamado, S.; Xie, H. L.

2018-02-01

An ultra-strong and ductile Mg-8.2Gd-3.8Y-1Zn-0.4Zr (wt pct) alloy was developed by using hot extrusion to modify the microstructure via forced-air cooling and an artificial aging treatment. A superior strength-ductility balance was obtained that had a tensile yield strength of 466 MPa and an elongation to failure of 14.5 pct. The local strain evolution during the in situ testing of the ultra-strong and ductile alloy was quantitatively analyzed with high-resolution electron backscattered diffraction and digital image correlation. The fracture behavior during the tensile test was characterized by synchrotron X-ray tomography along with SEM and STEM observations. The alloy showed a bimodal microstructure, consisting of dynamically recrystallized (DRXed) grains with random orientations and elongated hot-worked grains with < { 10{\\bar{1}}0} > parallel to the extrusion direction. The DRXed grains were deformed by the basal <;a> slip and the hot-worked grains were deformed by the prismatic slip dominantly. The strain evolution analysis indicated that the multilayered structure relaxed the strain localization via strain transfer from the DRXed to the hot-worked regions, which led to the high ductility of the alloy. Precipitation of the γ' on basal planes and the β' phases on the prismatic planes of the α-Mg generated closed volumes, which enhanced the strength by pinning dislocations effectively, and contributed to the high ductility by impeding the propagation of micro-cracks inside the grains. The deformation incompatibility between the hot-worked grains and the arched block-shaped long-period stacking ordered (LPSO) phases induced the crack initiation and propagation, which fractured the alloy.

In Situ SEM Observations of Fracture Behavior of Laser Welded-Brazed Al/Steel Dissimilar Joint

NASA Astrophysics Data System (ADS)

Xia, Hongbo; Tan, Caiwang; Li, Liqun; Ma, Ninshu

2018-03-01

Laser welding-brazing of 6061-T6 aluminum alloy to DP590 dual-phase steel with Al-Si12 flux-cored filler wire was performed. The microstructure at the brazing interface was characterized. Fracture behavior was observed and analyzed by in situ scanning electron microscope. The microstructure of the brazing interface showed that inhomogeneous intermetallic compounds formed along the thickness direction, which had a great influence on the crack initiation and propagation. In the top region, the reaction layer at the interface consisted of scattered needle-like Fe(Al,Si)3 and serration-shaped Fe1.8Al7.2Si. In the middle region, the compound at the interface was only serration-shaped Fe1.8Al7.2Si. In the bottom region, the interface was composed of lamellar-shaped Fe1.8Al7.2Si. The cracks were first detected in the bottom region and propagated from bottom to top along the interface. At the bottom region, the crack initiated and propagated along the Fe1.8Al7.2Si/weld seam interface during the in situ tensile test. When the crack propagated into the middle region, a deflection of crack propagation appeared. The crack first propagated along the steel/Fe1.8Al7.2Si interface and then moved along the weld seam until the failure of the joint. The tensile strength of the joint was 146.5 MPa. Some micro-cracks were detected at Fe(Al,Si)3 and the interface between the steel substrate and Fe(Al,Si)3 in the top region while the interface was still connected.

One-Pot Synthesis of Multifunctional Polymers by Light-Controlled Radical Polymerization and Enzymatic Catalysis with Candida antarctica Lipase B.

PubMed

Hrsic, Emin; Keul, Helmut; Möller, Martin

2015-12-01

The preparation of multifunctional polymers and block copolymers by a straightforward one-pot reaction process that combines enzymatic transacylation with light-controlled polymerization is described. Functional methacrylate monomers are synthesized by enzymatic transacylation and used in situ for light-controlled polymerization, leading to multifunctional methacrylate-based polymers with well-defined microstructure. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Molybdenum disilicide composites

DOEpatents

Rodriguez, Robert P.; Petrovic, John J.

2001-01-01

Molybdenum disilicide/.beta.'-Si.sub.6-z Al.sub.z O.sub.z N.sub.8-z, wherein z=a number from greater than 0 to about 5, composites are made by use of in situ reactions among .alpha.-silicon nitride, molybdenum disilicide, and aluminum. Molybdenum disilicide within a molybdenum disilicide/.beta.'-Si.sub.6-z Al.sub.z O.sub.z N.sub.8-z eutectoid matrix is the resulting microstructure when the invention method is employed.

Experimental input for the design of metallic glass/crystalline composites

NASA Astrophysics Data System (ADS)

Hutchinson, Nicholas Willis

Bulk metallic glasses often exhibit exceptional strength and large elastic strains, but the structural applications of bulk metallic glasses are limited by their extremely low tensile ductility. Below the glass transition temperature of the alloy, plastic deformation occurs primarily in narrow shear bands, which propagate unimpeded through the monolithic glass structure, resulting in catastrophic failure under tensile loading. A number of studies have added crystalline reinforcements to the glassy matrix in an effort to block shear band propagation and increase ductility. The reinforcements in these bulk metallic glass matrix composites (BMGMC's) can be added as ex situ particles or fibers infiltrated by the glass-forming liquid [1], or can be formed in situ, either via devitrification of the glass during post-processing [2] or as a second phase that precipitates from the melt during solidification [3]. The size, distribution, and mechanical properties of the reinforcement phase have significant impact on the ductility of the composite. However, surprisingly little quantitative microstructural information is available for BMGMC's, particularly those formed by precipitation from the melt. In this work, we examine two in situ BMGMC's in which a ductile crystalline phase precipitates during solidification of the melt, resulting in a complex dendritic structure embedded in a continuous glass matrix. A 3D serial sectioning process was used to image the microstructure at regular intervals by removing slices of material using a dual beam focused ion-scanning electron microscope (FIB). Due to the complex nature of the microstructure, measurements of key features were conducted using a 3D measurement method that was developed for this purpose. Experiments were also conducted to provide experimental input for the development and tuning of finite element models. Changes in the elastic modulus of the composite were evaluated over a range of stresses that encompassed the yield point of the composite. An interesting increase in the modulus was observed prior to yielding. The work is concluded with a study of the accumulation of strain within the composite microstructure during tensile loading. The strain was determined and evaluated by a digital image correlation method. [1] R. B. Dandliker, R. D. Conner, and W. L. Johnson, "Melt infiltration casting of bulk metallic-glass matrix composites," J. Mater. Res., vol. 13, no. 10, pp. 2896--2901, 1998. [2] J. Eckert, J. Das, S. Pauly, and C. Duhamel, "Mechanical Properties of Bulk Metallic Glasses and Composites," J. Mater. Res., vol. 22, no. 2, pp. 285--301, 2007. [3] D. C. Hofmann, J.-Y. Suh, A. Wiest, G. Duan, M.-L. Lind, M. D. Demetriou, and W. L. Johnson, "Designing metallic glass matrix composites with high toughness and tensile ductility.," Nature, vol. 451, no. 7182, pp. 1085--9, Feb. 2008.

X-Ray Radiographic Observation of Directional Solidification Under Microgravity: XRMON-GF Experiments on MASER12 Sounding Rocket Mission

NASA Technical Reports Server (NTRS)

Reinhart, G.; NguyenThi, H.; Bogno, A.; Billia, B.; Houltz, Y.; Loth, K.; Voss, D.; Verga, A.; dePascale, F.; Mathiesen, R. H.;

Quantification of tissue texture with photoacoustic spectrum analysis

NASA Astrophysics Data System (ADS)

Wang, Xueding; Xu, Guan; Meng, Zhuo-Xian; Lin, Jiandie; Carson, Paul

2014-05-01

Photoacoustic (PA) imaging is an emerging technology that could map the functional contrasts in deep biological tissues in high resolution by "listening" to the laser induced thermoelastic waves. Almost all of the current studies in PA imaging are focused on the intensity of the PA signals as an indication of the optical absorbance of the biological tissues. Our group has for the first time demonstrated that the frequency domain power distribution of the broadband PA signals encode the texture information within the regions-of-interest (ROI). Following the similar method of ultrasound spectral analysis (USSA), photoacoustic spectrum analysis (PASA) could evaluate the relative concentrations and, more importantly, the dimensions of microstructures of the optically absorbing materials in biological tissues, including lipid, collagen, water and hemoglobin. By providing valuable insights into tissue pathology, PASA should benefit basic research and clinical management of many diseases, and may help achieve eventual "noninvasive biopsy". In this work, taking advantage of the optical absorption contrasts contributed by lipid and hemoglobin at 1200-nm and 532-nm wavelengths respectively, we investigated the capability of PASA in identifying histological changes corresponding to fat accumulation livers through the study on ex vivo and in situ mouse models. The PA signals from the mouse livers were acquired using our PA and US dual-modality imaging system, and analyzed in the frequency domain. After quantifying the power spectrum by fitting it to a first order model, three spectral parameters, including the intercept, the midband fit and the slope, were extracted and used to differentiate fatty livers from normal livers. The comparison between the PASA parameters from the normal and the fatty livers supports our hypotheses that PASA can quantitatively identify the microstructure changes in liver tissues for differentiating normal and fatty livers.

Segmentation-free image processing and analysis of precipitate shapes in 2D and 3D

NASA Astrophysics Data System (ADS)

Bales, Ben; Pollock, Tresa; Petzold, Linda

2017-06-01

Segmentation based image analysis techniques are routinely employed for quantitative analysis of complex microstructures containing two or more phases. The primary advantage of these approaches is that spatial information on the distribution of phases is retained, enabling subjective judgements of the quality of the segmentation and subsequent analysis process. The downside is that computing micrograph segmentations with data from morphologically complex microstructures gathered with error-prone detectors is challenging and, if no special care is taken, the artifacts of the segmentation will make any subsequent analysis and conclusions uncertain. In this paper we demonstrate, using a two phase nickel-base superalloy microstructure as a model system, a new methodology for analysis of precipitate shapes using a segmentation-free approach based on the histogram of oriented gradients feature descriptor, a classic tool in image analysis. The benefits of this methodology for analysis of microstructure in two and three-dimensions are demonstrated.

Oxygen flux and dielectric response study of Mixed Ionic-Electronic Conducting (MIEC) heterogeneous functional materials

NASA Astrophysics Data System (ADS)

Rabbi, Fazle

Dense mixed ionic-electronic conducting (MIEC) membranes consisting of ionic conductive perovskite-type and/or fluorite-type oxides and high electronic conductive spinel type oxides, at elevated temperature can play a useful role in a number of energy conversion related systems including the solid oxide fuel cell (SOFC), oxygen separation and permeation membranes, partial oxidization membrane reactors for natural gas processing, high temperature electrolysis cells, and others. This study will investigate the impact of different heterogeneous characteristics of dual phase ionic and electronic conductive oxygen separation membranes on their transport mechanisms, in an attempt to develop a foundation for the rational design of such membranes. The dielectric behavior of a material can be an indicator for MIEC performance and can be incorporated into computational models of MIEC membranes in order to optimize the composition, microstructure, and ultimately predict long term membrane performance. The dielectric behavior of the MIECs can also be an indicator of the transport mechanisms and the parameters they are dependent upon. For this study we chose a dual phase MIEC oxygen separation membrane consisting of an ionic conducting phase: gadolinium doped ceria-Ce0.8 Gd0.2O2 (GDC) and an electronic conductive phase: cobalt ferrite-CoFe2O4 (CFO). The membranes were fabricated from mixtures of Nano-powder of each of the phases for different volume percentages, sintered with various temperatures and sintering time to form systematic micro-structural variations, and characterized by structural analysis (XRD), and micro-structural analysis (SEM-EDS). Performance of the membranes was tested for variable partial pressures of oxygen across the membrane at temperatures from 850°C-1060°C using a Gas Chromatography (GC) system. Permeated oxygen did not directly correlate with change in percent mixture. An intermediate mixture 60%GDC-40%CFO had the highest flux compared to the 50%GDC-50%CFO and 80%GDC-20%CFO mixtures. Material characterization suggests the emergence of a third phase contributing to the behavior. Microstructural studies suggested changes in micro-structure of a given volume fraction for different sintering temperature and sintering time. Flux variation was observed for membranes with the same constituent volume fraction but different micro-structure indicating the effects of the micro-structure on the overall oxygen permeation. To correlate the experimental flux measurement with a standard Wagner's flux equation, different microstructural characteristics were studied to incorporate them into a modified Wagner's flux equation. In-situ broadband dielectric spectroscopy measurements over a temperature range of 850°C-1060°C and frequency range of (0.1Hz-1MHz) of the operating 60%GDC-40%CFO mixture oxygen separation membranes were measured using a NOVOCONTROL dielectric spectroscopy test system. Dielectric response of the operating membrane was studied to identify the charge transfer process in the membrane. A computational model to study the dielectric impedance response of different microstructure was developed using a COMSOL(TM) Multiphysics qasi-static electromagnetic module. This model was validated using model materials with regular geometric shapes. To measure impedance of real micro/nano-structures of the membrane material, domains required for the COMSOL calculation were obtained from actual micro/nano structures by using 3D scans from X-ray nano and micro tomography. Simpleware(TM) software was used to generate 3D domains from image slices obtained from the 3D x-ray scans. Initial voltage distributions on the original microstructure were obtained from the computational model. Similarly, development of a primary model for simulating ionic/electronic species flow inside of an MIEC was also begun. The possibility of using broadband dielectric spectroscopy methods to understand and anticipate the flux capabilities of MIECs to reduce the cost and time of development of such material systems was explored.

Factors affecting the microstructure and mechanical properties of Ti-Al3Ti core-shell-structured particle-reinforced Al matrix composites

NASA Astrophysics Data System (ADS)

Guo, Baisong; Yi, Jianhong; Ni, Song; Shen, Rujuan; Song, Min

2016-04-01

This work studied the effects of matrix powder and sintering temperature on the microstructure and mechanical properties of in situ formed Ti-Al3Ti core-shell-structured particle-reinforced pure Al-based composites. It has been shown that both factors have significant effects on the morphology of the reinforcements and densification behaviour of the composites. Due to the strong interfacial bonding and the limitation of the crack propagation in the intermetallic shell during deformation by soft Al matrix and Ti core, the composite fabricated using fine spherical-shaped Al powder and sintered at 570 °C for 5 h has the optimal combination of the overall mechanical properties. The study provides a direction for the optimum combination of high strength and ductility of the composites by adjusting the fabrication parameters.

Analysis of in-service failures and advances in microstructural characterization. Microstructural science Volume 26

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

Abramovici, E.; Northwood, D.O.; Shehata, M.T.

1999-01-01

The contents include Analysis of In-Service Failures (tutorials, transportation industry, corrosion and materials degradation, electronic and advanced materials); 1998 Sorby Award Lecture by Kay Geels, Struers A/S (Metallographic Preparation from Sorby to the Present); Advances in Microstructural Characterization (characterization techniques using high resolution and focused ion beam, characterization of microstructural clustering and correlation with performance); Advanced Applications (advanced alloys and intermetallic compounds, plasma spray coatings and other surface coatings, corrosion, and materials degradation).

Lead-germanium ohmic contact on to gallium arsenide formed by the solid phase epitaxy of germanium: A microstructure study

NASA Astrophysics Data System (ADS)

Radulescu, Fabian

2000-12-01

Driven by the remarkable growth in the telecommunication market, the demand for more complex GaAs circuitry continued to increase in the last decade. As a result, the GaAs industry is faced with new challenges in its efforts to fabricate devices with smaller dimensions that would permit higher integration levels. One of the limiting factors is the ohmic contact metallurgy of the metal semiconductor field effect transistor (MESFET), which, during annealing, induces a high degree of lateral diffusion into the substrate. Because of its limited reaction with the substrate, the Pd-Ge contact seems to be the most promising candidate to be used in the next generation of MESFET's. The Pd-Ge system belongs to a new class of ohmic contacts to compound semiconductors, part of an alloying strategy developed only recently, which relies on solid phase epitaxy (SPE) and solid phase regrowth to "un-pin" the Fermi level at the surface of the compound semiconductor. However, implementing this alloy into an integrated process flow proved to be difficult due to our incomplete understanding of the microstructure evolution during annealing and its implications on the electrical properties of the contact. The microstructure evolution and the corresponding solid state reactions that take place during annealing of the Pd-Ge thin films on to GaAs were studied in connection with their effects on the electrical properties of the ohmic contact. The phase transformations sequence, transition temperatures and activation energies were determined by combining differential scanning calorimetry (DSC) for thermal analysis with transmission electron microscopy (TEM) for microstructure identification. In-situ TEM annealing experiments on the Pd/Ge/Pd/GaAs ohmic contact system have permitted real time determination of the evolution of contact microstructure. The kinetics of the solid state reactions, which occur during ohmic contact formation, were determined by measuring the grain growth rates associated with each phase from the videotape recordings. With the exception of the Pd-GaAs interactions, it was found that four phase transformations occur during annealing of the Pd:Ge thin films on top of GaAs. The microstructural information was correlated with specific ohmic contact resistivity measurements performed in accordance with the transmission line method (TLM) and these results demonstrated that the Ge SPE growth on top of GaAs renders the optimal electrical properties for the contact. By using the focused ion beam (FIB) method to produce microcantilever beams, the residual stress present in the thin film system was studied in connection with the microstructure. Although, the PdGe/epi-Ge/GaAs seemed to be the optimal microstructural configuration, the presence of PdGe at the interface with GaAs did not damage the contact resistivity significantly. These results made it difficult to establish a charge transport mechanism across the interface but they explained the wide processing window associated with this contact.

Quantitatively characterizing microstructural variations of skin tissues during ultraviolet radiation damaging process based on Mueller matrix polarimetry

NASA Astrophysics Data System (ADS)

Sheng, Wei; He, Honghui; Dong, Yang; Ma, Hui

2018-02-01

As one of the most fundamental features of light, polarization can be used to develop imaging techniques which can provide insight into the optical and structural properties of tissues. Especially, the Mueller matrix polarimetry is suitable to detect the changes in collagen and elastic fibres, which are the main compositions of skin tissue. Here we demonstrate a novel quantitative, non-contact and in situ technique to monitor the microstructural variations of skin tissue during ultraviolet radiation (UVR) induced photoaging based on Mueller matrix polarimetry. Specifically, we measure the twodimensional (2D) backscattering Mueller matrices of nude mouse skin samples, then calculate and analyze the Mueller matrix derived parameters during the skin photoaging and self-repairing processes. To induce three-day skin photoaging, the back skin of each mouse is irradiated with UVR (0.05J/cm2) for five minutes per day. After UVR, the microstructures of the nude mouse skin are damaged. During the process of UV damage, we measure the backscattering Mueller matrices of the mouse skin samples and examine the relationship between the Mueller matrix parameters and the microstructural variations of skin tissue quantitatively. The comparisons between the UVR damaged groups with and without sunscreens show that the Mueller matrix derived parameters are potential indicators for fibrous microstructure variation in skin tissue. The pathological examinations and Monte Carlo simulations confirm the relationship between the values of Mueller matrix parameters and the changes of fibrous structures. Combined with smart phones or wearable devices, this technique may have a good application prospect in the fields of cosmetics and dermatological health.

Effect of Heat Input on the Tensile Damage Evolution in Pulsed Laser Welded Ti6Al4V Titanium Sheets

NASA Astrophysics Data System (ADS)

Liu, Jing; Gao, Xiaolong; Zhang, Jianxun

2016-11-01

The present paper is focused on studying the effect of heat input on the tensile damage evolution of pulsed Nd:YAG laser welding of Ti6Al4V alloy under monotonic loading. To analyze the reasons that the tensile fracture site of the pulsed-laser-welded Ti6Al4V sheet joints changes with the heat input under monotonic loading, the microstructure of the sample with different nominal strain values was investigated by in situ observation. Experiment results show that the tensile ductility and fatigue life of welded joints with low heat input are higher than that of welded joints with high heat input. Under tensile loads, the critical engineering strain for crack initiation is much lower in the welded joint with high heat input than in the welded joints with low and medium heat input. And the microstructural damage accumulation is much faster in the fusion zone than in the base metal for the welded joints with high input, whereas the microstructural damage accumulation is much faster in the base metal than in the fusion zone for the welded joints with low input. Consequently, the welded joints fractured in the fusion zone for the welds with high heat input, whereas the welded joints ruptured in the base metal for the welds with low heat input. It is proved that the fine grain microstructure produced by low heat input can improve the critical nominal strain for crack initiation and the resistance ability of microstructural damage.

High-temperature tensile cell for in situ real-time investigation of carbon fibre carbonization and graphitization processes

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

Behr, Michael; Rix, James; Landes, Brian

2016-10-17

A new high-temperature fibre tensile cell is described, developed for use at the Advanced Photon Source at Argonne National Laboratory to enable the investigation of the carbonization and graphitization processes during carbon fibre production. This cell is used to heat precursor fibre bundles to temperatures up to ~2300°C in a controlled inert atmosphere, while applying tensile stress to facilitate formation of highly oriented graphitic microstructure; evolution of the microstructure as a function of temperature and time during the carbonization and higher-temperature graphitization processes can then be monitored by collecting real-time wide-angle X-ray diffraction (WAXD) patterns. As an example, the carbonizationmore » and graphitization behaviour of an oxidized polyacrylonitrile fibre was studied up to a temperature of ~1750°C. Real-time WAXD revealed the gradual increase in microstructure alignment with the fibre axis with increasing temperature over the temperature range 600–1100°C. Above 1100°C, no further changes in orientation were observed. The overall magnitude of change increased with increasing applied tensile stress during carbonization. As a second example, the high-temperature graphitizability of PAN- and pitch-derived commercial carbon fibres was studied. Here, the magnitude of graphitic microstructure evolution of the pitch-derived fibre far exceeded that of the PAN-derived fibres at temperatures up to ~2300°C, indicating its facile graphitizability.« less

Phase-contrast x-ray imaging of microstructure and fatigue-crack propagation in single-crystal nickel-base superalloys

NASA Astrophysics Data System (ADS)

Husseini, Naji Sami

Single-crystal nickel-base superalloys are ubiquitous in demanding turbine-blade applications, and they owe their remarkable resilience to their dendritic, hierarchical microstructure and complex composition. During normal operations, they endure rapid low-stress vibrations that may initiate fatigue cracks. This failure mode in the very high-cycle regime is poorly understood, in part due to inadequate testing and diagnostic equipment. Phase-contrast imaging with coherent synchrotron x rays, however, is an emergent technique ideally suited for dynamic processes such as crack initiation and propagation. A specially designed portable ultrasonic-fatigue apparatus, coupled with x-ray radiography, allows real-time, in situ imaging while simulating service conditions. Three contrast mechanisms - absorption, diffraction, and phase contrast - span the immense breadth of microstructural features in superalloys. Absorption contrast is sensitive to composition and crack displacements, and diffraction contrast illuminates dislocation aggregates and crystallographic misorientations. Phase contrast enhances electron-density gradients and is particularly useful for fatigue-crack studies, sensitive to internal crack tips and openings less than one micrometer. Superalloy samples were imaged without external stresses to study microstructure and mosaicity. Maps of rhenium and tungsten concentrations revealed strong segregation to the center of dendrites, as manifested by absorption contrast. Though nominally single crystals, dendrites were misoriented from the bulk by a few degrees, as revealed by diffraction contrast. For dynamic studies of cyclic fatigue, superalloys were mounted in the portable ultrasonic-fatigue apparatus, subjected to a mean tensile stress of ˜50-150 MPa, and cycled in tension to initiate and propagate fatigue cracks. Radiographs were recorded every thousand cycles over the multimillion-cycle lifetime to measure micron-scale crack growth. Crack openings were very small, as determined by absorption and phase contrast, and suggested multiple fracture modes for propagation along {111} planes at room temperature, which was verified by finite element analysis. With increasing temperature, cracks became Mode I (perpendicular to the loading axis) in character and more sensitive to the microstructure. Advancing plastic zones ahead of crack tips altered the crystallographic quality, from which diffraction contrast anticipated initiation and propagation. These studies demonstrate the extreme sensitivity of x-ray radiography for detailed studies of superalloys and crack growth processes.

Investigation of a Novel NDE Method for Monitoring Thermomechanical Damage and Microstructure Evolution in Ferritic-Martensitic Steels for Generation IV Nuclear Energy Systems

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

Nagy, Peter

2013-09-30

The main goal of the proposed project is the development of validated nondestructive evaluation (NDE) techniques for in situ monitoring of ferritic-martensitic steels like Grade 91 9Cr-1Mo, which are candidate materials for Generation IV nuclear energy structural components operating at temperatures up to ~650{degree}C and for steam-generator tubing for sodium-cooled fast reactors. Full assessment of thermomechanical damage requires a clear separation between thermally activated microstructural evolution and creep damage caused by simultaneous mechanical stress. Creep damage can be classified as "negligible" creep without significant plastic strain and "ordinary" creep of the primary, secondary, and tertiary kind that is accompanied bymore » significant plastic deformation and/or cavity nucleation and growth. Under negligible creep conditions of interest in this project, minimal or no plastic strain occurs, and the accumulation of creep damage does not significantly reduce the fatigue life of a structural component so that low-temperature design rules, such as the ASME Section III, Subsection NB, can be applied with confidence. The proposed research project will utilize a multifaceted approach in which the feasibility of electrical conductivity and thermo-electric monitoring methods is researched and coupled with detailed post-thermal/creep exposure characterization of microstructural changes and damage processes using state-of-the-art electron microscopy techniques, with the aim of establishing the most effective nondestructive materials evaluation technique for particular degradation modes in high-temperature alloys that are candidates for use in the Next Generation Nuclear Plant (NGNP) as well as providing the necessary mechanism-based underpinnings for relating the two. Only techniques suitable for practical application in situ will be considered. As the project evolves and results accumulate, we will also study the use of this technique for monitoring other GEN IV materials. Through the results obtained from this integrated materials behavior and NDE study, new insight will be gained into the best nondestructive creep and microstructure monitoring methods for the particular mechanisms identified in these materials. The proposed project includes collaboration with a national laboratory partner and the results will also serve as a foundation to guide the efforts of scientists in the DOE laboratory, university, and industrial communities concerned with the technological challenges of monitoring creep and microstructural evolution in materials planned to be used in Generation IV Nuclear Energy Systems.« less

3D/4D analyses of damage and fracture behaviours in structural materials via synchrotron X-ray tomography.

PubMed

Toda, Hiroyuki

2014-11-01

X-ray microtomography has been utilized for the in-situ observation of various structural metals under external loading. Recent advances in X-ray microtomography provide remarkable tools to image the interior of materials. In-situ X-ray microtomography provides a unique possibility to access the 3D character of internal microstructure and its time evolution behaviours non-destructively, thereby enabling advanced techniques for measuring local strain distribution. Local strain mapping is readily enabled by processing such high-resolution tomographic images either by the particle tracking technique or the digital image correlation technique [1]. Procedures for tracking microstructural features which have been developed by the authors [2], have been applied to analyse localised deformation and damage evolution in a material [3]. Typically several tens of thousands of microstructural features, such as particles and pores, are tracked in a tomographic specimen (0.2 - 0.3 mm(3) in volume). When a sufficient number of microstructural features is dispersed in 3D space, the Delaunay tessellation algorithm is used to obtain local strain distribution. With these techniques, 3D strain fields can be measured with reasonable accuracy. Even local crack driving forces, such as local variations in the stress intensity factor, crack tip opening displacement and J integral along a crack front line, can be measured from discrete crack tip displacement fields [4]. In the present presentation, complicated crack initiation and growth behaviour and the extensive formation of micro cracks ahead of a crack tip are introduced as examples.A novel experimental method has recently been developed by amalgamating a pencil beam X-Ray diffraction (XRD) technique with the microstructural tracking technique [5]. The technique provides information about individual grain orientations and 1-micron-level grain morphologies in 3D together with high-density local strain mapping. The application of this technique to the deformation behavior of a polycrystalline aluminium alloy will be demonstrated in the presentation [6].The synchrotron-based microtomography has been mainly utilized to light materials due to their good X-ray transmission. In the present talk, the application of the synchrotron-based microtomography to steels will be also introduced. Degradation of contrast and spatial resolution due to forward scattering could be avoided by selecting appropriate experimental conditions in order to obtain superior spatial resolution close to the physical limit even in ferrous materials [7]. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

In Situ Production of Hard Metal Matrix Composite Coating on Engineered Surfaces Using Laser Cladding Technique

NASA Astrophysics Data System (ADS)

Raza, Mohammad Shahid; Hussain, Manowar; Kumar, Vikash; Das, Alok Kumar

2017-01-01

The growing need for high wear-resistant surface with enhanced physical properties has led to extensive researches in the field of surface engineering. Laser cladding emerged to be a promising method to achieve these objectives in a cost-effective way. The present paper studies the viability of cladding of tungsten disulfide (WS2) powder by using 400 W continuous-wave fiber laser. WS2 was used as a coating material, which was decomposed at higher temperature and underwent several chemical reactions. By this process, in situ formation of metal matrix composites and hard face coating on the substrate surface were attained. The characterization of laser cladded surface was done to study its morphological, microstructural, mechanical and tribological properties. It was observed that cladding of WS2 powder on 304 SS resulted in the formation of Cr-W-C-Fe metal matrix composite having improved mechanical and tribological properties. The value of microhardness of the coated surface was found to increase three to four times in comparison with the parent material surface. Wear test results indicated a decrease in wear by 1/9th (maximum) as compared to the parent 304 SS surface. The volume fractions of tungsten particles on the cladded surface were also investigated through EDS analysis.

High temperature microstructural stability and recrystallization mechanisms in 14YWT alloys

DOE PAGES

Aydogan, E.; El-Atwani, O.; Takajo, S.; ...

2018-02-09

In-situ neutron diffraction experiments were performed on room temperature compressed 14YWT nanostructured ferritic alloys at 1100°C and 1150°C to understand their thermally activated static recrystallization mechanisms. The existence of high density of Y-Ti-O rich nano-oxides (<5 nm) shift the recrystallization temperature up due to Zener pinning of the grain boundaries, making these materials attractive for high temperature applications. This study serves to quantify the texture evolution in-situ and understand the effect of particles on the recrystallization mechanisms in 14YWT alloys. We have shown, both experimentally and theoretically, that there is considerable recovery in the 20% compressed sample after 6.5 hmore » annealing at 1100°C while recrystallization occurs within an hour of annealing at 1100°C and 1150°C in the 60% compressed samples. Moreover, the 60% compressed samples show {112}<110> and {112}<111> texture components during annealing, in contrast to the conventional recrystallization textures in body centered cubic alloys. Furthermore, nano-oxide size, shape, density and distribution are considerably different in unrecrystallized and abnormally grown grains. Transmission electron microscopy analysis shows that oxide particles having a size between 5 and 30 nm play a critical role for recrystallization mechanisms in 14YWT nanostructured ferritic alloys.« less

High temperature annealing of ion irradiated tungsten

DOE PAGES

Ferroni, Francesco; Yi, Xiaoou; Arakawa, Kazuto; ...

2015-03-21

In this study, transmission electron microscopy of high temperature annealing of pure tungsten irradiated by self-ions was conducted to elucidate microstructural and defect evolution in temperature ranges relevant to fusion reactor applications (500–1200°C). Bulk isochronal and isothermal annealing of ion irradiated pure tungsten (2 MeV W + ions, 500°C, 1014 W +/cm 2) with temperatures of 800, 950, 1100 and 1400°C, from 0.5 to 8 h, was followed by ex situ characterization of defect size, number density, Burgers vector and nature. Loops with diameters larger than 2–3 nm were considered for detailed analysis, among which all loops had View themore » MathML source and were predominantly of interstitial nature. In situ annealing experiments from 300 up to 1200°C were also carried out, including dynamic temperature ramp-ups. These confirmed an acceleration of loop loss above 900°C. At different temperatures within this range, dislocations exhibited behaviour such as initial isolated loop hopping followed by large-scale rearrangements into loop chains, coalescence and finally line–loop interactions and widespread absorption by free-surfaces at increasing temperatures. An activation energy for the annealing of dislocation length was obtained, finding E a=1.34±0.2 eV for the 700–1100°C range.« less

High temperature microstructural stability and recrystallization mechanisms in 14YWT alloys

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

Aydogan, E.; El-Atwani, O.; Takajo, S.

In-situ neutron diffraction experiments were performed on room temperature compressed 14YWT nanostructured ferritic alloys at 1100°C and 1150°C to understand their thermally activated static recrystallization mechanisms. The existence of high density of Y-Ti-O rich nano-oxides (<5 nm) shift the recrystallization temperature up due to Zener pinning of the grain boundaries, making these materials attractive for high temperature applications. This study serves to quantify the texture evolution in-situ and understand the effect of particles on the recrystallization mechanisms in 14YWT alloys. We have shown, both experimentally and theoretically, that there is considerable recovery in the 20% compressed sample after 6.5 hmore » annealing at 1100°C while recrystallization occurs within an hour of annealing at 1100°C and 1150°C in the 60% compressed samples. Moreover, the 60% compressed samples show {112}<110> and {112}<111> texture components during annealing, in contrast to the conventional recrystallization textures in body centered cubic alloys. Furthermore, nano-oxide size, shape, density and distribution are considerably different in unrecrystallized and abnormally grown grains. Transmission electron microscopy analysis shows that oxide particles having a size between 5 and 30 nm play a critical role for recrystallization mechanisms in 14YWT nanostructured ferritic alloys.« less

Direct Observation of the Thickness-Induced Crystallization and Stress Build-Up during Sputter-Deposition of Nanoscale Silicide Films.

PubMed

Krause, Bärbel; Abadias, Gregory; Michel, Anny; Wochner, Peter; Ibrahimkutty, Shyjumon; Baumbach, Tilo

2016-12-21

The kinetics of phase transitions during formation of small-scale systems are essential for many applications. However, their experimental observation remains challenging, making it difficult to elucidate the underlying fundamental mechanisms. Here, we combine in situ and real-time synchrotron X-ray diffraction (XRD) and X-ray reflectivity (XRR) experiments with substrate curvature measurements during deposition of nanoscale Mo and Mo 1-x Si x films on amorphous Si (a-Si). The simultaneous measurements provide direct evidence of a spontaneous, thickness-dependent amorphous-to-crystalline (a-c) phase transition, associated with tensile stress build-up and surface roughening. This phase transformation is thermodynamically driven, the metastable amorphous layer being initially stabilized by the contributions of surface and interface energies. A quantitative analysis of the XRD data, complemented by simulations of the transformation kinetics, unveils an interface-controlled crystallization process. This a-c phase transition is also dominating the stress evolution. While stress build-up can significantly limit the performance of devices based on nanostructures and thin films, it can also trigger the formation of these structures. The simultaneous in situ access to the stress signal itself, and to its microstructural origins during structure formation, opens new design routes for tailoring nanoscale devices.

Microstructural Evolution and Phase Formation in Rapidly Solidified Ni-25.3 At. Pct Si Alloy

NASA Astrophysics Data System (ADS)

Cao, Leigang; Cochrane, Robert F.; Mullis, Andrew M.

2015-10-01

The drop-tube technique was used to solidify droplets of the Ni-25.3 at. pct Si alloy at high cooling rates. XRD, SEM, and TEM analysis revealed that the metastable phase, Ni25Si9, formed as the dominant phase in all ranges of the droplets, with γ-Ni31Si12 and β 1-Ni3Si also being present. Three different microstructures were observed: the regular and anomalous eutectic structures and near single-phase structure containing small inclusions of a second phase, termed here as heteroclite structure. Both eutectic structures comprise alternating lamellae of Ni25Si9 and β 1-Ni3Si, which, we conjecture, is a consequence of an unobserved eutectic reaction between the Ni25Si9 and β 1-Ni3Si phases. The matrix of the heteroclite structure is also identified as the metastable phase Ni25Si9, in which twined growth is observed in the TEM. As the cooling rate is increased (particle size decreased), the proportion of droplets displaying the entire heteroclite structure tends to increase, with its fraction increasing from 13.91 pct (300 to 500 µm) to 40.10 pct (75 to 106 µm). The thermodynamic properties of the Ni25Si9 phase were also studied by in-situ heating during XRD analysis and by DTA. This showed the decomposition of Ni25Si9 to β 1 and γ-Ni31Si12 for temperatures in excess of 790 K (517 °C).

Combustion synthesis of advanced materials. [using in-situ infiltration technique

NASA Technical Reports Server (NTRS)

Moore, J. J.; Feng, H. J.; Perkins, N.; Readey, D. W.

1992-01-01

The combustion synthesis of ceramic-metal composites using an in-situ liquid infiltration technique is described. The effect of varying the reactants and their stoichiometry to provide a range of reactant and product species i.e. solids, liquids and gases, with varying physical properties e.g. thermal conductivity, on the microstructure and morphology of synthesized products is also described. Alternatively, conducting the combustion synthesis reaction in a reactive gas environment is also discussed, in which advantages can be gained from the synergistic effects of combustion synthesis and vapor phase transport. In each case, the effect of the presence or absence of gravity (density) driven fluid flow and vapor transport is discussed as is the potential for producing new and perhaps unique materials by conducting these SHS reactions under microgravity conditions.

Mechanism of the α -ɛ phase transformation in iron

NASA Astrophysics Data System (ADS)

Dewaele, A.; Denoual, C.; Anzellini, S.; Occelli, F.; Mezouar, M.; Cordier, P.; Merkel, S.; Véron, M.; Rausch, E.

2015-05-01

The α -Fe↔ɛ -Fe pressure-induced transformation under pure hydrostatic static compression has been characterized with in situ x-ray diffraction using α -Fe single crystals as starting samples. The forward transition starts at 14.9 GPa, and the reverse at 12 GPa, with a width of α -ɛ coexistence domain of the order of 2 GPa. The elastic stress in the sample increases in this domain, and partially relaxes after completion of the transformation. Orientation relations between parent α -Fe and child ɛ -Fe have been determined, which definitely validates the Burgers path for the direct transition. On the reverse transition, an unexpected variant selection is observed. X-ray diffraction data, complemented with ex situ microstructural observations, suggest that this selection is caused by defects and stresses accumulated during the direct transition.

In Situ Elevated Temperature Testing of Fly Ash Based Geopolymer Composites.

PubMed

Vickers, Les; Pan, Zhu; Tao, Zhong; van Riessen, Arie

2016-06-03

In situ elevated temperature investigations using fly ash based geopolymers filled with alumina aggregate were undertaken. Compressive strength and short term creep tests were carried out to determine the onset temperature of viscous flow. Fire testing using the standard cellulose curve was performed. Applying a load to the specimen as the temperature increased reduced the temperature at which viscous flow occurred (compared to test methods with no applied stress). Compressive strength increased at the elevated temperature and is attributed to viscous flow and sintering forming a more compact microstructure. The addition of alumina aggregate and reduction of water content reduced the thermal conductivity. This led to the earlier onset and shorter dehydration plateau duration times. However, crack formation was reduced and is attributed to smaller thermal gradients across the fire test specimen.

Effect of in situ exopolysaccharide production on physicochemical, rheological, sensory, and microstructural properties of the yogurt drink ayran: an optimization study based on fermentation kinetics.

PubMed

Yilmaz, M T; Dertli, E; Toker, O S; Tatlisu, N B; Sagdic, O; Arici, M

2015-03-01

Exopolysaccharide (EPS)-producing starter cultures are preferred for the manufacture of fermented milk products to improve rheological and technological properties. However, no clear correlation exists between EPS production and the rheological and technological properties of fermented milk products such as the yogurt drink ayran. In this study, 4 different strain conditions (EPS- and EPS+ Streptococcus thermophilus strains) were tested as a function of incubation temperature (32, 37, or 42°C) and time (2, 3, or 4 h) to determine the effect of culture type and in situ EPS production on physicochemical, rheological, sensory, and microstructural properties of ayran. Furthermore, we assessed the effect of fermentation conditions on amounts of EPS production by different EPS-producing strains during ayran production. A multifactorial design of response surface methodology was used to model linear, interaction, and quadratic effects of these variables on steady shear rheological properties of ayran samples and in situ EPS production levels. The physicochemical and microbiological characteristics of ayran samples altered depending on incubation conditions and strain selection. Steady shear tests showed that ayran samples inoculated with EPS+ strains exhibited pseudoplastic flow behavior. Production of ayran with EPS- strain (control sample) resulted in the lowest apparent viscosity values (η50), whereas those produced with the combination of 2 EPS+ strains yielded ayran with notably increased η50 values. We concluded that incubation time was the variable with the greatest effect on η50, consistency coefficient (K), and flow behavior index (n) values. In situ EPS production was also affected by these conditions during ayran fermentation in which strain-specific metabolism conditions were found to be the most important factor for EPS production. In addition, these findings correlated the amount of in situ EPS produced with the rheological properties of ayran. Scanning electron microscopy images of the samples showed differences in structural features, revealing a prominent network strand structure in the ayran samples inoculated with the admixture of 2 EPS-producing strains incubated at 37°C for 3 h. These results provide useful information for large-scale production of ayran by the dairy industry. Copyright © 2015 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

EBSD Analysis of Relationship Between Microstructural Features and Toughness of a Medium-Carbon Quenching and Partitioning Bainitic Steel

NASA Astrophysics Data System (ADS)

Li, Qiangguo; Huang, Xuefei; Huang, Weigang

2017-12-01

A multiphase microstructure of bainite, martensite and retained austenite in a 0.3C bainitic steel was obtained by a novel bainite isothermal transformation plus quenching and partitioning (B-QP) process. The correlations between microstructural features and toughness were investigated by electron backscatter diffraction (EBSD), and the results showed that the multiphase microstructure containing approximately 50% bainite exhibits higher strength (1617 MPa), greater elongation (18.6%) and greater impact toughness (103 J) than the full martensite. The EBSD analysis indicated that the multiphase microstructure with a smaller average local misorientation (1.22°) has a lower inner stress concentration possibility and that the first formed bainitic ferrite plates in the multiphase microstructure can refine subsequently generated packets and blocks. The corresponding packet and block average size decrease from 11.9 and 2.3 to 8.4 and 1.6 μm, respectively. A boundary misorientation analysis indicated that the multiphase microstructure has a higher percentage of high-angle boundaries (67.1%) than the full martensite (57.9%) because of the larger numbers and smaller sizes of packets and blocks. The packet boundary obstructs crack propagation more effectively than the block boundary.

IMEC-9: The 9th Israel Materials Engineering Conference. Program & Abstracts

DTIC Science & Technology

1999-12-07

non- toxic , magnetite (FesC^) nanoparticles of very narrow size distribution in sizes ranging from approximately 20 nm up to 0.1 urn. The process for...Israel 17 Composites I Hall G Chair: R. Albalak 13:30 -13:50 Synthesis of Dense Oxide -Based In Situ Composites via Thermal Explosion/SHS...Tsionsky, Israel 16:00 -16:20 The Effect of Composition and Microstructure on the Corrosion Behavior of Magnesium- Aluminium Alloys P. Uzan, D. Eliezer

Numerical simulation of dendrite growth in nickel-based superalloy and validated by in-situ observation using high temperature confocal laser scanning microscopy

NASA Astrophysics Data System (ADS)

Yan, Xuewei; Xu, Qingyan; Liu, Baicheng

2017-12-01

Dendritic structures are the predominant microstructural constituents of nickel-based superalloys, an understanding of the dendrite growth is required in order to obtain the desirable microstructure and improve the performance of castings. For this reason, numerical simulation method and an in-situ observation technology by employing high temperature confocal laser scanning microscopy (HT-CLSM) were used to investigate dendrite growth during solidification process. A combined cellular automaton-finite difference (CA-FD) model allowing for the prediction of dendrite growth of binary alloys was developed. The algorithm of cells capture was modified, and a deterministic cellular automaton (DCA) model was proposed to describe neighborhood tracking. The dendrite and detail morphology, especially hundreds of dendrites distribution at a large scale and three-dimensional (3-D) polycrystalline growth, were successfully simulated based on this model. The dendritic morphologies of samples before and after HT-CLSM were both observed by optical microscope (OM) and scanning electron microscope (SEM). The experimental observations presented a reasonable agreement with the simulation results. It was also found that primary or secondary dendrite arm spacing, and segregation pattern were significantly influenced by dendrite growth. Furthermore, the directional solidification (DS) dendritic evolution behavior and detail morphology were also simulated based on the proposed model, and the simulation results also agree well with experimental results.

Development of in-Situ Al-Si/CuAl₂ Metal Matrix Composites: Microstructure, Hardness, and Wear Behavior.

PubMed

Tash, Mahmoud M; Mahmoud, Essam R I

2016-06-02

In the present work, in-situ metal matrix composites were fabricated through squeeze casting. The copper particles were dispersed with different weight percentages (3%, 6%, 10%, and 15%) into Al-12% Si piston alloy. Also, heat treatments were performed at 380 °C and 450 °C for holding times of 6 and 18 h. The microstructures, X-ray diffractometer (XRD) pattern, hardness, and wear characteristics were evaluated. The results showed that these copper particles have reacted with the aluminum under all of the aforementioned processing conditions resulting in the formation of fine copper aluminide intermetallics. Most of the intermetallics were CuAl₂, while AlCu appeared in a small ratio. Additionally, these intermetallics were homogenously distributed within the alloy matrix with up to 6% Cu addition. The amounts of those intermetallics increased after performing heat treatment. Most of these intermetallics were CuAl₂ at 380 °C, while the Cu-rich intermetallics appeared at 450 °C. Increasing the holding time to 18 h, however, led to grain coarsening and resulted in the formation of some cracks. The hardness of the resulting composite materials was improved. The hardness value reached to about 170 HV after heat treating at 380 °C for 8 h. The wear resistance of the resulting composite materials was remarkably improved, especially at lower additions of Cu and at the lower heat treatment temperature.

Modelling deformation and fracture in confectionery wafers

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

Mohammed, Idris K.; Charalambides, Maria N.; Williams, J. Gordon

2015-01-22

The aim of this research is to model the deformation and fracture behaviour of brittle wafers often used in chocolate confectionary products. Three point bending and compression experiments were performed on beam and circular disc samples respectively to determine the 'apparent' stress-strain curves in bending and compression. The deformation of the wafer for both these testing types was observed in-situ within an SEM. The wafer is modeled analytically and numerically as a composite material with a core which is more porous than the skins. X-ray tomography was used to generate a three dimensional volume of the wafer microstructure which wasmore » then meshed and used for quantitative analysis. A linear elastic material model, with a damage function and element deletion, was used and the XMT generated architecture was loaded in compression. The output from the FE simulations correlates closely to the load-deflection deformation observed experimentally.« less

The High Resolution Powder Diffraction Beam Line at ESRF.

PubMed

Fitch, A N

2004-01-01

The optical design and performance of the high-resolution powder diffraction beam line BM16 at ESRF are discussed and illustrated. Some recent studies carried out on BM16 are described, including crystal structure solution and refinement, anomalous scattering, in situ measurements, residual strain in engineering components, investigation of microstructure, and grazing-incidence diffraction from surface layers. The beam line is built on a bending magnet, and operates in the energy range from 5 keV to 40 keV. After the move to an undulator source in 2002, it will benefit from an extented energy range up to 60 keV and increased flux and resolution. It is anticipated that enhancements to the data quality will be achieved, leading to the solution of larger crystal structures, and improvements in the accuracy of refined structures. The systematic exploitation of anisotropic thermal expansion will help reduce the effects of peak overlap in the analysis of powder diffraction data.

Effects of helium implantation on the tensile properties and microstructure of Ni₇₃P₂₇ metallic glass nanostructures

DOE PAGES

Liontas, Rachel; Gu, X. Wendy; Fu, Engang; ...

2014-09-10

We report fabrication and nanomechanical tension experiments on as-fabricated and helium-implanted ~130 nm diameter Ni₇₃P₂₇ metallic glass nano-cylinders. The nano-cylinders were fabricated by a templated electroplating process and implanted with He⁺ at energies of 50, 100, 150, and 200 keV to create a uniform helium concentration of ~3 at. % throughout the nano-cylinders. Transmission electron microscopy (TEM) imaging and through-focus analysis reveal that the specimens contained ~2 nm helium bubbles distributed uniformly throughout the nano-cylinder volume. In-situ tensile experiments indicate that helium-implanted specimens exhibit enhanced ductility as evidenced by a 2-fold increase in plastic strain over as-fabricated specimens, with nomore » sacrifice in yield and ultimate tensile strengths. This improvement in mechanical properties suggests that metallic glasses may actually exhibit a favorable response to high levels of helium implantation.« less

In situ synthesis of hydroxyapatite coating by laser cladding.

PubMed

Wang, D G; Chen, C Z; Ma, J; Zhang, G

2008-10-15

HA bioceramic coatings were synthesized on titanium substrate by laser cladding using cheap calcium carbonate and calcium hydrogen phosphate. The thermodynamic condition for synthesizing HA was calculated by software Matlab 5.0, the microstructure and phase analysis of laser clad HA bioceramic coatings were studied by electron probe microanalyser (EPMA), X-ray diffractometer (XRD) and transmission electron microscopy (TEM). The theoretical results show that the Gibbs free enthalpy for the synthesis of HA phase is satisfied, and the presence of HA phase in the clad coatings was then further verified by XRD and the selected area diffraction patterns. When the laser power is 600W and the scanning speed is 3.5mm/s, the compact HA bioceramic coatings were obtained, which have cellular dendritic structure and consist of the phases of HA, alpha-Ca(2)P(2)O(7), CaO and CaTiO(3).

Thermal imaging of Al-CuO thermites

NASA Astrophysics Data System (ADS)

Densmore, John; Sullivan, Kyle; Kuntz, Joshua; Gash, Alex

2013-06-01

We have performed spatial in-situ temperature measurements of aluminum-copper oxide thermite reactions using high-speed color pyrometry. Electrophoretic deposition was used to create thermite microstructures. Tests were performed with micron- and nano-sized particles at different stoichiometries. The color pyrometry was performed using a high-speed color camera. The color filter array on the image sensor collects light within three spectral bands. Assuming a gray-body emission spectrum a multi-wavelength ratio analysis allows a temperature to be calculated. An advantage of using a two-dimensional image sensor is that it allows heterogeneous flames to be measured with high spatial resolution. Light from the initial combustion of the Al-CuO can be differentiated from the light created by the late time oxidization with atmosphere. This work performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

High Temperature Mechanical Behavior of MgAl2O4-YAG Eutectic Ceramic In Situ Composites by Float Zone Method

NASA Astrophysics Data System (ADS)

Abalı, Serkan

2017-09-01

The directionally solidified eutectic MgAl2O4-Y3Al5O12 crystal was prepared at a pressure of 0.4 MPa of ambient nitrogen gas by the high frequency induction heated floating zone furnace. In order to determine the high temperature characteristics, directionally solidified MgAl2O4-Y3Al5O12 eutectic phase has been analyzed with creep test, tensile strength, young modulus and fracture toughness at the various temperatures and the microstructural variations have been studied according to the analysis results. It has been seen that directionally solidified with zone melting MgAl2O4-YAG eutectic ceramic which has given the value of 168 MPa below 10-6/s strain rate at 1,700 °C temperature has revealed minimum stress.

Modelling deformation and fracture in confectionery wafers

NASA Astrophysics Data System (ADS)

Mohammed, Idris K.; Charalambides, Maria N.; Williams, J. Gordon; Rasburn, John

2015-01-01

The aim of this research is to model the deformation and fracture behaviour of brittle wafers often used in chocolate confectionary products. Three point bending and compression experiments were performed on beam and circular disc samples respectively to determine the 'apparent' stress-strain curves in bending and compression. The deformation of the wafer for both these testing types was observed in-situ within an SEM. The wafer is modeled analytically and numerically as a composite material with a core which is more porous than the skins. X-ray tomography was used to generate a three dimensional volume of the wafer microstructure which was then meshed and used for quantitative analysis. A linear elastic material model, with a damage function and element deletion, was used and the XMT generated architecture was loaded in compression. The output from the FE simulations correlates closely to the load-deflection deformation observed experimentally.

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

NASA Astrophysics Data System (ADS)

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

2006-12-01

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

Thermographic Microstructure Monitoring in Electron Beam Additive Manufacturing

PubMed Central

Raplee, J.; Plotkowski, A.; Kirka, M. M.; Dinwiddie, R.; Okello, A.; Dehoff, R. R.; Babu, S. S.

2017-01-01

To reduce the uncertainty of build performance in metal additive manufacturing, robust process monitoring systems that can detect imperfections and improve repeatability are desired. One of the most promising methods for in situ monitoring is thermographic imaging. However, there is a challenge in using this technology due to the difference in surface emittance between the metal powder and solidified part being observed that affects the accuracy of the temperature data collected. The purpose of the present study was to develop a method for properly calibrating temperature profiles from thermographic data to account for this emittance change and to determine important characteristics of the build through additional processing. The thermographic data was analyzed to identify the transition of material from metal powder to a solid as-printed part. A corrected temperature profile was then assembled for each point using calibrations for these surface conditions. Using this data, the thermal gradient and solid-liquid interface velocity were approximated and correlated to experimentally observed microstructural variation within the part. This work shows that by using a method of process monitoring, repeatability of a build could be monitored specifically in relation to microstructure control. PMID:28256595

Prediction of Thermal Transport Properties of Materials with Microstructural Complexity

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

Chen, Youping

This project aims at overcoming the major obstacle standing in the way of progress in dynamic multiscale simulation, which is the lack of a concurrent atomistic-continuum method that allows phonons, heat and defects to pass through the atomistic-continuum interface. The research has led to the development of a concurrent atomistic-continuum (CAC) methodology for multiscale simulations of materials microstructural, mechanical and thermal transport behavior. Its efficacy has been tested and demonstrated through simulations of dislocation dynamics and phonon transport coupled with microstructural evolution in a variety of materials and through providing visual evidences of the nature of phonon transport, such asmore » showing the propagation of heat pulses in single and polycrystalline solids is partially ballistic and partially diffusive. In addition to providing understanding on phonon scattering with phase interface and with grain boundaries, the research has contributed a multiscale simulation tool for understanding of the behavior of complex materials and has demonstrated the capability of the tool in simulating the dynamic, in situ experimental studies of nonequilibrium transient transport processes in material samples that are at length scales typically inaccessible by atomistically resolved methods.« less

Microstructural Features Controlling the Variability in Low-Cycle Fatigue Properties of Alloy Inconel 718DA at Intermediate Temperature

NASA Astrophysics Data System (ADS)

Texier, Damien; Gómez, Ana Casanova; Pierret, Stéphane; Franchet, Jean-Michel; Pollock, Tresa M.; Villechaise, Patrick; Cormier, Jonathan

2016-03-01

The low-cycle fatigue behavior of two direct-aged versions of the nickel-based superalloy Inconel 718 (IN718DA) was examined in the low-strain amplitude regime at intermediate temperature. High variability in fatigue life was observed, and abnormally short lifetimes were systematically observed to be due to crack initiation at (sub)-surface non-metallic inclusions. However, crack initiation within (sub)-surface non-metallic inclusions did not necessarily lead to short fatigue life. The macro- to micro-mechanical mechanisms of deformation and damage have been examined by means of detailed microstructural characterization, tensile and fatigue mechanical tests, and in situ tensile testing. The initial stages of crack micro-propagation from cracked non-metallic particles into the surrounding metallic matrix occupies a large fraction of the fatigue life and requires extensive local plastic straining in the matrix adjacent to the cracked inclusions. Differences in microstructure that influence local plastic straining, i.e., the δ-phase content and the grain size, coupled with the presence of non-metallic inclusions at the high end of the size distribution contribute strongly to the fatigue life variability.

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

MINERVA: A facility to study Microstructure and INterface Evolution in Realtime under VAcuum

NASA Astrophysics Data System (ADS)

Nicklin, Chris; Martinez-Hardigree, Josue; Warne, Adam; Green, Stephen; Burt, Martin; Naylor, John; Dorman, Adam; Wicks, Dean; Din, Salahud; Riede, Moritz

2017-10-01

A sample environment to enable real-time X-ray scattering measurements to be recorded during the growth of materials by thermal evaporation in vacuum is presented. The in situ capabilities include studying microstructure development with time or during exposure to different environmental conditions, such as temperature and gas pressure. The chamber provides internal slits and a beam stop, to reduce the background scattering from the X-rays passing through the entrance and exit windows, together with highly controllable flux rates of the evaporants. Initial experiments demonstrate some of the possibilities by monitoring the growth of bathophenanthroline (BPhen), a common molecule used in organic solar cells and organic light emitting diodes, including the development of the microstructure with time and depth within the film. The results show how BPhen nanocrystal structures coarsen at room temperature under vacuum, highlighting the importance of using real time measurements to understand the as-deposited pristine film structure and its development with time. More generally, this sample environment is versatile and can be used for investigation of structure-property relationships in a wide range of vacuum deposited materials and their applications in, for example, optoelectronic devices and energy storage.

Eclogite-facies metamorphic reactions under stress and faulting in granulites from the Bergen Arcs, Norway: an experimental investigation

NASA Astrophysics Data System (ADS)

Incel, Sarah; Hilairet, Nadège; Labrousse, Loïc; Andersen, Torgeir B.; Wang, Yanbin; Schubnel, Alexandre

2017-04-01

Field observations from the Bergen Arcs, Norway, demonstrate a network of pseudotachylites quenched under eclogite-facies conditions in mafic granulites. In these nominally anhydrous high-pressure high-temperature (HP/HT) rocks the formation of pseudotachylites, believed to represent fossilized earthquakes, cannot be explained by processes akin to dehydration embrittlement. On the contrary, the transition to eclogite is expected to involve hydration of the initial rock. To experimentally investigate the underlying mechanisms leading to brittle failure in HP/HT rocks, we performed deformation experiments on natural granulite samples from the Bergen Arcs. The experiments were conducted under eclogite-facies conditions (2-3 GPa, 990-1220 K) to trigger the breakdown of plagioclase - the main constituent of granulite. For these experiments, both a D-DIA and a Griggs apparatus were used. The D-DIA press is mounted on a synchrotron beamline, enabling us to monitor strain, stress, and phase changes in-situ while contemporaneously recording acoustic emissions. The Griggs experiments were performed on a new device installed at ENS Paris, in which only stress-strain were recorded, and post-mortem microstructures investigated. The initial material consisted of a fine grain size granulite powder (< 38 µm) composed of mainly plagioclase and minor amount of pyroxene. Hydrous phases are phlogopite and epidote group minerals that make up less than 1 vol. % of the total bulk rock powder plus the adhesion water on grain surfaces. Mechanical data together with XRD observations and the record of acoustic emissions demonstrate a correlation between stress drops, the growth of plagioclase breakdown products and the onset of acoustic emissions during deformation of our specimen within the eclogitic field. Microstructural analysis show remarkable similarities with that of the natural ecoligitic pseudotachylites of the Bergen arcs. The plagioclase decomposition products form narrow conjugated shear bands, along which dissected and displaced crystals are found in the samples. The lack of microstructural evidence for macroscopic brittle failure in our microstructures could be due to plastic overprinting of early brittle structures. Nevertheless, our preliminary experimental results show a strong correlation between strain localization, dynamic fracture propagation (rapid enough to produce AEs) and the eclogitization of granulite.

Additive manufacturing of materials: Opportunities and challenges

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

Babu, Sudarsanam Suresh; Love, Lonnie J.; Dehoff, Ryan R.

Additive manufacturing (also known as 3D printing) is considered a disruptive technology for producing components with topologically optimized complex geometries as well as functionalities that are not achievable by traditional methods. The realization of the full potential of 3D printing is stifled by a lack of computational design tools, generic material feedstocks, techniques for monitoring thermomechanical processes under in situ conditions, and especially methods for minimizing anisotropic static and dynamic properties brought about by microstructural heterogeneity. In this paper, we discuss the role of interdisciplinary research involving robotics and automation, process control, multiscale characterization of microstructure and properties, and high-performancemore » computational tools to address each of these challenges. In addition, emerging pathways to scale up additive manufacturing of structural materials to large sizes (>1 m) and higher productivities (5–20 kg/h) while maintaining mechanical performance and geometrical flexibility are also discussed.« less

Additive manufacturing of materials: Opportunities and challenges

DOE PAGES

Babu, Sudarsanam Suresh; Love, Lonnie J.; Dehoff, Ryan R.; ...

2015-11-01

Additive manufacturing (also known as 3D printing) is considered a disruptive technology for producing components with topologically optimized complex geometries as well as functionalities that are not achievable by traditional methods. The realization of the full potential of 3D printing is stifled by a lack of computational design tools, generic material feedstocks, techniques for monitoring thermomechanical processes under in situ conditions, and especially methods for minimizing anisotropic static and dynamic properties brought about by microstructural heterogeneity. In this paper, we discuss the role of interdisciplinary research involving robotics and automation, process control, multiscale characterization of microstructure and properties, and high-performancemore » computational tools to address each of these challenges. In addition, emerging pathways to scale up additive manufacturing of structural materials to large sizes (>1 m) and higher productivities (5–20 kg/h) while maintaining mechanical performance and geometrical flexibility are also discussed.« less

Intergrannular strain evolution in a zircaloy-4 alloy with Widmanstatten microstructure

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

Clausen, Bjorn; Vogel, Sven C; Garlea, Eena

2009-01-01

A Zircaloy-4 alloy with Widmanstatten-Basketweave microstructure and random texture has been used to study the deformation systems responsible for the polycrystalline plasticity at the grain level. The evolution of internal strain and bulk texture is investigated using neutron diffraction and an elasto-plastic self-consistent (EPSC) modeling scheme. The macroscopic stress-strain behavior and intergranular (hkil-specific) strain development, parallel and perpendicular to the loading direction, were measured in-situ during uniaxial tensile loading. Then, the EPSC model was employed to simulate the experimental results. This modeling scheme accounts for the thermal anisotropy; elastic-plastic properties of the constituent grains; and activation, reorientation, and stress relaxationmore » associated with twinning. The agreement between the experiment and the model will be discussed as well as the critical resolved shear stresses (CRSS) and the hardening coefficients obtained from the model.« less

Evolution of twinning in extruded AZ31 alloy with bimodal grain structure

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

Garcés, G., E-mail: ggarces@cenim.csic.es

2017-04-15

Twinning in extruded AZ31 alloy with a bimodal grain structure is studied under compression along the extrusion direction. This study has combined in-situ measurements during the compression tests by Synchrotron Radiation Diffraction and Acoustic Emission techniques and the evaluation of the microstructure and texture in post-mortem compression samples deformed at different strains. The microstructure of the alloy is characterized by the coexistence of large areas of fine dynamic recrystallized grains and coarse non-recrystallized grains elongated along extrusion direction. Twinning occurs initially in large elongated grains before the macroscopic yield stress which is controlled by the twinning in equiaxed dynamically recrystallizedmore » grains. - Highlights: • The AZ31 extruded at low temperature exhibits a bimodal grains structure. • Twinning takes place before macroscopic yielding in coarse non-DRXed grains. • DRXed grains controls the beginning of plasticity in magnesium alloys with bimodal grain structure.« less

Microstructure and Properties of Zircon-Added Carbon Refractories for Blast Furnace

NASA Astrophysics Data System (ADS)

Zhu, Tianbin; Li, Yawei; Sang, Shaobai; Chen, Xilai; Zhao, Lei; Li, Yuanbing; Li, Shujing

2012-11-01

Microstructure and properties of zircon-added carbon refractory specimens for blast furnace (BF) were investigated with the aid of X-ray diffraction (XRD), a scanning electron microscope (SEM), energy-dispersive X-ray, mercury porosimetry, and a laser thermal conductivity (TC) meter. Additives could influence the matrix structures and improve the properties of specimens. With the increase of zircon powder content, the amount of SiC whiskers formed increased and their aspect ratio became larger, and the SiC whiskers tended to be distributed homogeneously. Zircon powder additions decreased the mean pore diameter and increased <1- μm pore volume by filling in pores via SiC, improved the TC and the cold crushing strength (CCS) due to the in-situ formation of the more well-developed SiC whiskers with high TC, and significantly reduced the molten iron attack to carbon specimens.

Irradiation Creep in Graphite

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

Ubic, Rick; Butt, Darryl; Windes, William

2014-03-13

An understanding of the underlying mechanisms of irradiation creep in graphite material is required to correctly interpret experimental data, explain micromechanical modeling results, and predict whole-core behavior. This project will focus on experimental microscopic data to demonstrate the mechanism of irradiation creep. High-resolution transmission electron microscopy should be able to image both the dislocations in graphite and the irradiation-induced interstitial clusters that pin those dislocations. The team will first prepare and characterize nanoscale samples of virgin nuclear graphite in a transmission electron microscope. Additional samples will be irradiated to varying degrees at the Advanced Test Reactor (ATR) facility and similarlymore » characterized. Researchers will record microstructures and crystal defects and suggest a mechanism for irradiation creep based on the results. In addition, the purchase of a tensile holder for a transmission electron microscope will allow, for the first time, in situ observation of creep behavior on the microstructure and crystallographic defects.« less

In situ imaging of microstructure formation in electronic interconnections

PubMed Central

Salleh, M. A. A. Mohd; Gourlay, C. M.; Xian, J. W.; Belyakov, S. A.; Yasuda, H.; McDonald, S. D.; Nogita, K.

2017-01-01

The development of microstructure during melting, reactive wetting and solidification of solder pastes on Cu-plated printed circuit boards has been studied by synchrotron radiography. Using Sn-3.0Ag-0.5Cu/Cu and Sn-0.7Cu/Cu as examples, we show that the interfacial Cu6Sn5 layer is present within 0.05 s of wetting, and explore the kinetics of flux void formation at the interface between the liquid and the Cu6Sn5 layer. Quantification of the nucleation locations and anisotropic growth kinetics of primary Cu6Sn5 crystals reveals a competition between the nucleation of Cu6Sn5 in the liquid versus growth of Cu6Sn5 from the existing Cu6Sn5 layer. Direct imaging confirms that the β-Sn nucleates at/near the Cu6Sn5 layer in Sn-3.0Ag-0.5Cu/Cu joints. PMID:28079120

Magnetite-hematite transformation: correlation between natural and synthetic features

NASA Astrophysics Data System (ADS)

Barbosa, Paola F.; Lagoeiro, Leonardo; Scholz, Ricardo; Graça, Leonardo M.; Mohallem, Nelcy

2015-06-01

The iron-oxide system can be used as a marker of oxidized and reduced conditions in closed systems. However, natural rocks with iron oxide minerals also exhibit such reactions, although the natural system is typically open. To understand the behaviour of this natural system, some similarities were investigated, in terms of crystallographic textures, between the microstructures of two systems: natural open system and synthetic closed system of iron oxide phase transformation. Particular cases of phase transformation in iron oxide minerals, described as natural reactions of magnetite to hematite and synthetic reactions of hematite to magnetite, were chosen. It is observed, in both scenarios, that the transformation obeys the topotaxial and epitaxial relationship, which are well described for the iron oxide system. However, in natural open systems, the precipitation of a new phase during the in situ transformation modifies the microstructures and must be taken into account as an important factor to describe them.

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

Chang, L. L.; Wang, Y. D.; Ren, Y.

Microstructure evolution, mechanical behaviors of cold rolled Ti-Nb alloys with different Nb contents subjected to different heat treatments were investigated. Here, optical microstructure and phase compositions of Ti-Nb alloys were characterized using optical microscopy and X-ray diffractometre, while mechanical behaviors of Ti-Nb alloys were examined by using tension tests. Stress-induced martensitic transformation in a Ti-30. at%Nb binary alloy was in-situ explored by synchrotron-based high-energy X-ray diffraction (HE-XRD). The results obtained suggested that mechanical behavior of Ti-Nb alloys, especially Young's modulus was directly dependent on chemical compositions and heat treatment process. According to the results of HE-XRD, α"-V1 martensite generated priormore » to the formation of α"-V2 during loading and a partial reversible transformation from α"-V1 to β phase was detected while α"-V2 tranformed to β completely during unloading.« less

Transmission Electron Microscope In Situ Straining Technique to Directly Observe Defects and Interfaces During Deformation in Magnesium

DOE PAGES

Morrow, Benjamin M.; Cerreta, E. K.; McCabe, R. J.; ...

2015-05-14

In-situ straining was used to study deformation behavior of hexagonal close-packed (hcp) metals.Twinning and dislocation motion, both essential to plasticity in hcp materials, were observed.Typically, these processes are characterized post-mortem by examining remnant microstructural features after straining has occurred. By imposing deformation during imaging, direct observation of active deformation mechanisms is possible. This work focuses on straining of structural metals in a transmission electron microscope (TEM), and a recently developed technique that utilizes familiar procedures and equipment to increase ease of experiments. In-situ straining in a TEM presents several advantages over conventional post-mortem characterization, most notably time-resolution of deformation andmore » streamlined identification of active deformation mechanisms. Drawbacks to the technique and applicability to other studies are also addressed. In-situ straining is used to study twin boundary motion in hcp magnesium. A {101¯2} twin was observed during tensile and compressive loading. Twin-dislocation interactions are directly observed. Notably, dislocations are observed to remain mobile, even after multiple interactions with twin boundaries, a result which suggests that Basinki’s dislocation transformation mechanism by twinning is not present in hcp metals. The coupling of in-situ straining with traditional post-mortem characterization yields more detailed information about material behavior during deformation than either technique alone.« less

MR-based trabecular bone microstructure is not altered in subjects with indolent systemic mastocytosis.

PubMed

Baum, Thomas; Karampinos, Dimitrios C; Brockow, Knut; Seifert-Klauss, Vanadin; Jungmann, Pia M; Biedermann, Tilo; Rummeny, Ernst J; Bauer, Jan S; Müller, Dirk

2015-01-01

Subjects with indolent systemic mastocytosis (ISM) have an increased risk for osteoporosis. It has been demonstrated that trabecular bone microstructure analysis improves the prediction of bone strength beyond dual-energy X-ray absorptiometry-based bone mineral density. The purpose of this study was to obtain Magnetic Resonance (MR)-based trabecular bone microstructure parameters as advanced imaging biomarkers in subjects with ISM (n=18) and compare them with those of normal controls (n=18). Trabecular bone microstructure parameters were not significantly (P>.05) different between subjects with ISM and controls. These findings revealed important pathophysiological information about ISM-associated osteoporosis and may limit the use of trabecular bone microstructure analysis in this clinical setting. Copyright © 2015 Elsevier Inc. All rights reserved.

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.

LLNL compiled first pages ordered by ascending B&R code

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

Campbell, G; Kumar, M; Tobin, J

We aim to develop a fundamental understanding of materials dynamics (from {micro}s to ns) in systems where the required combination of spatial and temporal resolution can only be reached by the dynamic transmission electron microscope (DTEM). In this regime, the DTEM is capable of studying complex transient phenomena with several orders of magnitude time resolution advantage over any existing in-situ TEM. Using the unique in situ capabilities and the nanosecond time resolution of the DTEM, we seek to study complex transient phenomena associated with rapid processes in materials, such as active sites on nanoscale catalysts and the atomic level mechanismsmore » and microstructural features for nucleation and growth associated with phase transformations in materials, specifically in martensite formation and crystallization reactions from the amorphous phase. We also will study the transient phase evolution in rapid solid-state reactions, such as those occurring in reactive multilayer foils (RMLF). Program Impact: The LLNL DTEM possesses unique capabilities for capturing time resolved images and diffraction patterns of rapidly evolving materials microstructure under strongly driven conditions. No other instrument in the world can capture images with <10 nm spatial resolution of interesting irreversible materials processes such as phase transformations, plasticity, or morphology changes with 15 ns time resolution. The development of this innovative capability requires the continuing collaboration of laser scientists, electron microscopists, and materials scientists experienced in time resolved observations of materials that exist with particularly relevant backgrounds at LLNL. The research team has made observations of materials processes that are possible by no other method, such as the rapid crystallization of thin film NiTi that identified a change in mechanism at high heating rates as compared to isothermal anneals through changes in nucleation and growth rates of the crystalline phase. The project is designed to reveal these fundamental processes and mechanisms in rapid microstructure evolution that form the foundation of understanding that is an integral part of the DOE-BES mission.« less

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

NASA Astrophysics Data System (ADS)

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

2017-04-01

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

Low-Temperature Reactivities of Ultra-High Temperature Ceramics (Hf-X System)

DTIC Science & Technology

2005-12-01

as interacting fillers with the preceramic polymer formulations. In situ formation of the SiC phase was also evaluated as a practical approach in...led to a renewal of activities to fabricate MB2/ SiC composites as the materials of choice, because of their high thermal and oxidation resistance...HfB2/ SiC composite microstructures (and also HfC, ZrB2, and ZrC composites ) under pressureless conditions. These can be employed in reactive and

Experimental investigation of in-situ transformations of the M 7C3 carbide in the cast Fe-Cr-Ni alloy

NASA Astrophysics Data System (ADS)

Kraposhin, V. S.; Kondrat'ev, S. Yu.; Talis, A. L.; Anastasiadi, G. P.

2017-03-01

The microstructure and the phase composition of a heat-resistant Fe-Cr-Ni alloy (0. 45C-25Cr-35Ni) has been investigated in the cast state and after annealing at 1150°C for 2-100 h. After a 2-h high-temperature annealing, the fragmentation of the crystal structure of the eutectic M 7C3 carbides into domains of 500 nm in size with a partial transition into M 23C6 carbides is observed. After a 100-h holding, the complete transition of the hexagonal M 7C3 carbides into M 23C6 with a face-centered cubic structure occurs. The carbide transition M 7C3 → M 23 can be considered to be an in situ transformation.

Design and application of a mechanical load frame for in situ investigation of ferromagnetic shape memory alloys by magnetic force microscopy.

PubMed

Niklasch, D; Maier, H J; Karaman, I

2008-11-01

An in situ mechanical load frame has been developed for a commercially available atomic force microscope. This frame allows examining changes in topography and magnetic domain configuration under a given constant load or strain. First results obtained on Ni-Mn-Ga ferromagnetic shape memory alloy single crystals are presented. The magnetic force microscopy (MFM) measurements under different strain levels confirm the one-to-one correspondence, i.e., the magnetomicrostructural coupling between the martensite twins and the magnetic domains. Additionally, the growth of the twin variant with favorable orientation to the compression axis during martensite detwinning was observed. It will be shown that this load frame can be used for the investigation of the relationship between the microstructure and the magnetic domain structure in ferromagnetic shape memory alloys by MFM.

Thorium-Free Versus Thoriated Plasma Gun Electrodes: Statistical Evaluation of Coating Properties

NASA Astrophysics Data System (ADS)

Colmenares-Angulo, Jose; Molz, Ronald; Hawley, David; Seshadri, Ramachandran Chidambaram

2016-04-01

Industries throughout the world today have an increased awareness of environmental, health, and safety issues. This, together with recent Nuclear Regulatory Commission changes concerning source material (e.g., thorium) has added complexity in the supply chain of thoriated tungsten commonly used in plasma spray gun spares. In the interest of a safer and more sustainable work environment, Oerlikon Metco has developed thorium-free material solutions proven to have longer service life than conventional thoriated spares. This work reports on the effect, if any, caused by tungsten compositional changes and extended service life in coating properties. Microstructure, coating efficiency parameters, hardness, particle state, in situ coating stress, and ex situ modulus are evaluated over the service life duration of the nozzle, comparing coatings with thoriated and non-thoriated nozzles and electrodes with the same spray parameters.

In Situ Elevated Temperature Testing of Fly Ash Based Geopolymer Composites

PubMed Central

Vickers, Les; Pan, Zhu; Tao, Zhong; van Riessen, Arie

2016-01-01

In situ elevated temperature investigations using fly ash based geopolymers filled with alumina aggregate were undertaken. Compressive strength and short term creep tests were carried out to determine the onset temperature of viscous flow. Fire testing using the standard cellulose curve was performed. Applying a load to the specimen as the temperature increased reduced the temperature at which viscous flow occurred (compared to test methods with no applied stress). Compressive strength increased at the elevated temperature and is attributed to viscous flow and sintering forming a more compact microstructure. The addition of alumina aggregate and reduction of water content reduced the thermal conductivity. This led to the earlier onset and shorter dehydration plateau duration times. However, crack formation was reduced and is attributed to smaller thermal gradients across the fire test specimen. PMID:28773568

On the role of magnetic field intensity for better micro-structural characterization during Barkhausen Noise analysis

NASA Astrophysics Data System (ADS)

Yusufzai, Mohd Zaheer Khan; Vashista, M.

2018-04-01

Barkhausen Noise analysis is a popular and preferred technique for micro-structural characterization. The root mean square value and peak value of Barkhausen Noise burst are important parameters to assess the micro-hardness and residual stress. Barkhausen Noise burst can be enveloped using a curve known as Barkhausen Noise profile. Peak position of profile changes with change in micro-structure. In the present work, raw signal of Barkhausen Noise burst was obtained from Ni based sample at various magnetic field intensity to observe the effect of variation in field intensity on Barkhausen Noise burst. Raw signal was opened using MATLAB to further process for microstructure analysis. Barkhausen Noise analysis parameters such as magnetizing frequency, number of burst, high pass and low pass filter frequency were kept constant and magnetizing field was varied in wide range between 200 Oe to 1200 Oe. The processed profiles of Barkhausen Noise burst obtained at various magnetizing field intensity clearly reveals requirement of optimum magnetic field strength for better characterization of micro-structure.

Can multi-scale calibrations allow MT-derived resistivities to be used to probe the structure of the deep crust?

NASA Astrophysics Data System (ADS)

Toy, Virginia; Billia, Marco; Easingwood, Richard; Kirilova, Martina; Kluge, Emma; Sauer, Katrina; Sutherland, Rupert; Timms, Nicholas; Townend, John

2017-04-01

Our current knowledge of microstructural and mechanical controls on rock resistivity is such that identical magnetotelluric (MT) anomalies could result from a highly mineralized but extinct shear zone, or from an unmineralized, fluid saturated, active shear zone. In pursuit of the ability to interpret the structure and activity (rather than just the presence) of buried geological structures from electromagnetic data, we are investigating correlations between rock structure and electrical properties of ductile shear zone rocks recovered from the active Alpine Fault Zone, New Zealand. Multi-scale measurements of resistivity exist for this zone: its ductile portions have anomalously high electrical conductivity identified in MT models constructed as part of the South Island Geophysical Transect (SIGHT). Additionally wireline resistivities were measured in situ to 820 m depth during the recent Deep Fault Drilling Project (DFDP-2), and resisistivity of hand samples has been measured at laboratory conditions [Kluge et al., Abstract EGU2017-10139]. In exhumed and borehole samples, the distributions and arrangements of conductivity carriers - graphite, amorphous carbon, and grain boundary pores that would have contained brines or other conductive fluids at depth, have been characterised. These vary systematically according to the total ductile shear strain they have accommodated [Kirilova et al., Abstract EGU2017-5773; Sauer et al., Abstract EGU2017-10485]. Transmission electron microscopy analyses of grain boundaries also indicate that they contain carbon. The next phases of our investigation involve: (i) construction of crustal fluid composition models by quantitative microstructural and compositional/mineralogical mapping of fluid remnants and their solid residues and calibration of these using in situ measurements of fluid composition in DFDP-2 at depths to 820 m; (ii) calculation of resistivities for real microstructures based on electrical properties of the individual component minerals and fluids - for microstructures fully characterised in three-dimensions; (iii) measurement of the effects of dynamic linking of phases during ductile creep of solid rock on complex resistivity of DFDP samples at a range of realistic crustal temperatures and pressures. A particular challenge in this study is to determine appropriate scaling relationships of electrical properties among samples, boreholes, and MT models because dielectric constants of minerals depend on frequency of the imposed current, which varies with scale and, consequently, measurement method. We invite discussion of strategies to overcome this.

Measurement of kinaesthetic properties of in-brine table olives by microstructure of fracture surface, sensory evaluation and texture profile analysis (TPA).

PubMed

Lanza, Barbara; Amoruso, Filomena

2018-02-02

A series of transformations occur in olive fruit both during ripening and processing. In particular, significant changes in the microstructural composition affect the flavour, texture, nutrients and overall quality of the end product. Texture is one of the sensory quality attributes of greatest importance to consumer acceptance. In the present work, kinaesthetic properties of in-brine table olives of three cultivars of Olea europaea L. (Bella di Cerignola, Peranzana and Taggiasca cvs) were provided by several measurements of olive tissue texture by sensory, rheological and microstructural approaches. Olives at the same stage of ripening and processed with the same technology, but belonging to different cultivars, showed significant differences at microstructural, sensorial and rheological levels. To describe the relationship between the three variables, multiple regression analysis and principal component analysis were chosen. Differences in microstructure were closely related both in terms of hardness measured by texture profile analysis and hardness measured by sensory analysis. The information provided could be an aid for screening and training of a sensory panel. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

In situ X-ray study of the structural evolution of gold nano-domains by spray deposition on thin conductive P3HT films.

PubMed

Al-Hussein, M; Schindler, M; Ruderer, M A; Perlich, J; Schwartzkopf, M; Herzog, G; Heidmann, B; Buffet, A; Roth, S V; Müller-Buschbaum, P

2013-02-26

Gold (Au) nanoparticles are deposited from aqueous solution onto one of the most used conductive polymers, namely poly(3-hexylthiophene) (P3HT), using airbrush deposition. We report on the structure formation and packing of the Au nanoparticles after a 5 s spray cycle. In situ grazing incidence small-angle X-ray scattering (GISAXS) measurements with 20 ms time resolution allow a real-time observation of the emergence and evolution of the microstructure during a spray cycle and subsequent solvent evaporation. The results reveal multistage nanoscale ordering of the Au nanoparticles during the spray cycle. Further ex situ atomic force microscopy measurements of the sprayed films showed the formation of Au monolayer islands on top of the polymer film. Our study suggests that the solvent-substrate interaction as well as solvent evaporation kinetics are important factors that need to be taken into consideration in order to grow a compact uniform monolayer film for the fabrication of ultrathin films using airbrush deposition.

A small-angle x-ray scattering system with a vertical layout.

PubMed

Wang, Zhen; Chen, Xiaowei; Meng, Lingpu; Cui, Kunpeng; Wu, Lihui; Li, Liangbin

2014-12-01

A small-angle x-ray scattering (SAXS) system with a vertical layout (V-SAXS) has been designed and constructed for in situ detection on nanostructures, which is well suitable for in situ study on self-assembly of nanoparticles at liquid interface and polymer processing. A steel-tower frame on a reinforced basement is built as the supporting skeleton for scattering beam path and detector platform, ensuring the system a high working stability and a high operating accuracy. A micro-focus x-ray source combining parabolic three-dimensional multi-layer mirror and scatteringless collimation system provides a highly parallel beam, which allows us to detect the very small angle range. With a sample-to-detector distance of 7 m, the largest measurable length scale is 420 nm in real space. With a large sample zone, it is possible to install different experimental setups such as film stretching machine, which makes the system perfect to follow the microstructures evolution of materials during processing. The capability of the V-SAXS on in situ study is tested with a drying experiment of a free latex droplet, which confirms our initial design.

Data on a Laves phase intermetallic matrix composite in situ toughened by ductile precipitates.

PubMed

Knowles, Alexander J; Bhowmik, Ayan; Purkayastha, Surajit; Jones, Nicholas G; Giuliani, Finn; Clegg, William J; Dye, David; Stone, Howard J

2017-10-01

The data presented in this article are related to the research article entitled "Laves phase intermetallic matrix composite in situ toughened by ductile precipitates" (Knowles et al.) [1]. The composite comprised a Fe 2 (Mo, Ti) matrix with bcc (Mo, Ti) precipitated laths produced in situ by an aging heat treatment, which was shown to confer a toughening effect (Knowles et al.) [1]. Here, details are given on a focused ion beam (FIB) slice and view experiment performed on the composite so as to determine that the 3D morphology of the bcc (Mo, Ti) precipitates were laths rather than needles. Scanning transmission electron microscopy (S(TEM)) micrographs of the microstructure as well as energy dispersive X-ray spectroscopy (EDX) maps are presented that identify the elemental partitioning between the C14 Laves matrix and the bcc laths, with Mo rejected from the matrix into laths. A TEM selected area diffraction pattern (SADP) and key is provided that was used to validate the orientation relation between the matrix and laths identified in (Knowles et al.) [1] along with details of the transformation matrix determined.

Dynamic in-situ sensing of fluid-dispersed 2D materials integrated on microfluidic Si chip.

PubMed

Hogan, Benjamin T; Dyakov, Sergey A; Brennan, Lorcan J; Younesy, Salma; Perova, Tatiana S; Gun'ko, Yurii K; Craciun, Monica F; Baldycheva, Anna

2017-02-10

In this work, we propose a novel approach for wafer-scale integration of 2D materials on CMOS photonic chip utilising methods of synthetic chemistry and microfluidics technology. We have successfully demonstrated that this approach can be used for integration of any fluid-dispersed 2D nano-objects on silicon-on-insulator photonics platform. We demonstrate for the first time that the design of an optofluidic waveguide system can be optimised to enable simultaneous in-situ Raman spectroscopy monitoring of 2D dispersed flakes during the device operation. Moreover, for the first time, we have successfully demonstrated the possibility of label-free 2D flake detection via selective enhancement of the Stokes Raman signal at specific wavelengths. We discovered an ultra-high signal sensitivity to the xyz alignment of 2D flakes within the optofluidic waveguide. This in turn enables precise in-situ alignment detection, for the first practicable realisation of 3D photonic microstructure shaping based on 2D-fluid composites and CMOS photonics platform, while also representing a useful technological tool for the control of liquid phase deposition of 2D materials.

Comparison of in situ microstructure measurements to different turbulence closure schemes in a 3-D numerical ocean circulation model

NASA Astrophysics Data System (ADS)

Costa, Andrea; Doglioli, Andrea M.; Marsaleix, Patrick; Petrenko, Anne A.

2017-12-01

In situ measurements of kinetic energy dissipation rate ε and estimates of eddy viscosity KZ from the Gulf of Lion (NW Mediterranean Sea) are used to assess the ability of k - ɛ and k - ℓ closure schemes to predict microscale turbulence in a 3-D numerical ocean circulation model. Two different surface boundary conditions are considered in order to investigate their influence on each closure schemes' performance. The effect of two types of stability functions and optical schemes on the k - ɛ scheme is also explored. Overall, the 3-D model predictions are much closer to the in situ data in the surface mixed layer as opposed to below it. Above the mixed layer depth, we identify one model's configuration that outperforms all the other ones. Such a configuration employs a k - ɛ scheme with Canuto A stability functions, surface boundary conditions parameterizing wave breaking and an appropriate photosynthetically available radiation attenuation length. Below the mixed layer depth, reliability is limited by the model's resolution and the specification of a hard threshold on the minimum turbulent kinetic energy.

Non-Destructive Monitoring of Charge-Discharge Cycles on Lithium Ion Batteries using 7Li Stray-Field Imaging

PubMed Central

Tang, Joel A.; Dugar, Sneha; Zhong, Guiming; Dalal, Naresh S.; Zheng, Jim P.; Yang, Yong; Fu, Riqiang

2013-01-01

Magnetic resonance imaging provides a noninvasive method for in situ monitoring of electrochemical processes involved in charge/discharge cycling of batteries. Determining how the electrochemical processes become irreversible, ultimately resulting in degraded battery performance, will aid in developing new battery materials and designing better batteries. Here we introduce the use of an alternative in situ diagnostic tool to monitor the electrochemical processes. Utilizing a very large field-gradient in the fringe field of a magnet, stray-field-imaging (STRAFI) technique significantly improves the image resolution. These STRAFI images enable the real time monitoring of the electrodes at a micron level. It is demonstrated by two prototype half-cells, graphite∥Li and LiFePO4∥Li, that the high-resolution 7Li STRAFI profiles allow one to visualize in situ Li-ions transfer between the electrodes during charge/discharge cyclings as well as the formation and changes of irreversible microstructures of the Li components, and particularly reveal a non-uniform Li-ion distribution in the graphite. PMID:24005580

Microstructure and antibacterial property of in situ TiO(2) nanotube layers/titanium biocomposites.

PubMed

Cui, C X; Gao, X; Qi, Y M; Liu, S J; Sun, J B

2012-04-01

The TiO(2) nanotube layer was in situ synthesized on the surface of pure titanium by the electrochemical anodic oxidation. The diameter of nano- TiO(2) nanotubes was about 70~100 nm. The surface morphology and phase compositions of TiO(2) nanotube layers were observed and analyzed using the scanning electron microscope (SEM). The important processing parameters, including anodizing voltage, reaction time, concentration of electrolyte, were optimized in more detail. The photocatalytic activity of the nano- TiO(2) nanotube layers prepared with optimal conditions was evaluated via the photodegradation of methylthionine in aqueous solution. The antibacterial property of TiO(2) nanotube layers prepared with optimal conditions was evaluated by inoculating Streptococcus mutans on the TiO(2) nanotube layers in vitro. The results showed that TiO(2) nanotube layers/Ti biocomposites had very good antibacterial activity to resist Streptococcus mutans. As a dental implant biomaterial, in situ TiO(2) nanotube layer/Ti biocomposite has better and wider application prospects. Copyright © 2012 Elsevier Ltd. All rights reserved.

On the use of SEM correlative tools for in situ mechanical tests.

PubMed

Shi, Qiwei; Roux, Stéphane; Latourte, Félix; Hild, François; Loisnard, Dominique; Brynaert, Nicolas

2018-01-01

In situ SEM mechanical tests are key to study crystal plasticity. In particular, imaging and diffraction (EBSD) allow microstructure and surface kinematics to be monitored all along the test. However, to get a full benefit from different modalities, it is necessary to register all images and crystallographic orientation maps from EBSD into the same frame. Different correlative approaches tracking either Pt surface markings, crystal orientations or grain boundaries, allow such registrations to be performed and displacement as well as rotation fields to be measured, a primary information for crystal plasticity identification. However, the different contrasts that are captured in different modalities and unavoidable stage motions also give rise to artifacts that are to be corrected to register the different information onto the same material points. The same image correlation tools reveal very powerful to correct such artifacts. Illustrated by an in situ uniaxial tensile test performed on a bainitic-ferritic steel sample, recent advances in image correlation techniques are reviewed and shown to provide a comprehensive picture of local strain and rotation maps. Copyright © 2017 Elsevier B.V. All rights reserved.

In situ measurement of the rheological properties and agglomeration on cementitious pastes

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

Kim, Jae Hong; Yim, Hong Jae, E-mail: yimhj@knu.ac.kr; Ferron, Raissa Douglas

2016-07-15

Various factors influence the rheology of cementitious pastes, with the most important being the mixing protocol, mixture proportions, and mixture composition. This study investigated the influence of ground-granulated blast-furnace slag, on the rheological behavior of cementitious pastes. In tandem with the rheological measurements, fresh state microstructural measurements were conducted using three different techniques: A coupled stroboscope-rheometer, a coupled laser backscattering-rheometer, and a conventional laser diffraction technique. Laser diffraction and the coupled stroboscope-rheometer were not good measures of the in situ state of flocculation of a sample. Rather, only the laser backscattering technique allowed for in situ measurement on a highlymore » concentrated suspension (cementitious paste). Using the coupled laser backscattering-rheometer technique, a link between the particle system and rheological behavior was determined through a modeling approach that takes into account agglomeration properties. A higher degree of agglomeration was seen in the ordinary Portland cement paste than pastes containing the slag and this was related to the degree of capillary pressure in the paste systems.« less

Using in-situ diffraction, elastic plastic self-consistent models and microstructural analysis to interpret the low strain behavior of olivine polycrystals in the D-DIA apparatus

NASA Astrophysics Data System (ADS)

Burnley, P. C.; Kaboli, S.

2016-12-01

The textbook stress strain curve has an elastic response followed by a yield point and then plastic flow. Typically in rock deformation experiments the observed `elastic' behavior deviates from the Young's modulus because the mechanical response of the loading frame and friction in the sample assembly and between moving parts of the loading frame cannot be easily corrected for. Stress strain curves generated in a D-DIA apparatus used in conjunction with synchrotron x-rays should not have these problems because the sample length is measured directly by radiography and the stress in the sample is measured from the sample itself by x-ray diffraction. However, the sample's `elastic behavior', in many instances, still deviates from what is expected. For example, in constant strain rate experiments on both polycrystalline San Carlos olivine and fayalite olivine conducted at a variety of temperatures (25 - 1200 C) and pressures (4 and 7 GPa) although we are able to use elastic plastic self-consistent (EPSC) models to describe the plastic behavior of the olivine we are not able to fit the initial elastic behavior for all but the lowest temperature experiments. To a first approximation it appears that samples are generally more compliant than their elastic properties would predict and that the degree of softening is temperature dependent. For D-DIA experiments which have been conducted at strain rates of 10-5 /sec, there are not enough data points to really clarify what is happening in the elastic portion of the experiment. Therefore, we conducted a suite of low strain experiments at 5 x 10-6/sec at temperatures ranging from 400 C to 1200 C. For each experiment we fit the diffraction data using EPSC models. We will present the results from our diffraction analysis as well as detailed microstructural analysis of the experimental samples using electron backscatter diffraction (EBSD) and electron channeling contrast imaging (ECCI). The relative degree of relaxation observed for each grain population in the diffraction data as well as to the predictions of the EPSC model combined with the microstructural data, will be used create a more comprehensive picture of how individual grains and various grain populations contribute to the low strain mechanical behavior of the polycrystal.

Optimization of In-Situ Shot-Peening-Assisted Cold Spraying Parameters for Full Corrosion Protection of Mg Alloy by Fully Dense Al-Based Alloy Coating

NASA Astrophysics Data System (ADS)

Wei, Ying-Kang; Luo, Xiao-Tao; Li, Cheng-Xin; Li, Chang-Jiu

2017-01-01

Magnesium-based alloys have excellent physical and mechanical properties for a lot of applications. However, due to high chemical reactivity, magnesium and its alloys are highly susceptible to corrosion. In this study, Al6061 coating was deposited on AZ31B magnesium by cold spray with a commercial Al6061 powder blended with large-sized stainless steel particles (in-situ shot-peening particles) using nitrogen gas. Microstructure and corrosion behavior of the sprayed coating was investigated as a function of shot-peening particle content in the feedstock. It is found that by introducing the in-situ tamping effect using shot-peening (SP) particles, the plastic deformation of deposited particles is significantly enhanced, thereby resulting in a fully dense Al6061 coating. SEM observations reveal that no SP particle is deposited into Al6061 coating at the optimization spraying parameters. Porosity of the coating significantly decreases from 10.7 to 0.4% as the SP particle content increases from 20 to 60 vol.%. The electrochemical corrosion experiments reveal that this novel in-situ SP-assisted cold spraying is effective to deposit fully dense Al6061 coating through which aqueous solution is not permeable and thus can provide exceptional protection of the magnesium-based materials from corrosion.

Application of morphological synthesis for understanding electrode microstructure evolution as a function of applied charge/discharge cycles

DOE PAGES

Glazoff, Michael V.; Dufek, Eric J.; Shalashnikov, Egor V.

2016-09-15

Morphological analysis and synthesis operations were employed for analysis of electrode microstructure transformations and evolution accompanying the application of charge/discharge cycles to electrochemical storage systems (batteries). Using state-of-the-art morphological algorithms, it was possible to predict microstructure evolution in porous Si electrodes for Li-ion batteries with sufficient accuracy. Algorithms for image analyses (segmentation, feature extraction, and 3D-reconstructions using 2D-images) were also developed. Altogether, these techniques could be considered supplementary to phase-field mesoscopic approach to microstructure evolution that is based upon clear and definitive changes in the appearance of microstructure. However, unlike in phase-field, the governing equations for morphological approach are geometry-,more » not physics-based. Similar non-physics based approach to understanding different phenomena was attempted with the introduction of cellular automata. It is anticipated that morphological synthesis and analysis will represent a useful supplementary tool to phase-field and will render assistance to unraveling the underlying microstructure-property relationships. The paper contains data on electrochemical characterization of different electrode materials that was conducted in parallel to morphological study.« less

Micro-structural study and Rietveld analysis of fast reactor fuels: U-Mo fuels

NASA Astrophysics Data System (ADS)

Chakraborty, S.; Choudhuri, G.; Banerjee, J.; Agarwal, Renu; Khan, K. B.; Kumar, Arun

2015-12-01

U-Mo alloys are the candidate fuels for both research reactors and fast breeder reactors. In-reactor performance of the fuel depends on the microstructural stability and thermal properties of the fuel. To improve the fuel performance, alloying elements viz. Zr, Mo, Nb, Ti and fissium are added in the fuel. The first reactor fuels are normally prepared by injection casting. The objective of this work is to compare microstructure, phase-fields and hardness of as-cast four different U-Mo alloy (2, 5, 10 and 33 at.% Mo) fuels with the equilibrium microstructure of the alloys. Scanning electron microscope with energy dispersive spectrometer and optical microscope have been used to characterize the morphology of the as-cast and annealed alloys. The monoclinic α'' phase in as-cast U-10 at.% Mo alloy has been characterized through Rietveld analysis. A comparison of metallographic and Rietveld analysis of as-cast (dendritic microstructure) and annealed U-33 at.% Mo alloy, corresponding to intermetallic compound, has been reported here for the first time. This study will provide in depth understanding of microstructural and phase evolution of U-Mo alloys as fast reactor fuel.

Evolution of the three-dimensional collagen structure in vascular walls during deformation: an in situ mechanical testing under multiphoton microscopy observation.

PubMed

Nierenberger, Mathieu; Fargier, Guillaume; Ahzi, Saïd; Rémond, Yves

2015-08-01

The collagen fibers' three-dimensional architecture has a strong influence on the mechanical behavior of biological tissues. To accurately model this behavior, it is necessary to get some knowledge about the structure of the collagen network. In the present paper, we focus on the in situ characterization of the collagenous structure, which is present in porcine jugular vein walls. An observation of the vessel wall is first proposed in an unloaded configuration. The vein is then put into a mechanical tensile testing device. As the vein is stretched, three-dimensional images of its collagenous structure are acquired using multiphoton microscopy. Orientation analyses are provided for the multiple images recorded during the mechanical test. From these analyses, the reorientation of the two families of collagen fibers existing in the vein wall is quantified. We noticed that the reorientation of the fibers stops as the tissue stiffness starts decreasing, corresponding to the onset of damage. Besides, no relevant evolutions of the out of plane collagen orientations were observed. Due to the applied loading, our analysis also allowed for linking the stress relaxation within the tissue to its internal collagenous structure. Finally, this analysis constitutes the first mechanical test performed under a multiphoton microscope with a continuous three-dimensional observation of the tissue structure all along the test. It allows for a quantitative evaluation of microstructural parameters combined with a measure of the global mechanical behavior. Such data are useful for the development of structural mechanical models for living tissues.

The Hollow Spheres of the Orgueil Meteorite: A Re-Examination

NASA Technical Reports Server (NTRS)

Hoover, Richard B.; Jerman, Gregory; Rossignold-Strick, Maritine

2005-01-01

In 1971, Rossignol-Strick and Barghoorn provided images and a description of a number of spherical hollow microstructures showing well-defined walls in acid macerated extract of the Orgueil CI carbonaceous meteorite. Other forms such as membranes and spiral shaped structures were also reported. The carbon-rich (kerogen) hollow spheres were found to be in a narrowly constrained distribution of sizes (mainly 7 to 10 microns in diameter). Electron microprobe analysis revealed that these spheres contained Carbon, possibly P, N, and K. It was established that these forms could not be attributed to pollen or other recent terrestrial contaminants. It was concluded that they most probably represented organic coatings on globules of glass, olivine or magnetite in the meteorite. However, recent studies of the Orgueil meteorite have been carried out at the NASA/Marshall Space Flight Center with the S-4000 Hitachi Field Emission Scanning Electron Microscope (FESEM). These investigations have revealed the presence of numerous carbon encrusted spherical magnetite platelets and spherical and ovoidal bodies of elemental iron in-situ in freshly fractured interior surfaces of the meteorite. Their size range is also very narrowly constrained (typically approximately 6 to 12 microns) in diameter. High resolution images reveal that these bodies are also encrusted with a thin carbonaceous sheath and are surrounded by short nanofibrils that are shown to be composed of high purity iron by EDAX elemental analysis. We present Secondary and Backscatter Electron FESEM images and associated EDAX elemental analyses and 2D X-ray maps of these forms as we re-examine the hollow spheres of Orgueil and attempt to determine if they are representatives of the same population of indigenous microstructures.

Microstructural Evolution of HSLA ISO 3183 X80M (API 5L X80) Friction Stir Welded Joints

NASA Astrophysics Data System (ADS)

Hermenegildo, Tahiana F. C.; Santos, Tiago F. A.; Torres, Edwar A.; Afonso, Conrado R. M.; Ramirez, Antonio J.

2018-03-01

Evaluation was made of friction stir welded joints, identifying conditions that resulted in satisfactory welded joints free from defects and with microstructural characteristics that provided good mechanical properties. Microstructural characterization and cooling curve analysis of the joints with lower and higher heat inputs evidenced deformation below and above the non-recrystallization temperature (Tnr) and dynamic recrystallization during microstructural evolution. Microscopy analyses showed acicular ferrite, bainitic ferrite, and coalesced bainite microstructures in the stir zone of the cold weld (lower heat input), while the stir zone of the hot weld (higher heat input) contained bainitic ferrite, acicular ferrite, coalesced bainite, martensite, and dispersed carbides. Granular bainite and dispersed carbides were observed in all the heat affected zones. Analysis of the microstructural transformations, together with the thermal history of the joints, showed that the variable that had the greatest influence on the morphology of the bainite (granular bainite/bainitic ferrite) was the deformation temperature.

Small angle neutron scattering study of nano sized microstructure in Fe-Cr ODS steels for gen IV in-core applications.

PubMed

Han, Young-Soo; Mao, Xiadong; Jang, Jinsung

2013-11-01

The nano-sized microstructures in Fe-Cr oxide dispersion strengthened steel for Gen IV in-core applications were studied using small angle neutron scattering. The oxide dispersion strengthened steel was manufactured through hot isostatic pressing with various chemical compositions and fabrication conditions. Small angle neutron scattering experiments were performed using a 40 m small angle neutron scattering instrument at HANARO. Nano sized microstructures, namely, yttrium oxides and Cr-oxides were quantitatively analyzed by small angle neutron scattering. The yttrium oxides and Cr-oxides were also observed by transmission electron microscopy. The microstructural analysis results from small angle neutron scattering were compared with those obtained by transmission electron microscopy. The effects of the chemical compositions and fabrication conditions on the microstructure were investigated in relation to the quantitative microstructural analysis results obtained by small angle neutron scattering. The volume fraction of Y-oxide increases after fabrication, and this result is considered to be due to the formation of non-stochiometric Y-Ti-oxides.

Development of in-Situ Al-Si/CuAl2 Metal Matrix Composites: Microstructure, Hardness, and Wear Behavior

PubMed Central

Tash, Mahmoud M.; Mahmoud, Essam R. I.

2016-01-01

In the present work, in-situ metal matrix composites were fabricated through squeeze casting. The copper particles were dispersed with different weight percentages (3%, 6%, 10%, and 15%) into Al-12% Si piston alloy. Also, heat treatments were performed at 380 °C and 450 °C for holding times of 6 and 18 h. The microstructures, X-ray diffractometer (XRD) pattern, hardness, and wear characteristics were evaluated. The results showed that these copper particles have reacted with the aluminum under all of the aforementioned processing conditions resulting in the formation of fine copper aluminide intermetallics. Most of the intermetallics were CuAl2, while AlCu appeared in a small ratio. Additionally, these intermetallics were homogenously distributed within the alloy matrix with up to 6% Cu addition. The amounts of those intermetallics increased after performing heat treatment. Most of these intermetallics were CuAl2 at 380 °C, while the Cu-rich intermetallics appeared at 450 °C. Increasing the holding time to 18 h, however, led to grain coarsening and resulted in the formation of some cracks. The hardness of the resulting composite materials was improved. The hardness value reached to about 170 HV after heat treating at 380 °C for 8 h. The wear resistance of the resulting composite materials was remarkably improved, especially at lower additions of Cu and at the lower heat treatment temperature. PMID:28773564

Powder metallurgy processing and deformation characteristics of bulk multimodal nickel

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

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

2014-08-15

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

Effect of Heat Treatment on the Microstructure and Wear Properties of Al-Zn-Mg-Cu/In-Situ Al-9Si-SiCp/Pure Al Composite by Powder Metallurgy

NASA Astrophysics Data System (ADS)

Yu, Byung Chul; Bae, Ki-Chang; Jung, Je Ki; Kim, Yong-Hwan; Park, Yong Ho

2018-05-01

This study examined the effects of heat treatment on the microstructure and wear properties of Al-Zn-Mg-Cu/in-situ Al-9Si-SiCp/pure Al composites. Pure Al powder was used to increase densification but it resulted in heterogeneous precipitation as well as differences in hardness among the grains. Heat treatment was conducted to solve this problem. The heat treatment process consisted of three stages: solution treatment, quenching, and aging treatment. After the solution treatment, the main dissolved phases were η'(Mg4Zn7), η(MgZn2), and Al2Cu phase. An aging treatment was conducted over the temperature range, 100-240 °C, for various times. The GP zone and η'(Mg4Zn7) phase precipitated at a low aging temperature of 100-160 °C, whereas the η(MgZn2) phase precipitated at a high aging temperature of 200-240 °C. The hardness of the sample aged at 100-160 °C was higher than that aged at 200-240 °C. The wear test was conducted under various linear speeds with a load of 100 N. The aged composite showed a lower wear rate than that of the as-sintered composite under all conditions. As the linear speed was increased to 1.0 m/s, the predominant wear behavior changed from abrasive to adhesive wear in all composites.

Microstructure and wear resistance of Al2O3-M7C3/Fe composite coatings produced by laser controlled reactive synthesis

NASA Astrophysics Data System (ADS)

Tan, Hui; Luo, Zhen; Li, Yang; Yan, Fuyu; Duan, Rui

2015-05-01

Based on the principle of thermite reaction of Al and Fe2O3 powders, the Al2O3 ceramic reinforced Fe-based composite coatings were fabricated on a steel substrate by laser controlled reactive synthesis and cladding. The effects of different additions of thermite reactants on the phase transition, microstructure evolution, microhardness and wear resistance of the composite coatings were investigated by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Vickers microhardness and block-on-ring wear test, respectively. The results show that Al2O3 ceramic and M7C3 carbide are in situ synthesized via the laser controlled reactive synthesis. The Al2O3 ceramic and M7C3 carbides prefer to distribute along the γ-Fe phase boundary continuously, which separates the γ-Fe matrix and is beneficial to the grain refinement. With the increase of thermite reactants, the amount of Al2O3 ceramic and M7C3 carbide in the composite coatings increases gradually. Moreover the cladding layer changes from dendritic structure to columnar structure and martensite structure in the heat affected zone becomes coarse. The increased thermite reactants improve the microhardness and wear resistance of the in situ composite coatings obviously and enhance the hardness of the heat affected zone, which should be ascribed to the grain refinement, ceramic and carbide precipitation and solid solution strengthening.

Validation of a freshwater Otolith microstructure pattern for Nisqually Chinook Salmon (Oncorhynchus tshawytscha)

USGS Publications Warehouse

Lind-Null, Angie; Larsen, Kim

2011-01-01

The Nisqually Fall Chinook salmon (Oncorhynchus tshawytscha) population is one of 27 stocks in the Puget Sound (Washington) evolutionarily significant unit listed as threatened under the federal Endangered Species Act (ESA). Extensive restoration of the Nisqually River delta ecosystem has taken place to assist in recovery of the stock since estuary habitat is a critical transition zone for juvenile fall Chinook salmon. A pre-restoration baseline that includes the characterization of life history strategies, estuary residence times, growth rates and habitat use is needed to evaluate the potential response of hatchery and natural origin Chinook salmon to restoration efforts and to determine restoration success. Otolith microstructure analysis was selected as a tool to examine Chinook salmon life history, growth and residence in the Nisqually River estuary. The purpose of the current study is to incorporate microstructural analysis from the otoliths of juvenile Nisqually Chinook salmon collected at the downstream migrant trap within true freshwater (FW) habitat of the Nisqually River. The results from this analysis confirmed the previously documented Nisqually-specific FW microstructure pattern and revealed a Nisqually-specific microstructure pattern early in development (“developmental pattern”). No inter-annual variation in the microstructure pattern was visually observed when compared to samples from previous years. Furthermore, the Nisqually-specific “developmental pattern” and the FW microstructure pattern used in combination during analysis will allow us to recognize and separate with further confidence future unmarked Chinook salmon otolith collections into Nisqually-origin (natural or unmarked hatchery) and non-Nisqually origin categories. Freshwater mean increment width, growth rate and residence time were also calculated.

Intergranular degradation assessment via random grain boundary network analysis

DOEpatents

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

2002-01-01

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

Effect of Nano-Y2O3 on Microstructure and Crack Formation in Laser Direct-Deposited In Situ Particle-Reinforced Fe-Based Coatings

NASA Astrophysics Data System (ADS)

Yin, Guili; Chen, Suiyuan; Liu, Yuanyuan; Liang, Jing; Liu, Changsheng; Kuang, Zheng

2018-03-01

In situ hard-particle-reinforced Fe-based composite coatings were prepared on Q235 steel substrates by direct laser deposition using Fe-based alloy powders containing 2 wt.% B, 3 wt.% Si and 1-3 wt.% nano-Y2O3. The microstructures, phase compositions, hardnesses and wear resistances of the deposited coatings with different nano-Y2O3 contents were studied using metallographic microscopy, scanning electron microscopy, x-ray diffraction, transmission electron microscopy, microhardness tests and pin-on-disk abrasion tests (MMW-1A), respectively. The results showed that the appropriate addition of Y2O3 played a role in grain refinement and in decreasing the number of brittle phases and impurity elements in the grain boundaries. Consequently, the number of cracks in the laser-deposited coating also decreased. The Fe-based composite coatings were mainly composed of α-Fe, γ-Fe and in situ-produced reinforced particle phases, such as Cr23C6, Cr7C3, (Cr, Fe)7C3, Fe2B, and CrFeB. When the content of nano-Y2O3 was 2 wt.%, a Fe-based composite coating with a thickness of 4 mm that was free of cracks was obtained, and its surface hardness reached 650HV. Moreover, the wear resistance of the coating with 2 wt.% nano-Y2O3 was the best among the samples studied. The presence of nano-Y2O3 increased the solubility of Cr and Si in the solid solution, which eliminated the residual austenite region, and as a result, the phase transformation from γ-Fe to α-Fe was restrained and the transformation stress was also limited, thereby decreasing the probability of cracks in the coatings.

Processing and Mechanical Properties of NiAl-Based In-Situ Composites. Ph.D. Thesis Final Report

NASA Technical Reports Server (NTRS)

Johnson, David Ray

1994-01-01

In-situ composites based on the NiAl-Cr eutectic system were successfully produced by containerless processing and evaluated. The NiAl-Cr alloys had a fibrous microstructure while the NiAl-(Cr,Mo) alloys containing 1 at. percent or more molybdenum exhibited a lamellar structure. The NiAl-28Cr-6Mo eutectic displays promising high temperature strength while still maintaining a reasonable room temperature fracture toughness when compared to other NiAl-based materials. The Laves phase NiAlTa was used to strengthen NiAl and very promising creep strengths were found for the directionally solidified NiAl-NiAlTa eutectic. The eutectic composition was found to be near NiAl-15.5Ta (at. percent) and well aligned microstructures were produced at this composition. An off-eutectic composition of NiAl-14.5Ta was also processed, consisting of NiAl dendrites surrounded by aligned eutectic regions. The room temperature toughness of these two phase alloys was similar to that of polycrystalline NiAl even with the presence of the brittle Laves phase NiAlTa. Polyphase in-situ composites were generated by directional solidification of ternary eutectics. The systems investigated were the Ni-Al-Ta-X (X=Cr, Mo, or V) alloys. Ternary eutectics were found in each of these systems and both the eutectic composition and temperature were determined. Of these ternary eutectics, the one in the NiAl-Ta-Cr system was found to be the most promising. The fracture toughness of the NiAl-(Cr,Al)NiTa-Cr eutectic was intermediate between those of the NiAl-NiAlTa eutectic and the NiAl-Cr eutectic. The creep strength of this ternary eutectic was similar to or greater than that of the NiAl-Cr eutectic.

In situ grain fracture mechanics during uniaxial compaction of granular solids

NASA Astrophysics Data System (ADS)

Hurley, R. C.; Lind, J.; Pagan, D. C.; Akin, M. C.; Herbold, E. B.

2018-03-01

Grain fracture and crushing are known to influence the macroscopic mechanical behavior of granular materials and be influenced by factors such as grain composition, morphology, and microstructure. In this paper, we investigate grain fracture and crushing by combining synchrotron x-ray computed tomography and three-dimensional x-ray diffraction to study two granular samples undergoing uniaxial compaction. Our measurements provide details of grain kinematics, contacts, average intra-granular stresses, inter-particle forces, and intra-grain crystal and fracture plane orientations. Our analyses elucidate the complex nature of fracture and crushing, showing that: (1) the average stress states of grains prior to fracture vary widely in their relation to global and local trends; (2) fractured grains experience inter-particle forces and stored energies that are statistically higher than intact grains prior to fracture; (3) fracture plane orientations are primarily controlled by average intra-granular stress and contact fabric rather than the orientation of the crystal lattice; (4) the creation of new surfaces during fracture accounts for a very small portion of the energy dissipated during compaction; (5) mixing brittle and ductile grain materials alters the grain-scale fracture response. The results highlight an application of combined x-ray measurements for non-destructive in situ analysis of granular solids and provide details about grain fracture that have important implications for theory and modeling.

Effect of Low-Dose MDCT and Iterative Reconstruction on Trabecular Bone Microstructure Assessment.

PubMed

Kopp, Felix K; Holzapfel, Konstantin; Baum, Thomas; Nasirudin, Radin A; Mei, Kai; Garcia, Eduardo G; Burgkart, Rainer; Rummeny, Ernst J; Kirschke, Jan S; Noël, Peter B

2016-01-01

We investigated the effects of low-dose multi detector computed tomography (MDCT) in combination with statistical iterative reconstruction algorithms on trabecular bone microstructure parameters. Twelve donated vertebrae were scanned with the routine radiation exposure used in our department (standard-dose) and a low-dose protocol. Reconstructions were performed with filtered backprojection (FBP) and maximum-likelihood based statistical iterative reconstruction (SIR). Trabecular bone microstructure parameters were assessed and statistically compared for each reconstruction. Moreover, fracture loads of the vertebrae were biomechanically determined and correlated to the assessed microstructure parameters. Trabecular bone microstructure parameters based on low-dose MDCT and SIR significantly correlated with vertebral bone strength. There was no significant difference between microstructure parameters calculated on low-dose SIR and standard-dose FBP images. However, the results revealed a strong dependency on the regularization strength applied during SIR. It was observed that stronger regularization might corrupt the microstructure analysis, because the trabecular structure is a very small detail that might get lost during the regularization process. As a consequence, the introduction of SIR for trabecular bone microstructure analysis requires a specific optimization of the regularization parameters. Moreover, in comparison to other approaches, superior noise-resolution trade-offs can be found with the proposed methods.

Intrinsic stress in ZrN thin films: Evaluation of grain boundary contribution from in situ wafer curvature and ex situ x-ray diffraction techniques

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

Koutsokeras, L. E.; Department of Materials Science and Engineering, University of Ioannina, Ioannina 45110; Abadias, G.

2012-05-01

Low-mobility materials, like transition metal nitrides, usually undergo large residual stress when sputter-deposited as thin films. While the origin of stress development has been an active area of research for high-mobility materials, atomistic processes are less understood for low-mobility systems. In the present work, the contribution of grain boundary to intrinsic stress in reactively magnetron-sputtered ZrN films is evaluated by combining in situ wafer curvature measurements, providing information on the overall biaxial stress, and ex situ x-ray diffraction, giving information on elastic strain (and related stress) inside crystallites. The thermal stress contribution was also determined from the in situ stressmore » evolution during cooling down, after deposition was stopped. The stress data are correlated with variations in film microstructure and growth energetics, in the 0.13-0.42 Pa working pressure range investigated, and discussed based on existing stress models. At low pressure (high energetic bombardment conditions), a large compressive stress is observed due to atomic peening, which induces defects inside crystallites but also promotes incorporation of excess atoms in the grain boundary. Above 0.3-0.4 Pa, the adatom surface mobility is reduced, leading to the build-up of tensile stress resulting from attractive forces between under-dense neighbouring column boundary and possible void formation, while crystallites can still remain under compressive stress.« less

The study of in-situ formed alumina and aluminide intermetallic reinforced aluminum-based metal matrix composites

NASA Astrophysics Data System (ADS)

Yu, Peng

Aluminum-based metal matrix composites (MMCs) have been widely used as structural materials in the automobile and aerospace industry due to their specific properties. In this thesis, we report the fabrication of in-situ formed alumina and aluminide intermetallic reinforced aluminum-based metal matrix composites by the displacement reactions between Al and selected metal oxides (NiO, CuO and ZnO). These MMCs were produced when the Al-20wt% NiO, Al-20wt% CuO and Al-10wt% ZnO green compacts were reaction sintered in the tube furnaces. In this work, differential thermal analysis (DTA) was performed on the green samples. The green samples were then sintered separately in different tube furnaces for 30 minutes. In order to study the reaction mechanisms, the x-ray diffractometry (XRD) was used to obtain diffraction patterns of these sintered samples, the scanning electron microscope (SEM) and transmission electron microscope (TEM) were used to study the microstructures of these samples. The elemental quantitative compositions of samples were determined by the energy dispersive x-ray spectrometry (EDX). In order to study the effect of cooling rate on the samples, the green samples were further sintered to 1000°C and cooled down to room temperature in different conditions: by furnace-cooling, air-quenching, oil-quenching or NaCl-solution-quenching. The SEM, TEM and atomic force microscopy (AFM) were conducted to investigate their microstructures. A microhardness tester was used to measure the hardness values of these samples. It was found that during sintering of the Al-20wt% NiO green sample, displacement reaction between Al and NiO initially occurred in solid-solid form and was soon halted by its products that separated the NiO particles from the Al matrix. The reaction then resumed in solid-liquid form as the temperature increased to the eutectic temperature of Al3Ni-Al when liquid (Al, Ni) phase appeared in the sample. After cooling, Al2O 3 particles, Al3Ni proeutectic phase and fiber-like Al 3Ni-Al eutectic were found in the sintered Al-MMC sample. (Abstract shortened by UMI.)

Evaluation of agave fiber delignification by means of microscopy techniques and image analysis.

PubMed

Hernández-Hernández, Hilda M; Chanona-Pérez, Jorge J; Calderón-Domínguez, Georgina; Perea-Flores, María J; Mendoza-Pérez, Jorge A; Vega, Alberto; Ligero, Pablo; Palacios-González, Eduardo; Farrera-Rebollo, Reynold R

2014-10-01

Recently, the use of different types of natural fibers to produce paper and textiles from agave plants has been proposed. Agave atrovirens can be a good source of cellulose and lignin; nevertheless, the microstructural changes that happen during delignification have scarcely been studied. The aim of this work was to study the microstructural changes that occur during the delignification of agave fibers by means of microscopy techniques and image analysis. The fibers of A. atrovirens were obtained from leaves using convective drying, milling, and sieving. Fibers were processed using the Acetosolv pulping method at different concentrations of acetic acid; increasing acid concentration promoted higher levels of delignification, structural damage, and the breakdown of fiber clumps. Delignification followed by spectrometric analysis and microstructural studies were carried out by light, confocal laser scanning and scanning electron microscopy and showed that the delignification process follows three stages: initial, bulk, and residual. Microscopy techniques and image analysis were efficient tools for microstructural characterization during delignification of agave fibers, allowing quantitative evaluation of the process and the development of linear prediction models. The data obtained integrated numerical and microstructural information that could be valuable for the study of pulping of lignocellulosic materials.

Lab-on-fiber electrophoretic trace mixture separating and detecting an optofluidic device based on a microstructured optical fiber.

PubMed

Yang, Xinghua; Guo, Xiaohui; Li, Song; Kong, Depeng; Liu, Zhihai; Yang, Jun; Yuan, Libo

2016-04-15

We report an in-fiber integrated electrophoretic trace mixture separating and detecting an optofluidic optical fiber sensor based on a specially designed optical fiber. In this design, rapid in situ separation and simultaneous detection of mixed analytes can be realized under electro-osmotic flow in the microstructured optical fiber. To visually display the in-fiber separating and detecting process, two common fluorescent indicators are adopted as the optofluidic analytes in the optical fiber. Results show that a trace amount of the mixture (0.15 μL) can be completely separated within 3.5 min under a high voltage of 5 kV. Simultaneously, the distributed information of the separated analytes in the optical fiber can be clearly obtained by scanning along the optical fiber using a 355 nm laser. The emission from the analytes can be efficiently coupled into the inner core and guides to the remote end of the optical fiber. In addition, the thin cladding around the inner core in the optical fiber can prevent the fluorescent cross talk between the analytes in this design. Compared to previous optical fiber optofluidic devices, this device first realizes simultaneously separating treatment and the detection of the mixed samples in an optical fiber. Significantly, such an in-fiber integrated separating and detecting optofluidic device can find wide applications in various analysis fields involves mixed samples, such as biology, chemistry, and environment.

New constraints on deformation processes in serpentinite from sub-micron Raman Spectroscopy and TEM

NASA Astrophysics Data System (ADS)

Smith, S. A. F.; Tarling, M.; Rooney, J. S.; Gordon, K. C.; Viti, C.

2017-12-01

Extensive work has been performed to characterize the mineralogical and mechanical properties of the various serpentine minerals (i.e. antigorite, lizardite, chrysotile, polyhedral and polygonal serpentine). However, correct identification of serpentine minerals is often difficult or impossible using conventional analytical techniques such as optical- and SEM-based microscopy, X-ray diffraction and infrared spectroscopy. Transmission Electron Microscopy (TEM) is the best analytical technique to identify the serpentine minerals, but TEM requires complex sample preparation and typically results in very small analysis areas. Sub-micron confocal Raman spectroscopy mapping of polished thin sections provides a quick and relatively inexpensive way of unambiguously distinguishing the main serpentine minerals within their in-situ microstructural context. The combination of high spatial resolution (with a diffraction-limited system, 366 nm), large-area coverage (up to hundreds of microns in each dimension) and ability to map directly on thin sections allows intricate fault rock textures to be imaged at a sample-scale, which can then form the target of more focused TEM work. The potential of sub-micron Raman Spectroscopy + TEM is illustrated by examining sub-micron-scale mineral intergrowths and deformation textures in scaly serpentinites (e.g. dissolution seams, mineral growth in pressure shadows), serpentinite crack-seal veins and polished fault slip surfaces from a serpentinite-bearing mélange in New Zealand. The microstructural information provided by these techniques has yielded new insights into coseismic dehydration and amorphization processes and the interplay between creep and localised rupture in serpentinite shear zones.

Nanocomposite particles with improved microstructure for 3D culture systems and bone regeneration.

PubMed

Cecoltan, Sergiu; Stancu, Izabela-Cristina; Drăguşin, Diana Maria; Serafim, Andrada; Lungu, Adriana; Ţucureanu, Cătălin; Caraş, Iuliana; Tofan, Vlad Constantin; Sălăgeanu, Aurora; Vasile, Eugeniu; Mallet, Romain; Chappard, Daniel; Coman, Cristin; Istodorescu, Mircea; Iovu, Horia

2017-08-31

Nano-apatite and gelatin-alginate hydrogel microparticles have been prepared by a one-step synthesis combined with electrostatic bead generation, for the reconstruction of bone defects. Based on the analysis of bone composition, architecture and embryonic intramembranous ossification, a bio-inspired fabrication has been developed. Accordingly, the mineral phase has been in situ synthesized, calcifying the hydrogel matrix while the latter was crosslinked, finally generating microparticles that can assemble into a bone defect to ensure interconnected pores. Although nano-apatite-biopolymer composites have been widely investigated, microstructural optimization to provide improved distribution and stability of the mineral is rarely achieved. The optimization of the developed method progressively resulted in two types of formulations (15P and 7.5P), with 15 and 7.5 (wt%) phosphate content in the initial precursor. The osteolytic potential was investigated using differentiated macrophages. A commercially available calcium phosphate bone graft substitute (Eurocer 400) was incorporated into the hydrogel, and the obtained composites were in vitro tested for comparison. The cytocompatibility of the microparticles was studied with mouse osteoblast-like cell line MC3T3-E1. Results indicated the best in vitro performance have been obtained for the sample loaded with 7.5P. Preliminary evaluation of biocompatibility into a critical size (3 mm) defect in rabbits showed that 7.5P nanocomposite is associated with newly formed bone in the proximity of the microparticles, after 28 days.

Evidence of ancient microbial activity on Mars

NASA Astrophysics Data System (ADS)

Wallis, Jamie; Wickramasinghe, N. C.; Wallis, Daryl H.; Miyake, Nori; Wallis, M. K.; Hoover, Richard B.

2015-09-01

We report for the first time in situ observations of a relatively rare secondary iron arsenate-sulphate mineral named bukovskýite - Fe3+ 2(As5+O4)(S6+O4)(OH)•7(H2O) - found in a shock melt vein of the Tissint Martian meteorite. It is hypothesised that the mineral formed when high concentrations of aqueous H+, Fe(III), SO4 and AsO4 were maintained for long periods of time in microenvironments created within wet subsurface Martian clays. The aqueous H+, Fe(III), SO4 and AsO4 species arose from the microbial oxidation of FeS2 with concurrent release of sequestrated As. The availability of aqueous AsO4 would also be complemented by dissolution by-products of the microbial reduction of Feoxides influenced by dissolved organic matter that alters the redox state and the complexation of As, thus shifting As partitioning in favour of the solute phase. This hypothesis is substantially supported by SEM analysis of a 15μm spherical structure comprising of a carbonaceous outer coating with a inner core of FeS2 (pyrite) that showed the pyrite surface with spherical pits, and chains of pits, with morphologies distinct from abiotic alteration features. The pits and channels have a clustered, geometric distribution, typical of microbial activity, and are closely comparable to biologically mediated microstructures created by Fe- and S-oxidising microbes in the laboratory. These microstructures are interpreted as trace fossils resulting from the attachment of bacteria to the pyrite surfaces.

Effects of Hot-Hydrostatic Canned Extrusion on the Stock Utilization, Microstructure and Mechanical Properties of TiBw/TC4 Composites with Quasi-Continuous Network

PubMed Central

Feng, Yangju; Li, Bing; Cui, Guorong; Zhang, Wencong

2017-01-01

In-situ TiB whisker-reinforced Ti–6Al–4V (TC4) titanium matrix composites (TiBw/TC4) with quasi-continuous networks were successfully fabricated by vacuum hot-pressing sintering. The effects of the hot-hydrostatic canned extrusion on stock utilization, microstructure and mechanical properties of the TiBw/TC4 composites were investigated. It was satisfactory that the utilization of composites could be obviously improved by canned extrusion compared to that extruded without canned extrusion. The microstructure results showed that after canned extrusion the grain was refined and the TiB whiskers were distributed from a random array state to a state in which the whiskers were distributed along the extrusion direction. The properties testing results revealed that the tensile strength, the hardness and the ductility of the composites all significantly improved after extrusion due to the grain refinement and orientation of the TiB whisker caused by extrusion. Tensile fracture results showed that when the TiB whiskers were randomly distributed only part of them played a role in strengthening the matrix during the deformation process (as-sintered composites), while when the TiB whiskers were oriented all whiskers could strengthen the matrix during the tensile testing process (as-extruded composites). PMID:29068416

Stability Study of the RERTR Fuel Microstructure

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

Jian Gan; Dennis Keiser; Brandon Miller

2014-04-01

The irradiation stability of the interaction phases at the interface of fuel and Al alloy matrix as well as the stability of the fission gas bubble superlattice is believed to be very important to the U-Mo fuel performance. In this paper the recent result from TEM characterization of Kr ion irradiated U-10Mo-5Zr alloy will be discussed. The focus will be on the phase stability of Mo2-Zr, a dominated second phase developed at the interface of U-10Mo and the Zr barrier in a monolithic fuel plate from fuel fabrication. The Kr ion irradiations were conducted at a temperature of 200 degreesmore » C to an ion fluence of 2.0E+16 ions/cm2. To investigate the thermal stability of the fission gas bubble superlattice, a key microstructural feature in both irradiated dispersion U-7Mo fuel and monolithic U-10Mo fuel, a FIB-TEM sample of the irradiated U-10Mo fuel (3.53E+21 fission/cm3) was used for a TEM in-situ heating experiment. The preliminary result showed extraordinary thermal stability of the fission gas bubble superlattice. The implication of the TEM observation from these two experiments on the fuel microstructural evolution under irradiation will be discussed.« less

Microstructures and Mechanical Properties of Friction Tapered Stud Overlap Welding for X65 Pipeline Steel Under Wet Conditions

NASA Astrophysics Data System (ADS)

Xu, Y. C.; Jing, H. Y.; Han, Y. D.; Xu, L. Y.

2017-08-01

This paper exhibits a novel in situ remediation technique named friction tapered stud overlap welding (FTSOW) to repair a through crack in structures and components in extremely harsh environments. Furthermore, this paper presents variations in process data, including rotational speed, stud displacement, welding force, and torque for a typical FTSOW weld. In the present study, the effects of welding parameters on the microstructures and mechanical properties of the welding joints were investigated. Inapposite welding parameters consisted of low rotational speeds and welding forces, and when utilized, they increased the occurrence of a lack of bonding and unfilled defects within the weld. The microstructures with a welding zone and heat-affected zone mainly consisted of upper bainite. The hardness value was highest in the welding zone and lowest in the base material. During the pull-out tests, all the welds failed in the stud. Moreover, the defect-free welds broke at the interface of the lap plate and substrate during the cruciform uniaxial tensile test. The best tensile test results at different depths and shear tests were 721.6 MPa and 581.9 MPa, respectively. The favorable Charpy impact-absorbed energy was 68.64 J at 0 °C. The Charpy impact tests revealed a brittle fracture characteristic with a large area of cleavage.

Loading Path and Control Mode Effects During Thermomechanical Cycling of Polycrystalline Shape Memory NiTi

NASA Astrophysics Data System (ADS)

Nicholson, D. E.; Benafan, O.; Padula, S. A.; Clausen, B.; Vaidyanathan, R.

2018-01-01

Loading path dependencies and control mode effects in polycrystalline shape memory NiTi were investigated using in situ neutron and synchrotron X-ray diffraction performed during mechanical cycling and thermal cycling at constant strain. Strain-controlled, isothermal, reverse loading (to ± 4%) and stress-controlled, isothermal, cyclic loading (to ± 400 MPa for up to ten cycles) at room temperature demonstrated that the preferred martensite variants selected correlated directly with the macroscopic uniaxial strain and did not correlate with the compressive or tensile state of stress. During cyclic loading (up to ten cycles), no significant cycle-to-cycle evolution of the variant microstructure corresponding to a given strain was observed, despite changes in the slope of the stress-strain response with each cycle. Additionally, thermal cycling (to above and below the phase transformation) under constant strain (up to 2% tensile strain) showed that the martensite variant microstructure correlated directly with strain and did not evolve following thermal cycling, despite relaxation of stress in both martensite and austenite phases. Results are presented in the context of variant reorientation and detwinning processes in martensitic NiTi, the fundamental thermoelastic nature of such processes and the ability of the variant microstructure to accommodate irreversible deformation processes.

Microstructure and Properties of Polypropylene/Carbon Nanotube Nanocomposites

PubMed Central

Bikiaris, Dimitrios

2010-01-01

In the last few years, great attention has been paid to the preparation of polypropylene (PP) nanocomposites using carbon nanotubes (CNTs) due to the tremendous enhancement of the mechanical, thermal, electrical, optical and structural properties of the pristine material. This is due to the unique combination of structural, mechanical, electrical, and thermal transport properties of CNTs. However, it is well-known that the properties of polymer-based nanocomposites strongly depend on the dispersion of nanofillers and almost all the discussed properties of PP/CNTs nanocomposites are strongly related to their microstructure. PP/CNTs nanocomposites were, mainly, prepared by melt mixing and in situ polymerization. Young’s modulus, tensile strength and storage modulus of the PP/CNTs nanocomposites can be increased with increasing CNTs content due to the reinforcement effect of CNTs inside the polymer matrix. However, above a certain CNTs content the mechanical properties are reduced due to the CNTs agglomeration. The microstructure of nanocomposites has been studied mainly by SEM and TEM techniques. Furthermore, it was found that CNTs can act as nucleating agents promoting the crystallization rates of PP and the addition of CNTs enhances all other physical properties of PP. The aim of this paper is to provide a comprehensive review of the existing literature related to PP/CNTs nanocomposite preparation methods and properties studies.

Ultrafast synchrotron X-ray imaging studies of microstructure fragmentation in solidification under ultrasound

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

Wang, Bing; Tan, Dongyue; Lee, Tung Lik

Ultrasound processing of metal alloys is an environmental friendly and promising green technology for liquid metal degassing and microstructural refinement. However many fundamental issues in this field are still not fully understood, because of the difficulties in direct observation of the dynamic behaviours caused by ultrasound inside liquid metal and semisolid metals during the solidification processes. In this paper, we report a systematic study using the ultrafast synchrotron X-ray imaging (up to 271,554 frame per second) technique available at the Advanced Photon Source, USA and Diamond Light Source, UK to investigate the dynamic interactions between the ultrasonic bubbles/acoustic flow andmore » the solidifying phases in a Bi-8%Zn alloy. The experimental results were complimented by numerical modelling. The chaotic bubble implosion and dynamic bubble oscillations were revealed in-situ for the first time in liquid metal and semisolid metal. The fragmentation of the solidifying Zn phases and breaking up of the liquid-solid interface by ultrasonic bubbles and enhanced acoustic flow were clearly demonstrated and agreed very well with the theoretical calculations. The research provides unambiguous experimental evidence and robust theoretical interpretation in elucidating the dominant mechanisms of microstructure fragmentation and refinement in solidification under ultrasound.« less

Effects of Hot-Hydrostatic Canned Extrusion on the Stock Utilization, Microstructure and Mechanical Properties of TiBw/TC4 Composites with Quasi-Continuous Network.

PubMed

Feng, Yangju; Li, Bing; Cui, Guorong; Zhang, Wencong

2017-10-25

In-situ TiB whisker-reinforced Ti-6Al-4V (TC4) titanium matrix composites (TiBw/TC4) with quasi-continuous networks were successfully fabricated by vacuum hot-pressing sintering. The effects of the hot-hydrostatic canned extrusion on stock utilization, microstructure and mechanical properties of the TiBw/TC4 composites were investigated. It was satisfactory that the utilization of composites could be obviously improved by canned extrusion compared to that extruded without canned extrusion. The microstructure results showed that after canned extrusion the grain was refined and the TiB whiskers were distributed from a random array state to a state in which the whiskers were distributed along the extrusion direction. The properties testing results revealed that the tensile strength, the hardness and the ductility of the composites all significantly improved after extrusion due to the grain refinement and orientation of the TiB whisker caused by extrusion. Tensile fracture results showed that when the TiB whiskers were randomly distributed only part of them played a role in strengthening the matrix during the deformation process (as-sintered composites), while when the TiB whiskers were oriented all whiskers could strengthen the matrix during the tensile testing process (as-extruded composites).

Microstructure and properties of Fe-based composite coating by laser cladding Fe-Ti-V-Cr-C-CeO2 powder

NASA Astrophysics Data System (ADS)

Zhang, Hui; Zou, Yong; Zou, Zengda; Wu, Dongting

2015-01-01

In situ TiC-VC reinforced Fe-based cladding layer was obtained on low carbon steel surface by laser cladding with Fe-Ti-V-Cr-C-CeO2 alloy powder. The microstructure, phases and properties of the cladding layer were investigated by X-ray diffractometry (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), transmission electron microscopy (TEM), potentio-dynamic polarization and electro-chemical impedance spectroscopy (EIS). Results showed Fe-Ti-V-Cr-C-CeO2 alloy powder formed a good cladding layer without defects such as cracks and pores. The phases of the cladding layer were α-Fe, γ-Fe, TiC, VC and TiVC2. The microstructures of the cladding layer matrix were lath martensite and retained austenite. The carbides were polygonal blocks with a size of 0.5-2 μm and distributed uniformly in the cladding layer. High resolution transmission electron microscopy showed the carbide was a complex matter composed of nano TiC, VC and TiVC2. The cladding layer with a hardness of 1030 HV0.2 possessed good wear and corrosion resistance, which was about 16.85 and 9.06 times than that of the substrate respectively.

Metastable growth of pure wurtzite InGaAs microstructures.

PubMed

Ng, Kar Wei; Ko, Wai Son; Lu, Fanglu; Chang-Hasnain, Connie J

2014-08-13

III-V compound semiconductors can exist in two major crystal phases, namely, zincblende (ZB) and wurtzite (WZ). While ZB is thermodynamically favorable in conventional III-V epitaxy, the pure WZ phase can be stable in nanowires with diameters smaller than certain critical values. However, thin nanowires are more vulnerable to surface recombination, and this can ultimately limit their performances as practical devices. In this work, we study a metastable growth mechanism that can yield purely WZ-phased InGaAs microstructures on silicon. InGaAs nucleates as sharp nanoneedles and expand along both axial and radial directions simultaneously in a core-shell fashion. While the base can scale from tens of nanometers to over a micron, the tip can remain sharp over the entire growth. The sharpness maintains a high local surface-to-volume ratio, favoring hexagonal lattice to grow axially. These unique features lead to the formation of microsized pure WZ InGaAs structures on silicon. To verify that the WZ microstructures are truly metastable, we demonstrate, for the first time, the in situ transformation from WZ to the energy-favorable ZB phase inside a transmission electron microscope. This unconventional core-shell growth mechanism can potentially be applied to other III-V materials systems, enabling the effective utilization of the extraordinary properties of the metastable wurtzite crystals.

Creep Crack Initiation and Growth Behavior for Ni-Base Superalloys

NASA Astrophysics Data System (ADS)

Nagumo, Yoshiko; Yokobori, A. Toshimitsu, Jr.; Sugiura, Ryuji; Ozeki, Go; Matsuzaki, Takashi

The structural components which are used in high temperature gas turbines have various shapes which may cause the notch effect. Moreover, the site of stress concentration might have the heterogeneous microstructural distribution. Therefore, it is necessary to clarify the creep fracture mechanism for these materials in order to predict the life of creep fracture with high degree of accuracy. In this study, the creep crack growth tests were performed using in-situ observational testing machine with microscope to observe the creep damage formation and creep crack growth behavior. The materials used are polycrystalline Ni-base superalloy IN100 and directionally solidified Ni-base superalloy CM247LC which were developed for jet engine turbine blades and gas turbine blades in electric power plants, respectively. The microstructural observation of the test specimens was also conducted using FE-SEM/EBSD. Additionally, the analyses of two-dimensional elastic-plastic creep finite element using designed methods were conducted to understand the effect of microstructural distribution on creep damage formation. The experimental and analytical results showed that it is important to determine the creep crack initiation and early crack growth to predict the life of creep fracture and it is indicated that the highly accurate prediction of creep fracture life could be realized by measuring notch opening displacement proposed as the RNOD characteristic.

Experimental and Computational Investigation of Structural Integrity of Dissimilar Metal Weld Between Ferritic and Austenitic Steel

NASA Astrophysics Data System (ADS)

Santosh, R.; Das, G.; Kumar, S.; Singh, P. K.; Ghosh, M.

2018-03-01

The structural integrity of dissimilar metal welded (DMW) joint consisting of low-alloy steel and 304LN austenitic stainless steel was examined by evaluating mechanical properties and metallurgical characteristics. INCONEL 82 and 182 were used as buttering and filler materials, respectively. Experimental findings were substantiated through thermomechanical simulation of the weld. During simulation, the effect of thermal state and stress distribution was pondered based on the real-time nuclear power plant environment. The simulation results were co-related with mechanical and microstructural characteristics. Material properties were varied significantly at different fusion boundaries across the weld line and associated with complex microstructure. During in-situ deformation testing in a scanning electron microscope, failure occurred through the buttering material. This indicated that microstructure and material properties synergistically contributed to altering the strength of DMW joints. Simulation results also depicted that the stress was maximum within the buttering material and made its weakest zone across the welded joint during service exposure. Various factors for the failure of dissimilar metal weld were analyzed. It was found that the use of IN 82 alloy as the buttering material provided a significant improvement in the joint strength and became a promising material for the fabrication of DMW joint.

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.

Ultrafast synchrotron X-ray imaging studies of microstructure fragmentation in solidification under ultrasound

DOE PAGES

Wang, Bing; Tan, Dongyue; Lee, Tung Lik; ...

2017-11-03

Ultrasound processing of metal alloys is an environmental friendly and promising green technology for liquid metal degassing and microstructural refinement. However many fundamental issues in this field are still not fully understood, because of the difficulties in direct observation of the dynamic behaviours caused by ultrasound inside liquid metal and semisolid metals during the solidification processes. In this paper, we report a systematic study using the ultrafast synchrotron X-ray imaging (up to 271,554 frame per second) technique available at the Advanced Photon Source, USA and Diamond Light Source, UK to investigate the dynamic interactions between the ultrasonic bubbles/acoustic flow andmore » the solidifying phases in a Bi-8%Zn alloy. The experimental results were complimented by numerical modelling. The chaotic bubble implosion and dynamic bubble oscillations were revealed in-situ for the first time in liquid metal and semisolid metal. The fragmentation of the solidifying Zn phases and breaking up of the liquid-solid interface by ultrasonic bubbles and enhanced acoustic flow were clearly demonstrated and agreed very well with the theoretical calculations. The research provides unambiguous experimental evidence and robust theoretical interpretation in elucidating the dominant mechanisms of microstructure fragmentation and refinement in solidification under ultrasound.« less

Experimental and Computational Investigation of Structural Integrity of Dissimilar Metal Weld Between Ferritic and Austenitic Steel

NASA Astrophysics Data System (ADS)

Santosh, R.; Das, G.; Kumar, S.; Singh, P. K.; Ghosh, M.

2018-06-01

The structural integrity of dissimilar metal welded (DMW) joint consisting of low-alloy steel and 304LN austenitic stainless steel was examined by evaluating mechanical properties and metallurgical characteristics. INCONEL 82 and 182 were used as buttering and filler materials, respectively. Experimental findings were substantiated through thermomechanical simulation of the weld. During simulation, the effect of thermal state and stress distribution was pondered based on the real-time nuclear power plant environment. The simulation results were co-related with mechanical and microstructural characteristics. Material properties were varied significantly at different fusion boundaries across the weld line and associated with complex microstructure. During in-situ deformation testing in a scanning electron microscope, failure occurred through the buttering material. This indicated that microstructure and material properties synergistically contributed to altering the strength of DMW joints. Simulation results also depicted that the stress was maximum within the buttering material and made its weakest zone across the welded joint during service exposure. Various factors for the failure of dissimilar metal weld were analyzed. It was found that the use of IN 82 alloy as the buttering material provided a significant improvement in the joint strength and became a promising material for the fabrication of DMW joint.

Loading Path and Control Mode Effects During Thermomechanical Cycling of Polycrystalline Shape Memory NiTi

NASA Astrophysics Data System (ADS)

Nicholson, D. E.; Benafan, O.; Padula, S. A.; Clausen, B.; Vaidyanathan, R.

2018-03-01

Loading path dependencies and control mode effects in polycrystalline shape memory NiTi were investigated using in situ neutron and synchrotron X-ray diffraction performed during mechanical cycling and thermal cycling at constant strain. Strain-controlled, isothermal, reverse loading (to ± 4%) and stress-controlled, isothermal, cyclic loading (to ± 400 MPa for up to ten cycles) at room temperature demonstrated that the preferred martensite variants selected correlated directly with the macroscopic uniaxial strain and did not correlate with the compressive or tensile state of stress. During cyclic loading (up to ten cycles), no significant cycle-to-cycle evolution of the variant microstructure corresponding to a given strain was observed, despite changes in the slope of the stress-strain response with each cycle. Additionally, thermal cycling (to above and below the phase transformation) under constant strain (up to 2% tensile strain) showed that the martensite variant microstructure correlated directly with strain and did not evolve following thermal cycling, despite relaxation of stress in both martensite and austenite phases. Results are presented in the context of variant reorientation and detwinning processes in martensitic NiTi, the fundamental thermoelastic nature of such processes and the ability of the variant microstructure to accommodate irreversible deformation processes.

In situ-measurement of ice deformation from repeated borehole logging of the EPICA Dronning Maud Land (EDML) ice core, East Antarctica.

NASA Astrophysics Data System (ADS)

Jansen, Daniela; Weikusat, Ilka; Kleiner, Thomas; Wilhelms, Frank; Dahl-Jensen, Dorthe; Frenzel, Andreas; Binder, Tobias; Eichler, Jan; Faria, Sergio H.; Sheldon, Simon; Panton, Christian; Kipfstuhl, Sepp; Miller, Heinrich

2017-04-01

The European Project for Ice Coring in Antarctica (EPICA) ice core was drilled between 2001 and 2006 at the Kohnen Station, Antarctica. During the drilling process the borehole was logged repeatedly. Repeated logging of the borehole shape is a means of directly measuring the deformation of the ice sheet not only on the surface but also with depth, and to derive shear strain rates for the lower part, which control the volume of ice transported from the inner continent towards the ocean. The logging system continuously recorded the tilt of the borehole with respect to the vertical (inclination) as well as the heading of the borehole with respect to magnetic north (azimuth) by means of a compass. This dataset provides the basis for a 3-D reconstruction of the borehole shape, which is changing over time according to the predominant deformation modes with depth. The information gained from this analysis can then be evaluated in combination with lattice preferred orientation, grain size and grain shape derived by microstructural analysis of samples from the deep ice core. Additionally, the diameter of the borehole, which was originally circular with a diameter of 10 cm, was measured. As the ice flow velocity at the position of the EDML core is relatively slow (about 0.75 m/a), the changes of borehole shape between the logs during the drilling period were very small and thus difficult to interpret. Thus, the site has been revisited in the Antarctic summer season 2016 and logged again using the same measurement system. The change of the borehole inclination during the time period of 10 years clearly reveals the transition from a pure shear dominated deformation in the upper part of the ice sheet to shear deformation at the base. We will present a detailed analysis of the borehole parameters and the deduced shear strain rates in the lower part of the ice sheet. The results are discussed with respect to ice microstructural data derived from the EDML ice core. Microstructural data directly reflect the deformation conditions, as the ice polycrystal performs the deformation which leads e.g. to characteristic lattice orientation distributions and grain size and shape appearance. Though overprinted by recrystallization (due to the hot environment for the ice) and the slow deformation, analysis of statistically significant grain numbers reveals indications typical for the changing deformation regimes with depth. Additionally we compare our results with strain rates derived from a simulation with a model for large scale ice deformation, the Parallel Ice Sheet Model (PISM).

Twinning behaviors of a rolled AZ31 magnesium alloy under multidirectional loading

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

Hou, Dewen

The microstructure and texture evolution of an AZ31 magnesium rolled sheet during quasi-static compression at strain rates of 10{sup −3} s{sup −1} has been investigated by in situ electron backscattered diffraction. The influence of the initial and pre-deformed texture on the predominant deformation mechanisms during compression has been examined. It has been found that extensive grain reorientation due to (10 − 12) tensile twinning appeared when compressed along transverse direction. Tensile twin variants were observed under this loading condition, and different variants will cause an effect to the following deformation. Several twinning modes occurred with continuative loading along rolling direction.more » - Highlights: •Twinning behaviors were investigated through in situ multidirectional compressive tests. •Deformation behavior was affected by the twin variants. •Four types of twinning behaviors were observed during deformation process.« less

Design of a miniature flow cell for in situ x-ray imaging of redox flow batteries

NASA Astrophysics Data System (ADS)

Jervis, Rhodri; Brown, Leon D.; Neville, Tobias P.; Millichamp, Jason; Finegan, Donal P.; Heenan, Thomas M. M.; Brett, Dan J. L.; Shearing, Paul R.

2016-11-01

Flow batteries represent a possible grid-scale energy storage solution, having many advantages such as scalability, separation of power and energy capabilities, and simple operation. However, they can suffer from degradation during operation and the characteristics of the felt electrodes are little understood in terms of wetting, compression and pressure drops. Presented here is the design of a miniature flow cell that allows the use of x-ray computed tomography (CT) to study carbon felt materials in situ and operando, in both lab-based and synchrotron CT. Through application of the bespoke cell it is possible to observe felt fibres, electrolyte and pore phases and therefore enables non-destructive characterisation of an array of microstructural parameters during the operation of flow batteries. Furthermore, we expect this design can be readily adapted to the study of other electrochemical systems.

In Situ Formation of Decavanadate-Intercalated Layered Double Hydroxide Films on AA2024 and their Anti-Corrosive Properties when Combined with Hybrid Sol Gel Films

PubMed Central

Wu, Junsheng; Peng, Dongdong; He, Yuntao; Du, Xiaoqiong; Zhang, Zhan; Zhang, Bowei; Li, Xiaogang; Huang, Yizhong

2017-01-01

A layered double hydroxide (LDH) film was formed in situ on aluminum alloy 2024 through a urea hydrolysis method, and a decavanadate-intercalated LDH (LDH-V) film fabricated through the dip coating method. The microstructural and morphological characteristics were investigated by scanning electron microscopy (SEM). The corrosion-resistant performance was analyzed by electrochemical impedance spectroscopy (EIS), scanning electrochemical microscopy (SECM), and a salt-spray test (SST).The SEM results showed that a complete and defect-free surface was formed on the LDH-VS film. The anticorrosion results revealed that the LDH-VS film had better corrosion-resistant properties than the LDH-S film, especially long-term corrosion resistance. The mechanism of corrosion protection was proposed to consist of the self-healing effect of the decavanadate intercalation and the shielding effect of the sol-gel film. PMID:28772785

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

Luce, F. P.; Azevedo, G. de M.; Baptista, D. L.

The formation and time resolved behavior of individual Pb nanoparticles embedded in silica have been studied by in-situ transmission electron microscopy observations at high temperatures (400–1100 °C) and under 200 keV electron irradiation. It is shown that under such extreme conditions, nanoparticles can migrate at long distances presenting a Brownian-like behavior and eventually coalesce. The particle migration phenomenon is discussed considering the influence of the thermal energy and the electron irradiation effects on the atomic diffusion process which is shown to control particle migration. These results and comparison with ex-situ experiments tackle the stability and the microstructure evolution of nanoparticles systems undermore » extreme conditions. It elucidates on the effects of energetic particle irradiation-annealing treatments either as a tool or as a detrimental issue that could hamper their long-term applications in radiation-harsh environments such as in space or nuclear sectors.« less

Microstructural changes in CdSe-coated ZnO nanowires evaluated by in situ annealing in transmission electron microscopy and x-ray diffraction

NASA Astrophysics Data System (ADS)

Majidi, Hasti; Winkler, Christopher R.; Taheri, Mitra L.; Baxter, Jason B.

2012-07-01

We report on the crystallite growth and phase change of electrodeposited CdSe coatings on ZnO nanowires during annealing. Both in situ transmission electron microscopy (TEM) and x-ray diffraction (XRD) reveal that the nanocrystal size increases from ˜3 to ˜10 nm upon annealing at 350 °C for 1 h and then to more than 30 nm during another 1 h at 400 °C, exhibiting two distinct growth regimes. Nanocrystal growth occurs together with a structural change from zinc blende to wurtzite. The structural transition begins at 350 °C, which results in the formation of stacking faults. Increased crystallite size, comparable to the coating thickness, can improve charge separation in extremely thin absorber solar cells. We demonstrate a nearly two-fold improvement in power conversion efficiency upon annealing.

Effect of He implantation on the microstructure of zircaloy-4 studied using in situ TEM

NASA Astrophysics Data System (ADS)

Tunes, M. A.; Harrison, R. W.; Greaves, G.; Hinks, J. A.; Donnelly, S. E.

2017-09-01

Zirconium alloys are of great importance to the nuclear industry as they have been widely used as cladding materials in light-water reactors since the 1960s. This work examines the behaviour of these alloys under He ion implantation for the purposes of developing understanding of the fundamental processes behind their response to irradiation. Characterization of zircaloy-4 samples using TEM with in situ 6 keV He irradiation up to a fluence of 2.7 ×1017ions ·cm-2 in the temperature range of 298 to 1148 K has been performed. Ordered arrays of He bubbles were observed at 473 and 1148 K at a fluence of 1.7 ×1017ions ·cm-2 in αZr, the hexagonal compact (HCP) and in βZr, the body centred cubic (BCC) phases, respectively. In addition, the dissolution behaviour of cubic Zr hydrides under He irradiation has been investigated.

IN SITU Deposition of Fe-TiC Nanocomposite on Steel by Laser Cladding

NASA Astrophysics Data System (ADS)

Razavi, Mansour; Rahimipour, Mohammad Reza; Ganji, Mojdeh; Ganjali, Mansoreh; Gangali, Monireh

The possibility of deposition of Fe-TiC nanocomposite on the surface of carbon steel substrate with the laser coating method had been investigated. Mechanical milling was used for the preparation of raw materials. The mixture of milled powders was used as a coating material on the substrate steel surface and a CO2 laser was used in continuous mode for coating. Microstructural studies were performed by scanning electron microscopy. Determinations of produced phases, crystallite size and mean strain have been done by X-ray diffraction. The hardness and wear resistance of coated samples were measured. The results showed that the in situ formation of Fe-TiC nanocomposite coating using laser method is possible. This coating has been successfully used to improve the hardness and wear resistance of the substrate so that the hardness increased by about six times. Coated iron and titanium carbide crystallite sizes were in the nanometer scale.

Validation of pore network simulations of ex-situ water distributions in a gas diffusion layer of proton exchange membrane fuel cells with X-ray tomographic images

NASA Astrophysics Data System (ADS)

Agaesse, Tristan; Lamibrac, Adrien; Büchi, Felix N.; Pauchet, Joel; Prat, Marc

2016-11-01

Understanding and modeling two-phase flows in the gas diffusion layer (GDL) of proton exchange membrane fuel cells are important in order to improve fuel cells performance. They are scientifically challenging because of the peculiarities of GDLs microstructures. In the present work, simulations on a pore network model are compared to X-ray tomographic images of water distributions during an ex-situ water invasion experiment. A method based on watershed segmentation was developed to extract a pore network from the 3D segmented image of the dry GDL. Pore network modeling and a full morphology model were then used to perform two-phase simulations and compared to the experimental data. The results show good agreement between experimental and simulated microscopic water distributions. Pore network extraction parameters were also benchmarked using the experimental data and results from full morphology simulations.

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

Hu, Qin; Zhao, Lichen; Wu, Jiang

Hybrid lead halide perovskites have emerged as high-performance photovoltaic materials with their extraordinary optoelectronic properties. In particular, the remarkable device efficiency is strongly influenced by the perovskite crystallinity and the film morphology. Here, we investigate the perovskites crystallisation kinetics and growth mechanism in real time from liquid precursor continually to the final uniform film. We utilize some advanced in situ characterisation techniques including synchrotron-based grazing incident X-ray diffraction to observe crystal structure and chemical transition of perovskites. The nano-assemble model from perovskite intermediated [PbI 6] 4– cage nanoparticles to bulk polycrystals is proposed to understand perovskites formation at a molecular-more » or nano-level. A crystallisation-depletion mechanism is developed to elucidate the periodic crystallisation and the kinetically trapped morphology at a mesoscopic level. Based on these in situ dynamics studies, the whole process of the perovskites formation and transformation from the molecular to the microstructure over relevant temperature and time scales is successfully demonstrated.« less

SMA texture and reorientation: simulations and neutron diffraction studies

NASA Astrophysics Data System (ADS)

Gao, Xiujie; Brown, Donald W.; Brinson, L. Catherine

2005-05-01

With increased usage of shape memory alloys (SMA) for applications in various fields, it is important to understand how the material behavior is affected by factors such as texture, stress state and loading history, especially for complex multiaxial loading states. Using the in-situ neutron diffraction loading facility (SMARTS diffractometer) and ex situ inverse pole figure measurement facility (HIPPO diffractometer) at the Los Alamos Neutron Science Center (LANCE), the macroscopic mechanical behavior and texture evolution of Nickel-Titanium (Nitinol) SMAs under sequential compression in alternating directions were studied. The simplified multivariant model developed at Northwestern University was then used to simulate the macroscopic behavior and the microstructural change of Nitinol under this sequential loading. Pole figures were obtained via post-processing of the multivariant results for volume fraction evolution and compared quantitatively well to the experimental results. The experimental results can also be used to test or verify other SMA constitutive models.

Hard X-ray-induced damage on carbon–binder matrix for in situ synchrotron transmission X-ray microscopy tomography of Li-ion batteries

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

Lim, Cheolwoong; Kang, Huixiao; De Andrade, Vincent

2017-03-21

The electrode of Li-ion batteries is required to be chemically and mechanically stable in the electrolyte environment forin situmonitoring by transmission X-ray microscopy (TXM). Evidence has shown that continuous irradiation has an impact on the microstructure and the electrochemical performance of the electrode. To identify the root cause of the radiation damage, a wire-shaped electrode is soaked in an electrolyte in a quartz capillary and monitored using TXM under hard X-ray illumination. The results show that expansion of the carbon–binder matrix by the accumulated X-ray dose is the key factor of radiation damage. Forin situTXM tomography, intermittent X-ray exposure duringmore » image capturing can be used to avoid the morphology change caused by radiation damage on the carbon–binder matrix.« less

Design and Concept of Polyzwitterionic Copolymer Microgel Drug Delivery Systems In Situ Loaded with Non-steroidal Anti-inflammatory Ibuprofen.

PubMed

Kostova, Bistra; Kamenska, Elena; Georgieva, Dilyana; Balashev, Konstantin; Rachev, Dimitar; Georgiev, George

2017-01-01

Nowadays, the modern pharmaceutical investigations are directed toward obtaining of new polymer micro- and nano-sized drug delivery carriers. In this respect, the use of hydrogel carriers based on polyzwitterions (PZIs) is an opportunity in the preparation of polymer drug delivery systems with desired characteristics. This paper describes the synthesis and characterization of micro-structured p(VA-co-DMAPS) systems with different compositions in situ loaded with Ibuprofen by emulsifier-free emulsion copolymerization (EEC) in water. The mean size of the prepared microparticles was measured by SEM and particles have been visualized by AFM. The inclusion of Ibuprofen in the polyzwitterionic copolymer microgel systems was established by using DSC. In vitro drug release experiments were carried out in order to estimate the ability of the obtained microgels to modify the release of water-insoluble Ibuprofen.

In-situ Synchrotron X-ray Studies of the Microstructure and Stability of In 2O 3 Epitaxial Films

DOE PAGES

Highland, M. J.; Hruszkewycz, S. O.; Fong, D. D.; ...

2017-10-16

Here, we report on the synthesis, stability, and local structure of In 2O 3 thin films grown via rf-magnetron sputtering and characterized by in-situ x-ray scattering and focused x-ray nanodiffraction. We find that In 2O 3 deposited onto (001)-oriented single crystal yttria-stabilized zirconia substrates adopts a Stranski–Krastanov growth mode at a temperature of 850°C, resulting in epitaxial, truncated square pyramids with (111) side walls. We find that at this temperature, the pyramids evaporate unless they are stabilized by a low flux of In 2O 3 from the magnetron source. Lastly, we also find that the internal lattice structure of onemore » such pyramid is made up of differently strained volumes, revealing local structural heterogeneity that may impact the properties of In 2O 3 nanostructures and films.« less

In situ transmission electron microscopy of transistor operation and failure.

PubMed

Wang, Baoming; Islam, Zahabul; Haque, Aman; Chabak, Kelson; Snure, Michael; Heller, Eric; Glavin, Nicholas

2018-08-03

Microscopy is typically used as a post-mortem analytical tool in performance and reliability studies on nanoscale materials and devices. In this study, we demonstrate real time microscopy of the operation and failure of AlGaN/GaN high electron mobility transistors inside the transmission electron microscope. Loading until failure was performed on the electron transparent transistors to visualize the failure mechanisms caused by self-heating. At lower drain voltages, thermo-mechanical stresses induce irreversible microstructural deformation, mostly along the AlGaN/GaN interface, to initiate the damage process. At higher biasing, the self-heating deteriorates the gate and catastrophic failure takes place through metal/semiconductor inter-diffusion and/or buffer layer breakdown. This study indicates that the current trend of recreating the events, from damage nucleation to catastrophic failure, can be replaced by in situ microscopy for a quick and accurate account of the failure mechanisms.

Effects of a High Magnetic Field on the Microstructure of Ni-Based Single-Crystal Superalloys During Directional Solidification

NASA Astrophysics Data System (ADS)

Xuan, Weidong; Lan, Jian; Liu, Huan; Li, Chuanjun; Wang, Jiang; Ren, Weili; Zhong, Yunbo; Li, Xi; Ren, Zhongming

2017-08-01

High magnetic fields are widely used to improve the microstructure and properties of materials during the solidification process. During the preparation of single-crystal turbine blades, the microstructure of the superalloy is the main factor that determines its mechanical properties. In this work, the effects of a high magnetic field on the microstructure of Ni-based single-crystal superalloys PWA1483 and CMSX-4 during directional solidification were investigated experimentally. The results showed that the magnetic field modified the primary dendrite arm spacing, γ' phase size, and microsegregation of the superalloys. In addition, the size and volume fractions of γ/ γ' eutectic and the microporosity were decreased in a high magnetic field. Analysis of variance (ANOVA) results showed that the effect of a high magnetic field on the microstructure during directional solidification was significant ( p < 0.05). Based on both experimental results and theoretical analysis, the modification of microstructure was attributed to thermoelectric magnetic convection occurring in the interdendritic regions under a high magnetic field. The present work provides a new method to optimize the microstructure of Ni-based single-crystal superalloy blades by applying a high magnetic field.

A Data Analytics Approach to Discovering Unique Microstructural Configurations Susceptible to Fatigue

NASA Astrophysics Data System (ADS)

Jha, S. K.; Brockman, R. A.; Hoffman, R. M.; Sinha, V.; Pilchak, A. L.; Porter, W. J.; Buchanan, D. J.; Larsen, J. M.; John, R.

2018-05-01

Principal component analysis and fuzzy c-means clustering algorithms were applied to slip-induced strain and geometric metric data in an attempt to discover unique microstructural configurations and their frequencies of occurrence in statistically representative instantiations of a titanium alloy microstructure. Grain-averaged fatigue indicator parameters were calculated for the same instantiation. The fatigue indicator parameters strongly correlated with the spatial location of the microstructural configurations in the principal components space. The fuzzy c-means clustering method identified clusters of data that varied in terms of their average fatigue indicator parameters. Furthermore, the number of points in each cluster was inversely correlated to the average fatigue indicator parameter. This analysis demonstrates that data-driven methods have significant potential for providing unbiased determination of unique microstructural configurations and their frequencies of occurrence in a given volume from the point of view of strain localization and fatigue crack initiation.

Thermally Stable Nanocrystalline Steel

NASA Astrophysics Data System (ADS)

Hulme-Smith, Christopher Neil; Ooi, Shgh Woei; Bhadeshia, Harshad K. D. H.

2017-10-01

Two novel nanocrystalline steels were designed to withstand elevated temperatures without catastrophic microstructural changes. In the most successful alloy, a large quantity of nickel was added to stabilize austenite and allow a reduction in the carbon content. A 50 kg cast of the novel alloy was produced and used to verify the formation of nanocrystalline bainite. Synchrotron X-ray diffractometry using in situ heating showed that austenite was able to survive more than 1 hour at 773 K (500 °C) and subsequent cooling to ambient temperature. This is the first reported nanocrystalline steel with high-temperature capability.

Modeling deformation behavior of Cu-Zr-Al bulk metallic glass matrix composites

NASA Astrophysics Data System (ADS)

Pauly, S.; Liu, G.; Wang, G.; Das, J.; Kim, K. B.; Kühn, U.; Kim, D. H.; Eckert, J.

2009-09-01

In the present work we prepared an in situ Cu47.5Zr47.5Al5 bulk metallic glass matrix composite derived from the shape memory alloy CuZr. We use a strength model, which considers percolation and a three-microstructural-element body approach, to understand the effect of the crystalline phase on the yield stress and the fracture strain under compressive loading, respectively. The intrinsic work-hardenability due to the martensitic transformation of the crystalline phase causes significant work hardening also of the composite material.

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.

Applications of synchrotron radiation to materials science: Diffraction imaging (topography) and microradiography

NASA Technical Reports Server (NTRS)

Kuriyama, Masao

1988-01-01

Synchrotron radiation sources are now available throughout the world. The use of hard X-ray radiation from these sources for materials science is described with emphasis on diffraction imaging for material characterization. With the availability of synchrotron radiation, real-time in situ measurements of dynamic microstructural phenomena have been started. This is a new area where traditional application of X-rays has been superseded. Examples are chosen from limited areas and are by no means exhaustive. The new emerging information will, no doubt, have great impact on materials science and engineering.

Passivation and alloying element retention in gas atomized powders

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

Heidloff, Andrew J.; Rieken, Joel R.; Anderson, Iver E.

A method for gas atomization of a titanium alloy, nickel alloy, or other alumina (Al.sub.2O.sub.3)-forming alloy wherein the atomized particles are exposed as they solidify and cool in a very short time to multiple gaseous reactive agents for the in-situ formation of a passivation reaction film on the atomized particles wherein the reaction film retains a precursor halogen alloying element that is subsequently introduced into a microstructure formed by subsequent thermally processing of the atomized particles to improve oxidation resistance.

Pectic homogalacturonan masks abundant sets of xyloglucan epitopes in plant cell walls.

PubMed

Marcus, Susan E; Verhertbruggen, Yves; Hervé, Cécile; Ordaz-Ortiz, José J; Farkas, Vladimir; Pedersen, Henriette L; Willats, William G T; Knox, J Paul

2008-05-22

Molecular probes are required to detect cell wall polymers in-situ to aid understanding of their cell biology and several studies have shown that cell wall epitopes have restricted occurrences across sections of plant organs indicating that cell wall structure is highly developmentally regulated. Xyloglucan is the major hemicellulose or cross-linking glycan of the primary cell walls of dicotyledons although little is known of its occurrence or functions in relation to cell development and cell wall microstructure. Using a neoglycoprotein approach, in which a XXXG heptasaccharide of tamarind seed xyloglucan was coupled to BSA to produce an immunogen, we have generated a rat monoclonal antibody (designated LM15) to the XXXG structural motif of xyloglucans. The specificity of LM15 has been confirmed by the analysis of LM15 binding using glycan microarrays and oligosaccharide hapten inhibition of binding studies. The use of LM15 for the analysis of xyloglucan in the cell walls of tamarind and nasturtium seeds, in which xyloglucan occurs as a storage polysaccharide, indicated that the LM15 xyloglucan epitope occurs throughout the thickened cell walls of the tamarind seed and in the outer regions, adjacent to middle lamellae, of the thickened cell walls of the nasturtium seed. Immunofluorescence analysis of LM15 binding to sections of tobacco and pea stem internodes indicated that the xyloglucan epitope was restricted to a few cell types in these organs. Enzymatic removal of pectic homogalacturonan from equivalent sections resulted in the abundant detection of distinct patterns of the LM15 xyloglucan epitope across these organs and a diversity of occurrences in relation to the cell wall microstructure of a range of cell types. These observations support ideas that xyloglucan is associated with pectin in plant cell walls. They also indicate that documented patterns of cell wall epitopes in relation to cell development and cell differentiation may need to be re-considered in relation to the potential masking of cell wall epitopes by other cell wall components.