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At least 379 records · Page 21

Advanced composite applications for sub-micron biologically derived microstructures

A major thrust of advanced material development is in the area of self-assembled ultra-fine particulate based composites (micro-composites). The application of biologically derived, self-assembled microstructures to form advanced composite materials is discussed. Hollow 0.5 micron diameter cylindrical shaped microcylinders self-assemble from diacetylenic lipids. These microstructures have a multiplicity of potential applications in the material sciences. Exploratory development is proceeding in application areas such as controlled release for drug delivery, wound repair, and biofouling as well as composites for electronic and magnetic applications, and high power microwave cathodes.

Schnur, J. M.↗

Mechanical Properties and Microstructural Characterization of Particulate Reinforced Diboride Composites for High Temperature Leading Edge Applications

Previous work on refractory diboride composites has shown that these systems have the potential for use in high temperature leading edge applications for reusable reentry vehicles. Experiments in reentry environments have shown that these materials have multiple use temperatures greater than 1900 C. The work to be discussed focuses on three compositions: HfB2/SiC, ZrB2/SiC, and ZrB2/C/SiC. These composites have been hot pressed and their mechanical properties measured at room and elevated temperatures. Extensive microstructural characterization has been conducted on polished cross sections and the fracture surfaces have been examined to determine their failure origins.

Ellerby, Donald T.↗

Mechanical Properties and Microstructural Characterization of Particulate Reinforced Diboride Composites for High Temperature Leading Edge Applications

Previous work on refractory diboride composites has shown that these systems have the potential for use in high temperature leading edge applications for reusable reentry vehicles. Experiments in reentry environments have shown that these materials have multiple use temperatures greater than 1900 C. The work to be discussed focuses on three compositions: HfB2/SiC, ZrB2/SiC, and ZrB2/C/SiC. These composites have been hot pressed and their mechanical properties measured at room and elevated temperatures. Extensive microstructural characterization has been conducted on polished cross sections and the fracture surfaces have been examined to determine their failure origins.

Ellerby, Donald T.↗

The influence of cobalt, tantalum, and tungsten on the microstructure of single crystal nickel-base superalloys

The influence of composition on the microstructure of single crystal nickel-base superalloys was investigated. Co was replaced by Ni, and Ta was replaced by either Ni or W, according to a matrix of compositions based on MAR-M247. Substitution of Ni for Co caused an increase in gamma-prime solvus temperature, an increase in gamma-gamma-prime lattice mismatch, and the precipitation of W-rich phases in the alloys with high refractory metal levels. Substitution of Ni for Ta caused large decreases in gamma-prime solvus temperature, gamma-prime volume fraction, and gamma-gamma-prime lattice mismatch, whereas substitution of W for Ta resulted in smaller decreases in these features. For the alloys with gamma-prime particles that remained coherent, substitution of Ni for Co caused an increase in gamma-prime coarsening rate. The two alloys with the largest magnitude of lattice mismatch possessed gamma-prime particles which lost coherency during unstressed aging and exhibited anomalously low coarsening rates. Creep exposure at 1000 C resulted in the formation of gamma-prime lamellae oriented perpendicular to the applied stress axis in all alloys.

Nathal, M. V.↗

The influence of microstructure on the tensile behavior of an aluminum metal matrix composite

The relationship between tensile properties and microstructure of a powder metallurgy aluminum alloy, 2009 was examined. The alloy was investigated both unreinforced and reinforced with 15 v/o SiC whiskers or 15 v/o SiC particulate to form a discontinuous metal matrix composite (MMC). The materials were investigated in the as-fabricated condition and in three different hot-rolled sheet thicknesses of 6.35, 3.18, and 1.8 mm. Image analysis was used to characterize the morphology of the reinforcements and their distributions within the matrix alloy. Fractographic examinations revealed that failure was associated with the presence of microstructural inhomogeneities which were related to both the matrix alloy and to the reinforcement. The results from these observations together with the matrix tensile data were used to predict the strengths and moduli of the MMC's using relatively simple models. The whisker MMC could be modeled as a short fiber composite and an attempt was made to model the particulate MMC as a dispersion/dislocation hardened alloy.

Birt, Michael J.↗

Non-equilibrium phase distribution in an Al-SiC composite

The phase distribution in an Al-SiC composite has been investigated using high resolution analytical electron microscopy. Particular attention was focused on Al-SiC interfaces, matrix boundaries and impurity phases which would impede the easy glide of dislocations. Small crystallites of MgO were distributed singly and in clusters along Al-SiC interfaces in all specimens. Interfacial segregation and precipitation involving alloy species apparently affected precipitation in the matrix, where the distribution of phases was found to be very heterogeneous. Matrix phases also included unusually large constituent particles and dispersoids, a consequence of the composite processing methods. The relationship between the observed microstructure and the composite mechanical behavior reported by others is discussed. The heterogeneous distribution of matrix phases is expected to result in a wide variaiton in local yield stress and local work-hardening rate within the composite.

Nutt, S. R.↗

Microstructural Preparation and Examination of Polymer-Matrix Composites

Adapting procedures widely used in the metallographic characterization of metals and alloys, the microstructural preparation and examination of three polymer-matrix composites (PMC's) is described. The materials investigated contained either hollow ceramic filler particles or woven, continuous carbon/graphite fibers. Since the two particulate composites were considered to be isotropic, only one sample orientation was prepared. For the fiber composite, both longitudinal and planar orientations were studied. Once prepared, the samples were examined using reflected light microscopy. A number of microstructural features were evaluated qualitatively, including porosity and cracks, filler-matrix interfacial bonding, filler particle characteristics (shape, size, size distribution, and loading variation) and fiber characteristics (orientation, packing variation, and discontinuities).

Elban, Wayne L.↗

Compositional Effects on Nickel-Base Superalloy Single Crystal Microstructures

Fourteen nickel-base superalloy single crystals containing 0 to 5 wt% chromium (Cr), 0 to 11 wt% cobalt (Co), 6 to 12 wt% molybdenum (Mo), 0 to 4 wt% rhenium (Re), and fixed amounts of aluminum (Al) and tantalum (Ta) were examined to determine the effect of bulk composition on basic microstructural parameters, including gamma' solvus, gamma' volume fraction, volume fraction of topologically close-packed (TCP) phases, phase chemistries, and gamma - gamma'. lattice mismatch. Regression models were developed to describe the influence of bulk alloy composition on the microstructural parameters and were compared to predictions by a commercially available software tool that used computational thermodynamics. Co produced the largest change in gamma' solvus over the wide compositional range used in this study, and Mo produced the largest effect on the gamma lattice parameter and the gamma - gamma' lattice mismatch over its compositional range, although Re had a very potent influence on all microstructural parameters investigated. Changing the Cr, Co, Mo, and Re contents in the bulk alloy had a significant impact on their concentrations in the gamma matrix and, to a smaller extent, in the gamma' phase. The gamma phase chemistries exhibited strong temperature dependencies that were influenced by the gamma and gamma' volume fractions. A computational thermodynamic modeling tool significantly underpredicted gamma' solvus temperatures and grossly overpredicted the amount of TCP phase at 982 C. Furthermore, the predictions by the software tool for the gamma - gamma' lattice mismatch were typically of the wrong sign and magnitude, but predictions could be improved if TCP formation was suspended within the software program. However, the statistical regression models provided excellent estimations of the microstructural parameters based on bulk alloy composition, thereby demonstrating their usefulness.

MacKay, Rebecca A.↗

Continuous fiber-reinforced titanium aluminide composites

An account is given of the fabrication techniques, microstructural characteristics, and mechanical behavior of a lightweight, high service temperature SiC-reinforced alpha-2 Ti-14Al-21Nb intermetallic-matrix composite. Fabrication techniques under investigation to improve the low-temperature ductility and environmental resistance of this material system, while reducing manufacturing costs to competitive levels, encompass powder-cloth processing, foil-fiber-foil processing, and thermal-spray processing. Attention is given to composite microstructure problems associated with fiber distribution and fiber-matrix interfaces, as well as with mismatches of thermal-expansion coefficient; major improvements are noted to be required in tensile properties, thermal cycling effects, mechanical damage, creep, and environmental effects.

Mackay, R. A.↗

Tailoring composition and deformation modes at the microstructural level for next generation low-cost high-strength austenitic stainless steels

The objective of this project is to enable deliberate development of cost-effective, hydrogen resistant alloys by establishing detailed relationships specific to the effects of alloy composition, short-range order (SRO), and microsegregation in the presence of hydrogen on the transition between homogeneous deformation and localized plasticity in shear bands. In collaboration with the International Institute for Carbon-Neutral Energy Research, I2CNER, at Kyushu University in Japan, we conceptualized, designed, and manufactured four austenitic alloys that maintain corrosion resistance and ensure lower cost relative to baseline commercial alloys. The mechanical properties and deformation modes of the novel alloys (KU alloys) were assessed in the presence of hydrogen (H). Correlations between composition and performance revealed that two of the KU alloys are suitable replacements for 316 steel, while another is a viable replacement for 304 steel at room temperature. We found that, in the presence of other austenite stabilizing elements namely Mn and N, replacing Ni with Cu does not lead to martensite formation as has been previously reported.1–3 Furthermore, we found that the addition of Cu leads to an earlier onset of multiple slip resulting in an relative earlier onset of a higher work hardening rate (WHR). Greater understanding of the relationships between alloy composition and SRO required the development of a novel advanced electron diffraction methodology to characterize SRO in complex FCC alloys. This innovative approach, which combines fluctuation and correlation analyses of diffuse-scattering signals, successfully differentiated between SRO and long-range ordering (LRO). Further investigations into annealed austenitic stainless steels could provide insights into manipulating SRO and its effects on material properties. Atomistic simulations provided understanding of SRO behavior that was difficult to capture experimentally. This project created the first spin cluster expansion model that is able to capture and describe SRO effects in Fe-Ni-Cr FCC alloys, accounting for the non-negligible effects of magnetism. An automated computational workflow was established to provide reliable predictions of SRO in Fe-Ni-Cr austenitic alloys, both with and without the presence of H atoms. Analysis of the propensity for SRO in Fe-Ni-Cr alloys revealed that H tends to cluster with specific, well-defined SRO domains. The computational framework is general purpose and can be extended to realistic stainless steels across diverse composition ranges. With confidence that SRO is possible in austenitic stainless steels, we developed a discrete dislocation finite element code to understand the interaction of dislocations with SRO in the presence of H. By incorporating H effects on the dislocation emission and SRO stress field we show that the critical stress for the dislocation pileup to breakthrough the SRO domain decreases in the presence of H, which directly contributes localized deformation at the macroscale. Through the simulation of a uniaxial tension test, we demonstrated that H-induced weakening of SRO stress field and H-enhanced dislocation emission can lead to the onset of shear localization at lower macroscopic strains. As a whole, this project identified three novel alloys that show improvements in performance and cost efficiency for H-facing applications by studying correlations between alloy chemistry and deformation behavior. We also made significant advancements to experimental and computational methodologies necessary to study the chemistry and distribution of SRO across a range of alloys, which in turn allowed us to demonstrate how deformation mechanisms change due to the contributions of SRO in austenitic alloys in the presence of H. The combined advancements in fundamental understanding with novel alloy development in this project has increased the viability of next generation H-technologies for the broader public through accessible low-cost alloys and accelerated development towards future H-infrastructure.

08 HYDROGEN↗

SiC Fiber-Reinforced Celsian Composites

Celsian is a promising matrix material for fiber-reinforced composites for high temperature structural applications. Processing and fabrication of small diameter multifilament silicon carbide tow reinforced celsian matrix composites are described. Mechanical and microstructural properties of these composites at ambient and elevated temperatures are presented. Effects of high-temperature exposures in air on the mechanical behavior of these composites are also given. The composites show mechanical integrity up to ~1100 C but degrade at higher temperatures in oxidizing atmospheres. A model has been proposed for the degradation of these composites in oxidizing atmospheres at high temperatures.

Bansal, Narottam P.↗

Microstructure, mechanical, and thermal properties of compositionally complex (Hf,Zr,Nb,Ti)B 2 ‒LaB 6 ceramics

Novel compositionally complex borides, (Hf,Zr,Nb,Ti)B 2 and (Hf,Zr,Nb,Ti)B 2 ‒LaB 6 , were fabricated using spark plasma sintering process. (Hf,Zr,Nb,Ti)B 2 ‒LaB 6 exhibits a dual-phase microstructure, in which (Hf,Zr,Nb,Ti)B 2 is a primary phase with the hexagonal structure and LaB 6 is a secondary phase with a cubic structure. The mechanical properties of both (Hf,Zr,Nb,Ti)B 2 and (Hf,Zr,Nb,Ti)B 2 ‒LaB 6 are comparable, with a combination of high hardness and moderate fracture toughness. Thermal diffusivity and conductivity of (Hf,Zr,Nb,Ti)B 2 are much lower than the individual transition metal borides but are significantly increased by the addition of LaB 6 . Herein, it is implied that the thermal properties of boride ceramics can be controlled through the appropriate design of principal metal element compositions.

borides↗

Automated Grain Boundary (GB) Segmentation and Microstructural Analysis in 347H Stainless Steel Using Deep Learning and Multimodal Microscopy

Austenitic 347H stainless steel offers superior mechanical properties and corrosion resistance required for extreme operating conditions such as high temperature. The change in microstructure due to composition and process variations is expected to impact material properties. Identifying microstructural features such as grain boundaries thus becomes an important task in the process-microstructure-properties loop. Applying convolutional neural network (CNN)-based deep learning models is a powerful technique to detect features from material micrographs in an automated manner. In contrast to microstructural classification, supervised CNN models for segmentation tasks require pixel-wise annotation labels. However, manual labeling of the images for the segmentation task poses a major bottleneck for generating training data and labels in a reliable and reproducible way within a reasonable timeframe. Microstructural characterization especially needs to be expedited for faster material discovery by changing alloy compositions. Here, in this study, we attempt to overcome such limitations by utilizing multimodal microscopy to generate labels directly instead of manual labeling. We combine scanning electron microscopy images of 347H stainless steel as training data and electron backscatter diffraction micrographs as pixel-wise labels for grain boundary detection as a semantic segmentation task. The viability of our method is evaluated by considering a set of deep CNN architectures. We demonstrate that despite producing instrumentation drift during data collection between two modes of microscopy, this method performs comparably to similar segmentation tasks that used manual labeling. Additionally, we find that naïve pixel-wise segmentation results in small gaps and missing boundaries in the predicted grain boundary map. By incorporating topological information during model training, the connectivity of the grain boundary network and segmentation performance is improved. Finally, our approach is validated by accurate computation on downstream tasks of predicting the underlying grain morphology distributions which are the ultimate quantities of interest for microstructural characterization.

36 MATERIALS SCIENCE↗

Aluminum alloy compositions and methods of making and using the same

The present disclosure concerns embodiments of aluminum alloy compositions exhibiting superior microstructural stability and strength at high temperatures. The disclosed aluminum alloy compositions comprise particular combinations of components that contribute the ability of the alloys to exhibit improved microstructural stability and hot tearing resistance as compared to conventional alloys. Also disclosed herein are embodiments of methods of making and using the alloys.

Shyam, Amit↗

Effect of electrochemical cycling on microstructures of nanocomposite silicon electrodes using hyperpolarized 129 Xe and 7 Li NMR spectroscopy

The microstructural stability of composite electrodes during electrochemical cycling is critically important as it dictates the performance of Li-ion batteries. The issue becomes even more important for the high capacity alloying anode such as silicon that typically exhibits dramatic lithiation–delithiation-induced volume changes. The solid electrolyte interphase (SEI) layer formed on the active electrode surface has a profound effect on the overall microstructural stability of composite electrodes. An ideal SEI layer allows Li+ ions in and out of the electrode, but is an insulator to electrons, preventing the electrolyte from being further reduced. However, the SEI layers formed during initial lithiation may experience changes or degradation with subsequent cycling, adversely affecting the electrode performance. A combination of hyperpolarized 129 Xe and 7 Li nuclear magnetic resonance spectroscopies was applied to probe the microstructures of nanocomposite silicon electrodes at various stages of the lithiation–delithiation cycle. The results obtained from this study shed light on the degradation mechanism of nanocomposite Si electrodes upon electrochemical cycling and should prove useful in the effort to design more robust electrodes in the future.

36 MATERIALS SCIENCE↗

In Situ Structural and Electrical Conductivity Characterization of Sr2MMoO6-δ Double Perovskite Solid Oxide Fuel Cell Anode Materials

In this study, a series of Sr 2 MMoO 6-δ double perovskite solid oxide fuel cell (SOFC) anode materials (where 0 <= δ <= 0.041 and M = Fe, Co, or Ni) were synthesized, and the changes in their morphologies under relevant SOFC operating conditions were explored. Ultra-small-angle X-ray scattering (USAXS), small-angle X-ray scattering (SAXS), and wide-angle X-ray scattering (WAXS) were used to determine changes in the microstructures and phase compositions of the anode materials at high temperatures and under a reducing atmosphere. The stability of the double perovskite structure was found to be highly dependent on the identity of the cation M, such that when M = Fe, the material remained stable over the course of the experiments. However, when M = Co or Ni, significant changes in the microstructure and phase composition were observed. An in situ study of the M = Co sample, in which electrical conductivity and USAXS/SAXS/WAXS measurements were conducted simultaneously, revealed the structural degradation mechanisms and electrical conductivity changes over a range of temperatures. To conduct these measurements, a cell was developed that allowed for a sample mounted on Pt wires to be placed in the X-ray beam and heated under gas flow comprising 4% mass H 2 and 96% mass N 2 . The resulting measurements allowed for the direct comparison of the electrical and morphological changes occurring in the material under operating conditions, such that increases in conductivity could be attributed to the growth of new phases.

25 ENERGY STORAGE↗

A Finite Difference Analysis of the Effect of Graphene Additions on the Electrical Conductivity of Polycrystalline Copper

A finite-difference method was used to explore the effect of graphene on the bulk electrical conductivity of copper-graphene composites. In this capacity, grain orientation information from pure copper and copper-graphene composites were used to generate synthetic 3D microstructures. The electrical conductivity of these microstructures were calculated using the finite difference method assuming different average grain sizes. From these calculations, we demonstrate that when high-conductivity grain boundaries are present within the microstructure arising from the presence of graphene, an increase in the bulk electrical conductivity is observed. On the other hand, the difference in textures between copper and copper-graphene composites may not account for a significant difference in bulk electrical conductivity. In comparison, the copper grain size has a considerably larger effect on electrical conductivity as previously anticipated. This is one of the first demonstrations of a physical basis for enhanced conductivity composites and presents pathways for further investigations on the effects of composite microstructural features, material interfaces and graphene content on electrical performance.

Frazier, William E.↗

3-D reconstruction and microstructural characterization of neutron-irradiated U-10Zr fuel using FIB-SEM serial sectioning

Herein, focused ion beam-scanning electron microscopy serial sectioning was applied to characterize the three-dimensional (3-D) porosity and phase regions of a neutron-irradiated U-10 wt% Zr fuel. The specimen was removed from an intermediate radial region of a fuel pin irradiated to 5.7 at.% burn-up. Backscattered electron imaging and energy-dispersive spectroscopy were performed on each serial section, allowing for the characterization of microstructural morphology and composition. Porosity size followed a lognormal distribution, ranging from 1.46 × 10 –4 to 25.58 µm 3 with a total porosity volume fraction of 13.02%. Distinctive microstructural regions were identified by composition and porosity: (1) a Zr-rich region with an average composition of 28.4 wt% Zr and a local porosity fraction of 6.88%, and (2) a U-rich region with an average composition of 97.0 wt% U and a local porosity fraction of 14.11%; subdivided into U-rich—high porosity (16.68%) and U-rich—low porosity (8.04%) regions. The detailed 3-D compositional and porosity regions can improve nuclear fuel performance codes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗