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At least 19 records

An efficient algorithm for generating diverse microstructure sets and delineating properties closures

Properties closures delineate the theoretical objective space for materials design problems, allowing designers to make informed trade-offs between competing constraints and target properties. In this paper, we present a new algorithm called hierarchical simplex sampling (HSS) that approximates properties closures more efficiently and faithfully than traditional optimization based approaches. By construction, HSS generates samples of microstructure statistics that span the corresponding microstructure hull. As a result, we also find that HSS can be coupled with synthetic polycrystal generation software to generate diverse sets of microstructures for subsequent mesoscale simulations. Finally, by more broadly sampling the space of possible microstructures, it is anticipated that such diverse microstructure sets will expand our understanding of the influence of microstructure on macroscale effective properties and inform the construction of higher-fidelity mesoscale structure-property models.

36 MATERIALS SCIENCE↗

Microstructure and growth model for rice-hull-derived SiC whiskers

The microstructure of silicon carbide whiskers grown from rice hulls has been studied using methods of high-resolution analytical electron microscopy. Small, partially crystalline inclusions (about 10 nm) containing calcium, manganese, and oxygen are concentrated in whisker core regions, while peripheral regions are generally inclusion free. The distinct microphase distribution is evidence of a two-stage growth process in which the core region grows first, followed by normal growth toward whisker sides. Partial dislocations extend radially from the core region to the surface and tend to be paired in V-shaped configurations. Whisker surfaces exhibit microroughness due to a tendency to develop small facets on close-packed planes. The microstructural data obtained from TEM observations are used as a basis for discussion of the mechanisms involved in whisker growth, and a model of the growth process is proposed. The model includes a two-dimensional growth mechanism involving vapor, liquid, and solid phases, although it is significantly different from the classical vapor-liquid-solid (VLS) process of whisker growth.

Nutt, Steven R.↗

The Effects of Seven Alloying Elements on the Microstructure and Stress-Rupture Behavior of Nickel-Base Superalloys

Seven alloying elements: Al, Cr, Ti, Nb, Ta, Mo, and W were added at two levels of concentration to produce a series of experimental nickel-base superalloys. Fifty alloys, representing a fraction of a 2 to the 7th power factorial design, were cast, tested, and analyzed. Each alloy's microstructure was characterized by phase extractions, X-ray diffraction, metallography and energy dispersive X-ray spectroscopy. Regression analysis was used to determine the effect of alloying element content on microstructure and stress-rupture life.

Hull, D. R.↗

As-received microstructure of a SiC/Ti-15-3 composite

A silicon carbide fiber reinforced titanium (Ti-15V-3Cr-3Sn-3Al) composite is metallographically examined. Several methods for examining composite materials are investigated and documented. Polishing techniques for this material are described. An interference layering method is developed to reveal the structure of the fiber, the reaction zone, and various phases within the matrix. Microprobe and transmission electron microscope (TEM) analyses are performed on the fiber/matrix interface. A detailed description of the fiber distribution as well as the microstructure of the fiber and matrix are presented.

Lerch, Bradley A.↗

Microstructure of a SiC/Ti-15-3 composite

A continuous SiC-fiber-reinforced titanium (Ti-15V-3Cr-3Sn-3A1) composite was metallographically examined. Several methods for examining composite materials were investigated and documented. Polishing techniques for this material are described. An interference layering method was developed to reveal the structure of the fiber, the reaction zone, and various phases within the matrix. Microprobe and TEM analyses were performed on the fiber-matrix interface. Detailed descriptions of the fiber distribution and the microstructure of the fiber and matrix are presented.

Lerch, B. A.↗

Fatigue failure of regenerator screens in a high frequency Stirling engine

Failure of Stirling Space Power Demonstrator Engine (SPDE) regenerator screens was investigated. After several hours of operation the SPDE was shut down for inspection and on removing the regenerator screens, debris of unknown origin was discovered along with considerable cracking of the screens in localized areas. Metallurgical analysis of the debris determined it to be cracked-off-deformed pieces of the 41 micron thickness Type 304 stainless steel wire screen. Scanning electron microscopy of the cracked screens revealed failures occurring at wire crossovers and fatigue striations on the fracture surface of the wires. Thus, the screen failure can be characterized as a fatigue failure of the wires. The crossovers were determined to contain a 30 percent reduction in wire thickness and a highly worked microstructure occurring from the manufacturing process of the wire screens. Later it was found that reduction in wire thickness occurred because the screen fabricator had subjected it to a light cold-roll process after weaving. Installation of this screen left a clearance in the regenerator allowing the screens to move. The combined effects of the reduction in wire thickness, stress concentration (caused by screen movement), and highly worked microstructure at the wire crossovers led to the fatigue failure of the screens.

Hull, David R.↗

Fatigue failure of regenerator screens in a high frequency Stirling engine

Failure of Stirling Space Power Demonstrator Engine (SPDE) regenerator screens was investigated. After several hours of operation the SPDE was shut down for inspection and on removing the regenator screens, debris of unknown origin was discovered along with considerable cracking of the screens in localized areas. Metallurgical analysis of the debris determined it to be cracked-off-deformed pieces of the 41 micron thickness Type 304 stainless steel wire screen. Scanning electron microscopy of the cracked screens revealed failures occurring at wire crossovers and fatigue striations on the fracture surface of the wires. Thus, the screen failure can be characterized as a fatigue failure of the wires. The crossovers were determined to contain 30 percent reduction in wire thickness and a highly worked microstructure occurring from the manufacturing process of the wire screens. Later it was found that reduction in wire thickness occurred because the screen fabricator had subjected it to a light cold-roll process after weaving. Installation of this screen left a clearance in the regenerator allowing the screens to move. The combined effects of the reduction in wire thickness, stress concentration (caused by screen movement), and highly worked microstructure at the wire crossovers led to the fatigue failure of the screens.

Hull, David R.↗

In Situ Transmission Electron Microscopy of High-Temperature Inconel-625 Corrosion by Molten Chloride Salts

This paper describes an approach to monitor high temperature molten chloride (MgCl 2 -NaCl-KCl) salt corrosion of Inconel-625 alloy in real time at high spatial resolution. The approach is based on a micro-environmental-cell assembly integrated into a transmission-electron-microscope goniometer to examine in situ the salt-alloy interface during corrosion, employing real time electron diffraction and imaging. It establishes procedures to minimize incorporation of H 2 O or O 2 from atmosphere in the chloride salts during sample fabrication and corrosion, which is critical to understanding the fundamental corrosion mechanisms. A clustering algorithm and a 2D Gaussian fit function are used to determine diffraction spot intensities in in situ diffraction patterns, to quantify alloy corrosion. This facilitates quantitative observation of the evolution of individual grains, in contrast to conventional macroscopic corrosion rate quantification. The isothermal corrosion rate of Inconel-625 in an anhydrous, unoxidized salt-stack is 220 ± 30 μm year -1 at 700 °C and 350 ± 20 μm year -1 at 800 °C. However, the corrosion rate at 700 °C increases five-fold to 1000 ± 170 μm year -1 when the salt stack is air-exposed, indicating the dominant effects of hydrated or oxidized impurities on corrosion acceleration. Furthermore, real time imaging of the microstructure evolution suggests that corrosion is initiated at grain boundaries.

14 SOLAR ENERGY↗

Effects of Morphology and Geometry of Inclusions on Two-Point Correlation Statistics in Two Phase Composites

A spectral form of the two-point correlation functions for two-phase composites is presented and the effects of secondary phase morphology, geometry and volume fraction on the coefficients of the corresponding series are studied. Initially, a principal component analysis is performed on the coefficients of the series and then, the effects of different morphological and geometrical parameters of the second phase inclusions on two-point correlation functions are examined. A direct linkage between the principal components of the coefficients with the morphological features (inclusion shape, aspect ratio and size) is established and the influence of preferred orientation of the anisotropic inclusions is also investigated. Finally a composite hull is constructed using the principal components of the coefficients in a three-dimensional space, which helps in determining the interrelation of properties and microstructures of any composite containing these types of inclusions.

97 MATHEMATICS AND COMPUTING↗

Microstructure Of A SIC/(Ti/V/Cr/Sn/Al) Composite

NASA technical memorandum reports on analysis of composite material made of SiC fibers in matrix of 0.76 Ti/0.15 V/0.03 Cr/0.03 Sn/0.03 Al (parts by weight) alloy. Purposes of study to investigate suitability of some metallographic techniques for use on composite materials in general and to obtain information about macrostructure and microstructure of this specific composite to provide guidance for experimental and theoretical studies of more advanced composites.

Lerch, Bradley A.↗

Correlative electron and ion beam analysis of the electrochemical performances of LiV 3 O 8 cathode films as a function of microstructures

Degradation mechanisms in LiV 3 O 8 cathode films (~500 nm) with different initial microstructures i.e., globular nanocrystals in amorphous matrix and needle-like nanocrystals, synthesized by annealing the cathodes at 150 °C and 300 °C for 6 h are studied by Transmission Electron Microscopy (TEM) and Auger Electron Spectroscopy (AES). In addition, a unique in-situ combination of TEM and Secondary Ion Mass Spectrometry (SIMS) imaging techniques, namely Parallel Ion and Electron beam Spectrometry (PIES) is carried out to measure the 3D distribution of V and Li with nanoscale resolution. These characterization studies focus on correlating the pre- and post-cycling microstructure to observed electrochemical performance. The LiV 3 O 8 cathode film with needle-like nanocrystals (300 °C) shows a higher initial capacity but it degrades rapidly compared to the film with globular nanocrystals embedded in amorphous matrix (150 °C). We observed that LiV 3 O 8 films with needle-like nanocrystals are more susceptible to cathode decohesion and vanadium dissolution than the films with globular nanocrystals embedded in amorphous matrix, explaining the differences in their electrochemical performance. The findings from this study have relevance to the development of thin film electrode microstructures for high capacity and cyclic stability.

25 ENERGY STORAGE↗

Characterization of Shocked Beryllium

Beryllium metal has many excellent structural properties in addition to its unique radiation characteristics, including: high elastic modulus, low Poisson's ratio, low density, and high melting point. However, it suffers from several major mechanical drawbacks: 1) high anisotropy - due to its hexagonal lattice structure and its susceptibility to crystallographic texturing; 2) susceptibility to impurity-induced fracture - due to grain boundary segregation; and 3) low intrinsic ductility at ambient temperatures thereby limiting fabricability. While large ductility results from deformation under the conditions of compression, the material can exhibit a brittle behavior under tension. Furthermore, there is a brittle to ductile transition at approximately 200 C under tensile conditions. While numerous studies have investigated the low-strain-rate constitutive response of beryllium, the combined influence of high strain rate and temperature on the mechanical behavior and microstructure of beryllium has received limited attention over the last 40 years. Prior studies have focused on tensile loading behavior, or limited conditions of dynamic strain rate and/or temperature. The beryllium used in this study was Grade S200-F (Brush Wellman, Inc., Elmore, OH) material. The work focused on high strain rate deformation and examine the validity of constitutive models in deformation rate regimes, including shock, the experiments were modeled using a Lagrangian hydrocode. Two constitutive strength (plasticity) models, the Preston-Tonks-Wallace (PTW) and Mechanical Threshold Stress (MTS) models, were calibrated using the same set of quasi-static and Hopkinson bar data taken at temperatures from 77K to 873K and strain rates from 0.001/sec to 4300/sec. In spite of being calibrated on the same data, the two models give noticeably different results when compared with the measured wave profiles. These high strain rate tests were conducted using both explosive drive and a gas gun to accelerate the material. Preliminary analysis of the results appears to indicate that, if fractured by the initial shock loading, the S200F Be remains sufficiently intact to support a shear stress following partial release and subsequent shock re-loading of the material. Additional 'arrested' drive shots were designed and tested to minimize the reflected tensile pulse in the sample. These tests were done to both validate the model and to put large shock induced compressive loads into the beryllium sample.

36 MATERIALS SCIENCE↗

Ultrasonic Inspection With Angular-Power-Spectrum Scanning

Principal advantage of angular-power-spectrum scanning (APSS) is that, unlike x-radiography and prior ultrasonic techniques, it reveals subtle distributions of microstructural features; e.g., variations in densities of micropores or regions in which fibers and matrices are poorly bonded to each other. Potential applications include development and characterization of composite-material components of large structures, such as buildings and bridges; determination of quality and detection of damage in fiberglass hulls, surfboards, ladders, and scaffolds; and development of porous prosthetic skins and complicated "smart" materials. Superposed diffraction patterns give clues to internal structural features of ceramic composites.

Generazio, Edward R.↗

Interrelation of material microstructure, ultrasonic factors, and fracture toughness of two phase titanium alloy

The pivotal role of an alpha-beta phase microstructure in governing fracture toughness in a titanium alloy, Ti-662, is demonstrated. The interrelation of microstructure and fracture toughness is demonstrated using ultrasonic measurement techniques originally developed for nondestructive evaluation and material property characterization. It is shown that the findings determined from ultrasonic measurements agree with conclusions based on metallurgical, metallographic, and fractographic observations concerning the importance of alpha-beta morphology in controlling fracture toughness in two phase titanium alloys.

Vary, A.↗

Characterization of Irradiated Metal Waste from the Pyrometallurgical Treatment of Used EBR-II Fuel

As part of the pyrometallurgical treatment of used Experimental Breeder Reactor-II fuel, a metal waste stream is generated consisting primarily of cladding hulls laden with fission products noble to the electrorefining process. Consolidation by melting at high temperature [1873 K (1600 degrees C)] has been developed to sequester the noble metal fission products (Zr, Mo, Tc, Ru, Rh, Te, and Pd) which remain in the iron-based cladding hulls. Zirconium from the uranium fuel alloy (U-10Zr) is also deposited on the hulls and forms Fe-Zr intermetallics which incorporate the noble metals as well as residual actinides during processing. Hence, Zr has been chosen as the primary indicator for consistency of the metal waste. Recently, the first production-scale metal waste ingot was generated and sampled to monitor Zr content for Fe-Zr intermetallic phase formation and validation of processing conditions. Chemical assay of the metal waste ingot revealed a homogeneous distribution of the noble metal fission products as well as the primary fuel constituents U and Zr. Microstructural characterization of the ingot confirmed the immobilization of the noble metals in the Fe-Zr intermetallic phase.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Microstructural and strength stability of a developmental CVD SiC fiber

The effects of thermal exposure on the room temperature tensile strength and microstructure of a developmental 50 micron CVD SiC fiber have been studied. The fibers were heat treated between 600 and 2000 C in 0.1 MPa argon and air environments for up to 100 hr. In the as-fabricated condition, the fibers showed approximately 6 GPa tensile strength. After argon treatment, the fibers showed strength degradation after 1 hr exposure beyond 1000 C, but those exposed between 1600 and 2000 C retained approximately 2 GPa strength. TEM results showed microstructural changes both in the surface coating and SiC sheath. Flaws created by the rearrangement of carbon in the surface coating and growth of equiaxed SiC grain zone in the SiC sheath are the suggested mechanisms of strength degradation. After air treatment, fibers showed strength degradation after only 2 min exposure at 600 C. Strength retention after 2 min at 1500 C was approximately 2 GPa. Oxidation of the surface coating is the primary reason for strength degradation.

Bhatt, Ramakrishna T.↗

Microstructural and strength stability of CVD SiC fibers in argon environment

The room temperature tensile strength and microstructure of three types of commercially available chemically vapor deposited silicon carbide fibers were measured after 1, 10, and 100 hour heat treatments under argon pressures of 0.1 to 310 MPa at temperatures to 2100 C. Two types of fiber had carbon-rich surface coatings and the other contained no coating. All three fiber types showed strength degradation beyond 1400 C. Time and temperature of exposure had greater influence on strength degradation than argon pressure. Recrystallization and growth of near stoichiometric SiC grains appears to be the dominant mechanism for the strength degradation.

Bhatt, Ramakrishna T.↗