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At least 1,081 records · Page 60

Nanoscale microstructure and chemistry of transparent gahnite glass-ceramics revealed by atom probe tomography

The nanoscale microstructure and chemistry of a transparent gahnite glass-ceramic and its precursor glass were investigated using atom probe tomography, transmission electron microscopy, and nuclear magnetic resonance spectroscopy. In the annealed precursor glass, statistically significant ZrO clustering was observed along with Si depletion within 2 nm of the ZrO clusters. This clustering is expected to be the first step in the nucleation and crystallization of the nucleating agent, ZrO 2 . In the glass-ceramic, gahnite (ZnAl 2 O 4 ) crystallites were found to exist in proximal locations to ZrO 2 and not in a core-shell arrangement. The residual glass composition was directly measured by atom probe, showing higher concentrations of Al, Zn, and Zr than previously expected. At the interfaces between the crystallites and residual glass, no enrichment or depletion zones were found. Our findings provide answers to outstanding questions surrounding the nucleation and elemental partitioning, microstructure, and the residual glass composition of transparent gahnite glass-ceramics.

36 MATERIALS SCIENCE↗

Compositionally-Driven Formation Mechanism of Hierarchical Morphologies in Co-Deposited Immiscible Alloy Thin Films

Co-deposited, immiscible alloy systems form hierarchical microstructures under specific deposition conditions that accentuate the difference in constituent element mobility. The mechanism leading to the formation of these unique hierarchical morphologies during the deposition process is difficult to identify, since the characterization of these microstructures is typically carried out post-deposition. We employ phase-field modeling to study the evolution of microstructures during deposition combined with microscopy characterization of experimentally deposited thin films to reveal the origin of the formation mechanism of hierarchical morphologies in co-deposited, immiscible alloy thin films. Our results trace this back to the significant influence of a local compositional driving force that occurs near the surface of the growing thin film. We show that local variations in the concentration of the vapor phase near the surface, resulting in nuclei (i.e., a cluster of atoms) on the film’s surface with an inhomogeneous composition, can trigger the simultaneous evolution of multiple concentration modulations across multiple length scales, leading to hierarchical morphologies. We show that locally, the concentration must be above a certain threshold value in order to generate distinct hierarchical morphologies in a single domain.

36 MATERIALS SCIENCE↗

Alumina-Reinforced Zirconia Composites

Alumina-reinforced zirconia composites, used as electrolyte materials for solid oxide fuel cells, were fabricated by hot pressing 10 mol percent yttria-stabilized zirconia (10-YSZ) reinforced with two different forms of alumina particulates and platelets each containing 0 to 30 mol percent alumina. Major mechanical and physical properties of both particulate and platelet composites including flexure strength, fracture toughness, slow crack growth, elastic modulus, density, Vickers microhardness, thermal conductivity, and microstructures were determined as a function of alumina content either at 25 C or at both 25 and 1000 C. Flexure strength and fracture toughness at 1000 C were maximized with 30 particulate and 30 mol percent platelet composites, respectively, while resistance to slow crack growth at 1000 C in air was greater for 30 mol percent platelet composite than for 30 mol percent particulate composites.

Choi, Sung R.↗

Internal strain analysis of ceramics using scanning laser acoustic microscopy

Quantitative studies of material behavior characteristics are essential for predicting the functionality of a material under its operating conditions. A nonintrusive methodology for measuring the in situ strain of small dimeter (to 11 microns) ceramic fibers under uniaxial tensile loading and the local internal strains of ceramics and ceramic composites under flexural loading is introduced. The strain measurements and experimentally observed mechanical behavior are analyzed in terms of the microstructural development and fracture behavior of each test specimen evaluated. Measurement and analysis of Nicalon silicon carbide (SiC) fiber (15 microns diameter) indicate that the mean elastic modulus of the individual fiber is 185.3 GPa. Deviations observed in the experimentally determined elastic modulus values between specimens were attributed to microstructural variations which occur during processing. Corresponding variations in the fracture surface morphology were also observed. The observed local mechanical behavior of a lithium alumino-silicate (LAS) glass ceramic, a LAS/SiC monofilament composite, and a calcium alumino-silicate (CAS)/SiC fully reinforced composite exhibits nonlinearities and apparent hysteresis due to the subcritical mechanical loading. Local hysteresis in the LAS matrices coincided with the occurrence of multiple fracture initiation sites, localized microcracking, and secondary cracking. The observed microcracking phenomenon was attributed to stress relaxation of residual stresses developed during processing, and local interaction of the crack front with the microstructure. The relaxation strain and stress predicted on apparent mechanical hysteresis effects were defined and correlated with the magnitude of the measured fracture stress for each specimen studied. This quantitative correlation indicated a repeatable measure of the stress at which matrix microcracking occurred for stress relief of each material system. Stress relaxation occurred prior to the onset of steady state cracking conditions. The relaxation stress occurred at 18.5 percent of the fracture stress in LAS and 11.0 percent of the yield stress in CAS/SiC. The relaxation stress ratio was dependent upon the dominant fracture mode of the LAS/SiC specimens. Relaxation stress ratios greater than 0.30 were observed for specimens which fractured due to shear at the fiber matrix interface; specimens which fracture due to tensile cracking had relaxation stress ratios less than 0.30. The stress relaxation ratio appeared to be a specific characteristic of the glass ceramic material. The measured stress relaxation for LAS indicated a measure of the inherent residual stresses in the material due to processing and suggested localized toughening mechanisms for brittle material structures.

Kent, Renee M.↗

Characterization of ceramics and intermetallics fabricated by self-propagating high-temperature synthesis

Three efforts aimed at investigating the process of self-propagating high temperature synthesis (SHS) for the fabrication of structural ceramics and intermetallics are summarized. Of special interest was the influence of processing variables such as exothermic dopants, gravity, and green state morphology in materials produced by SHS. In the first effort directed toward the fabrication of SiC, exothermic dopants of yttrium and zirconium were added to SiO2 or SiO2 + NiO plus carbon powder mix and processed by SHS. This approach was unsuccessful since it did not produce the desired product of crystalline SiC. In the second effort, the influence of gravity was investigated by examining Ni-Al microstructures which were produced by SHS combustion waves traveling with and opposite the gravity direction. Although final composition and total porosities of the combusted Ni-Al compounds were found to be gravity independent, larger pores were created in those specimens which were combusted opposite to the gravity force direction. Finally, it was found that green microstructure has a significant effect on the appearance of the combusted piece. Severe pressing laminations were observed to arrest the combustion front for TiC samples.

Hurst, Janet B.↗

High Tc composite silver/oxide superconductors

Factors involved in the strong flux pinning effect of high-Tc YBa2Cu3O7/AgO (Y-123/AgO) composite and other REE-123/AgO composites were investigated. Samples of superconducting REE-123 and REE-123/AgO (where REE was Nd, Sm, Eu, Gd, Dy, Ho, Er, or Y) were prepared and used to obtain magnetic moments, critical field, and microstructure data. The optimum heat treatment conditions for the formation of strong flux-pinning REE-123/AgO composites were found to be different for different REE-123 compounds. It was found that the annealing temperature depends on the ionic size of the REE, with larger rare-earth ions requiring higher temperature. It was also found that strong flux-pinning REE-123/AgO composites form only in a narrow annealing temperature range.

Curreri, P. A.↗

Microstructure and Properties of Thermally Sprayed Functionally Graded Coatings for Polymeric Substrates

The use of polymer matrix composites (PMCs) in the gas flow path of advanced turbine engines offers significant benefits for aircraft engine performance but their useful lifetime is limited by their poor erosion resistance. High velocity oxy-fuel (HVOF) sprayed polymer/cermet functionally graded (FGM) coatings are being investigated as a method to address this technology gap by providing erosion and oxidation protection to polymer matrix composites. The FGM coating structures are based on a polyimide matrix filled with varying volume fractions of WC-Co. The graded coating architecture was produced using a combination of internal and external feedstock injection, via two computer-controlled powder feeders and controlled substrate preheating. Porosity, coating thickness and volume fraction of the WC-Co filler retained in the coatings were determined using standard metallographic techniques and computer image analysis. The pull-off strength (often referred to as the adhesive strength) of the coatings was evaluated according to the ASTM D 4541 standard test method, which measured the greatest normal tensile force that the coating could withstand. Adhesive/cohesive strengths were determined for three different types of coating structures and compared based on the maximum indicated load and the surface area loaded. The nature and locus of the fractures were characterized according to the percent of adhesive and/or cohesive failure, and the tested interfaces and layers involved were analyzed by Scanning Electron Microscopy.

Ivosevic, M.↗

Microstructured Optical Fiber for X-ray Detection

A novel scintillating optical fiber is presented using a composite micro-structured quartz optical fiber. Scintillating materials are introduced into the multiple inclusions of the fiber. This creates a composite optical fiber having quartz as a cladding with an organic scintillating material core. X-ray detection using these fibers is compared to a collimated cadmium telluride (CdTe) detector over an energy range from 10 to 40 keV. Results show a good correlation between the fiber count rate trend and that of the CdTe detector.

DeHaven, Stanton L.↗

Effect of CMAS viscosity on the infiltration depth in thermal barrier coatings of different microstructures

Calcium magnesium aluminum silicate (CMAS) is one of the leading concerns for the gas turbine industry. The effects of CMAS viscosity and the coating microstructure on CMAS infiltration depth were explored by conducting a time dependent interaction study. Three CMAS compositions were used from literature, and their viscosities predicted through FactSage viscosity module were drastically different. The interaction was carried out on three different TBCs synthesized using the solution precursor plasma spray process (SPPS): two of the TBCs were made of yttrium aluminum garnet (YAG) having different microstructures that promote different modes of CMAS infiltration, and one TBC was made of gadolinium zirconate (GZO). All samples had stress relieving vertical cracks and different intensities of horizontally banded porosity, (inter pass boundaries IPBs). A concentration of 100 mg/cm 2 of CMAS was applied on the TBCs which were then subjected to a 5-minute interaction at 1300 °C. Samples were analyzed using scanning electron microscopy (SEM), electron dispersive X-ray spectroscopy (EDXS), and transmission electron microscopy (TEM). Low viscosity CMAS readily penetrated the TBCs while more viscous CMAS showed less penetration. The depth of CMAS infiltration depended on the coating microstructure. In the YAG with IPBs, the CMAS spread horizontally in the IPBs before infiltrating deeper, resulting in reduced infiltration depth compared to other samples in spite of having wider vertical cracks. TEM and EDXS analysis were performed to investigate the phases present in the CMAS-TBC interaction region in YAG. Two regions were chosen, the top TBC surface in direct contact with the sea of CMAS, and the region at the CMAS penetration ended within the coating. Finally, the results showed that no secondary phases like apatite were observed in YAG, thus it can be concluded that the arrest of CMAS happened solely because of CMAS viscosity and the short infiltration time.

36 MATERIALS SCIENCE↗

Operando neutron radiography validates a parameter-free transport–kinetics model for thick solid-state battery cathodes

Tortuosity-weighted interfacial flux for lithium (TWIF-Li) predicts through-thickness Li gradients in thick composite all-solid-state cathodes without fitted parameters. Image-derived microstructures, GITT-derived concentration-dependent solid diffusion, and tortuosity-weighted interfacial kinetics reproduce operando neutron radiography across practical rates, delivering transferable design rules to suppress transport-limited reaction fronts.

Adam, Andre [ORNL] (ORCID:0000000245023033)↗

Multiscale characterization and representation of variability in ceramic matrix composites

Low density, high strength, and high creep and oxidation resistance properties of ceramic matrix composites (CMCs) make them an ideal choice for use in extreme environments in space and military applications. This paper presents a detailed characterization study of structural and manufacturing flaws in Carbon fiber Silicon-Carbide-Nitride matrix (C/SiNC) CMCs at different length-scales. Energy-dispersive spectroscopy (EDS) is used for the chemical characterization of the material’s elemental constituents. High-resolution multiscale graphs obtained from scanning electron microscope (SEM) and confocal laser scanning microscope (LSM) are used to characterize the distribution and morphology of defects at different length scales. This is followed by the classification and quantification of the common manufacturing defects. An image processing algorithm based on the image segmentation process is developed to quantify the variability of various scale-dependent architectural parameters. Finally, a three-dimensional stochastic representative volume element (SRVE) generation algorithm is developed to provide precise representations of material textures at multiple length scales. The developed algorithm accurately accounts for material features and flaws based on a range of multiscale structural and defects characterization results.

36 MATERIALS SCIENCE↗

Examination of UC-ZrC after long term irradiation at thermionic temperature

Two fluoride tungsten clad UC-ZrC fueled capsules, designated as V-2C and V-2D, were examined a hot cell after irradiation in NASA Plum Brook Reactor at a maximum cladding temperature of 1930 K for 11,089 and 12,031 hours to burnups of 3.0 x 10 to the 20th power and 2.1 x 10 to the 20th power fission/c.c. respectively. Percentage of fission gas release from the fuel material was measured by radiochemical means. Cladding deformation, fuel-cladding interaction and microstructures of fuel, cladding, and fuel-cladding interface were studied metallographically. Compositions of dispersions in fuel, fuel matrix and fuel-cladding interaction layer were analyzed by electron microprobe techniques. Axial and radial distributions of burnup were determined by gamma-scan, autoradiography and isotopic burnup analysis. The results are presented and discussed in conjunction with the requirements of thermionic fuel elements for space power application.

Yang, L.↗

Factors affecting the strength of multipass low-alloy steel weld metal

The mechanical properties of multipass high-strength steel weld metals depend upon several factors, among the most important being: (1) The interaction between the alloy composition and weld metal cooling rate which determines the as-deposited microstructure; and (2) the thermal effects of subsequent passes on each underlying pass which alter the original microstructure. The bulk properties of a multipass weld are therefore governed by both the initial microstructure of each weld pass and its subsequent thermal history. Data obtained for a high strength low alloy steel weld metal confirmed that a simple correlation exists between mechanical properties and welding conditions if the latter are in turn correlated as weld cooling rate.

Krantz, B. M.↗

Infrared experiments for spaceborne planetary atmospheres research. Full report

The role of infrared sensing in atmospheric science is discussed and existing infrared measurement techniques are reviewed. Proposed techniques for measuring planetary atmospheres are criticized and recommended instrument developments for spaceborne investigations are summarized for the following phenomena: global and local radiative budget; radiative flux profiles; winds; temperature; pressure; transient and marginal atmospheres; planetary rotation and global atmospheric activity; abundances of stable constituents; vertical, lateral, and temporal distribution of abundances; composition of clouds and aerosols; radiative properties of clouds and aerosols; cloud microstructure; cloud macrostructure; and non-LTE phenomena.

Source record↗

From interstellar dust to comets

The bulk and microstructure of comet nuclei are derived from the morphological structure and chemical composition of submicron sized interstellar dust grains which have undergone cold aggregation in the pre-solar nebula. The evolutionary picture of dust which is emerging is a cyclic one in which the particles, before being destroyed or going into solar system bodies, find themselves during their 5 billion year lifetime alternately in diffuse clouds and in molecular clouds. A small silicate core captured within a molecular cloud accretes various ices and gradually builds up an inner mantle of organic refractory material which has been produced by photoprocessing of the volatile ices. Clumps of grains form, and then clumps of clumps, and so on, until finally we reach the size of the comet nucleus.

Greenberg, J. M.↗

Transformation to Ni5Al3 in a 63.0 at. pct Ni-Al alloy

Microstructures of 63 at. pct P/M Ni-Al alloys with a composition close to the stoichiometry of the Ni5Al3 phase were investigated using homogenized and quenched specimens aged at low temperatures for various times. Results of analyses of XRD data and electron microscopy observations were used for quantitative phase analysis, performed to calculate the (NiAl + Ni5Al3)/Ni5Al3 phase boundary locations. The measured lattice parameters of Ni5Al3 phase formed at 823, 873, and 923 K indicated an increase in tetragonality of the phase with increasing nickel content.

Khadkikar, P. S.↗