Search NASA⌕ Search

SEARCH · Search NASA

Results for “microstructural analysis”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 1,261 records · Page 70
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Observational Study of Clogging Specimens from the Tundish Well Showing Origin and Growth of a Clog in an Al-Killed Ti-Alloyed Steel Cast

Post-mortem tundish skull samples of Ti-alloyed, Al-killed IF steel have been studied regarding the formation of clogging. By using modern characterization equipment and applied methods, we performed a detailed characterization of microstructures found in the tundish well. Aside from the primary metallographic examination, newly developed methods of particle size distribution analysis based on population density functions (PDF) and newly developed electron microscope EDS template mapping have been applied, allowing differentiation of complex particles according to phases and interphase contact relationships. Furthermore, detailed EDS analyses of individual inclusions with complex substructure regarding minor and trace elements within the alumina networks have been performed. These composite data on carefully selected clog microstructures allowed us to observe the presence of layering microstructures throughout the clog: “Coarse” layers (abundant microbubbles and internally complex alumina aggregates) and “Fine” layers (no microbubbles and complex alumina aggregates). Two populations of particles: Population I (2 to 5 µm) and a Population II (5 to 20 µm) build up the layers, both having lognormal PDF, in contrast to power-law PDF of secondary metallurgy inclusions. Coarse layers are further distinguished by selective concentrations of spinel with lognormal PDF as well as the occurrence of complex alumina particles with metal sub-inclusions often with elevated Cr, V, and Si content. Based on these observations, we derive a model for the origin and accumulation of the inclusions making up the clog, which suggests that the NMI of the two dominant populations do not come from the bulk steel, although secondary metallurgy-derived inclusions can be traced in the clog. Overall, microstructures show that the clog behaves as a coherent solid, and is able to displace and fracture.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Investigating Accident Tolerant Fuel Concepts using the BISON Fuel Performance Code

There has been an increased interest in research of accident tolerant fuels (ATF) and claddings for use in commercial reactors ever since the events that occurred at the Fukushima Daiichi nuclear power plant in 2011. The economic impact of these events on the nuclear energy sector is significant. As a result, the United States Department of Energy's Office of Nuclear Energy accelerated research in nuclear fuel concepts with enhanced accident tolerance as part of its Fuel Cycle Research and Development (FCRD) Advanced Fuels Campaign (AFC). A report produced by the AFC entitled Light Water Reactor Accident Tolerant Fuel Performance Metrics outlines a set of metrics that can be used to guide selection of promising ATF concepts. Moreover, the report specifies that a down-selection is to occur in the 2016-2017 time frame, at which time the program will move from a proof-of-concept to a proof-of-principle stage with continued research and development into a small set of concepts. Given the time necessary for comprehensive irradiation experiments and post-irradiation examination, it is impossible to perform a complete set of experiments for material characterization. Therefore, the AFC is utilizing computational analysis tools in an effort to understand the proposed materials under a variety of normal operating and accident conditions. For some time, the DOE's Nuclear Energy Advanced Modeling and Simulation (NEAMS) program has been developing computational analysis tools for nuclear fuel simulation. These codes include BISON and Marmot which investigate fuel behavior at the continuum and microstructural scales, respectively. In 2014, NEAMS introduced what it calls High Impact Problems (HIPs) into its program plan. These HIPs are intended to make significant advancements in a particular area of nuclear power research in a short period of time (3 years or less). NEAMS has chosen an ATF project, which emphasizes utilizing BISON and Marmot to model proposed materials, as its first HIP. This summary focuses on the methodology being utilized for investigation of ATF concepts using the BISON fuel performance code. First, we give an overview of the model development for two candidate ATF materials, FeCrAl for cladding and uranium silicide (U{sub 3}Si{sub 2}) for fuel. Then, we present the approach for deciding which simulations are necessary given the importance of such simulations in providing a detailed report into the fuel performance behavior of these materials by the conclusion of the HIP. In absence of experimental data and given the aggressive schedule outlined by the AFC for ATF research and development, computational analysis tools are required. These tools are being used to help guide experiment design and to perform bounding and sensitivity studies to gain valuable information for which experimental data is limited. In support of this effort, models have been incorporated into BISON for simulation of U{sub 3}Si{sub 2} and FeCrAl. Continued material model development and engineering analysis will help address questions related to the performance of these ATF materials under normal operating and accident conditions. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2019

Direct measurements of slip irreversibility in a nickel-based superalloy using high resolution digital image correlation

Fatigue crack nucleation in crystalline materials typically develops due to highly localized cyclic slip. During a fatigue cycle, reverse slip differs locally from slip in the forward direction particularly in precipitate-containing materials such as superalloys. In this paper we report the first direct measurements of irreversibility at the scale of individual slip bands by high-resolution digital image correlation (DIC) in a polycrystalline nickel-based superalloy. Quantitative measurements of the slip irreversibility are challenging for regions of material that have a size that captures the microstructure and its variability. High spatial resolution at the nanometer scale during experimental measurements is needed to observe slip localization during deformation. Moreover, large fields are also needed to obtain the material response over statistically representative populations of microstructural configurations. Recently, high resolution scanning electron microscope (SEM) digital image correlation (DIC) has been extended for quantitative analysis of discontinuities induced by slip events using the Heaviside-DIC method. Therefore, this novel method provides quantitative measurements of slip localization at the specimen surface. In this paper, the Heaviside-DIC method is used to measure slip irreversibility and plastic strain accumulation in a nickel-based superalloy. The method detects bands with high levels of irreversibility early in cycling that ultimately form fatigue cracks upon further cycling. The local microstructural configurations that induce large amounts of plasticity and slip irreversibility are correlated to crack nucleation locations.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Impact of forging direction on the recrystallization behaviour of nickel base superalloy AD730 billet material at subsolvus temperatures

Highlights: • Large unrecrystallized grains present a fine distribution of intragranular γ′ precipitates; • Intragranular precipitates play a key role on strain distribution and subsequent recrystallization behaviour for AD730; • Continuous dynamic recrystallization (CDRX) promotes the gradual consumption of large unrecrystallized grains. • Undissolved secondary precipitates play a key role on the microstructural evolution of AD730 • No significant effect associated to the forging direction on the recrystallization behaviour of AD730 was found. AD730™ is a newly developed Ni-based superalloy for turbine disk applications produced by cast and wrought processes. Conventional ingot-to-billet conversion is an expensive and very complex operation. Because of the difficulties to achieve a uniform strain for recrystallization, large unrecrystallized grains are retained along this process. Heterogeneities of grain size have a negative impact on subsequent forging processes as well as ultrasonic inspectability of the destination part. The main aim of this work is to analyse the impact of both forging direction (billet, cogging) and strain (ε = 0.3–2) on the microstructural evolution of AD730 at subsolvus temperatures from a semi-finished product (billet) under conditions representative of both cogging and hot forging operations. Special attention to the presence of large unrecrystallized grains was paid. Double truncated cones (DTCs) were hot forged at subsolvus temperatures followed by air cooling. SEM and EBSD analysis were conducted in the as-received (billet) and the as-forged conditions. AD730 alloy presents a complex microstructure characterized by the presence of large unrecrystallized grains, aligned in the billet direction, with remarkable differences in γ′ precipitates distribution as compared to recrystallized structures. The fine distribution of primary γ′ precipitates (pinning effect) plays a key role on grain size control but also on the recrystallization behaviour. Continuous dynamic recrystallization (CDRX) mechanism was found to be operating in the large unrecrystallized grains, promoting the formation intragranular DRX grains and the gradual recrystallization of these grains. Strain presents a strong effect on the microstructural evolution of AD730, increasing the recrystallization fraction and refining the structure. By contrast, no significant effect associated to the forging direction was found. Conditions representative of cogging operations (ε ≤ 0.6) at subsolvus temperatures were translated into large fractions of unrecrystallized structures (strain accumulation).

36 MATERIALS SCIENCE↗
DOE OSTI2014

A facile one-pot method to Au–SnO{sub 2}-graphene ternary hybrid

In this article, we propose a facile one-pot route for synthesizing Au–SnO{sub 2}-graphene ternary hybrid. In the system, SnCl{sub 2} not only as the precursor of SnO{sub 2}, but also is employed as reducing agent for the effective reduction of both GO and HAuCl{sub 4} to graphene and Au nanoparticles, respectively. The obtained Au–SnO{sub 2}-graphene hybrid materials are characterized by atomic force microscopy, transmission electron microscopy, X-ray diffraction, Raman spectrum, X-ray photo-electron spectroscopy, and thermal gravimetric analysis. It is found that the content of Au nanoparticles decorated on the surface of graphene can be simply adjusted by changing the amount of HAuCl{sub 4} used in the synthesis process.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Enriched immersed finite element and isogeometric analysis: algorithms and data structures

Immersed finite element methods provide a convenient analysis framework for problems involving geometrically complex domains, such as those found in topology optimization and microstructures for engineered materials. However, their implementation remains a major challenge due to, among other things, the need to apply nontrivial stabilization schemes and generate custom quadrature rules. This article introduces the robust and computationally efficient algorithms and data structures comprising an immersed finite element preprocessing framework. The input to the preprocessor consists of a background mesh and one or more geometries defined on its domain. The output is structured into groups of elements with custom quadrature rules formatted such that common finite element assembly routines may be used without or with only minimal modifications. The key to the preprocessing framework is the construction of material topology information, concurrently with the generation of a quadrature rule, which is then used to perform enrichment and generate stabilization rules. While the algorithmic framework applies to a wide range of immersed finite element methods using different types of meshes, integration, and stabilization schemes, the preprocessor is presented within the context of the extended isogeometric analysis. This method utilizes a structured B-spline mesh, a generalized Heaviside enrichment strategy considering the material layout within individual basis functions’ supports, and face-oriented ghost stabilization. Using a set of examples, the effectiveness of the enrichment and stabilization strategies is demonstrated alongside the preprocessor’s robustness in geometric edge cases. Additionally, the performance and parallel scalability of the implementation are evaluated.

Computer implementation↗
DOE OSTI2013

Solution heat-treatment of Nb-modified MAR-M247 superalloy

MAR-M247 superalloy has excellent mechanical properties and good oxidation resistance at elevated temperatures. Niobium is an element known as {gamma} Prime phase hardener in nickel-based superalloys, besides promoting homogeneous distribution of MC carbides. This work is inserted in a project that aims to evaluate the total replacement of tantalum by niobium atoms in MAR-M247 superalloy (10.2 Co, 10.2 W, 8.5Cr, 5.6 Al, 1.6 Nb, 1.4 Hf, 1.1 Ti, 0.7 Mo, 0.15 C, 0.06 Zr, 0.015 B, Ni balance-wt.%). Based on microstructural characterizations (SEM and FEG-SEM, both with EDS) of the as-cast material and heat-treated materials as well as utilizing Thermocalc simulations and experiments of differential thermal analysis (DTA), heat-treatment at 1260 Degree-Sign C for 8 h was chosen as an ideal condition for the solution of Nb-modified MAR-M247 superalloy. The hardness of as-cast and ideally solution treated materials was 390 {+-} 14 HV and 415 {+-} 6 HV, respectively. - Highlights: Black-Right-Pointing-Pointer DTA and microstructure of MAR-M247(Nb) showed a good agreement with Thermocalc. Black-Right-Pointing-Pointer An ideal condition for solution heat-treatment of MAR-M247(Nb) is 1260 Degree-Sign C for 8 h. Black-Right-Pointing-Pointer It was an observed evidence of incipient melting in samples heat-treated at 1280 Degree-Sign C.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Study on Nanocellulose Properties Processed Using Different Methods and Their Aerogels

In this paper the effects of different mechanical methods including homogenization, ultrasonication and grinding on the properties of the nanocellulose materials and their aerogels, were investigated. The cellulose nanocrystal products, (CNC-H) and (CNC-U), were prepared by homogenization and ultrasonication of the acid hydrolyzed pulps, respectively. The aerogel products were produced by solvent exchanging of nanocellulose hydrogels with tertiary butyl alcohol and followed by freeze drying. The nanocellulose materials were studied using transmission electron microscopy, field emission scanning electron microscopy (FE-SEM), Fourier transformed infrared spectroscopy (TEM), X-ray diffraction (XRD), thermal gravimetric analysis (TGA). Size distribution and surface charges of the nanocellulose suspensions were measured by zetasizer. Also, the morphology, the porosity properties and surface area of the CNCs and CNF aerogels were investigated via FE-SEM and nitrogen adsorption–desorption isotherms. The results showed that CNC-H has higher surface charge, suspension stability (− 41.8 mV), crystallinity index (74.7%) and better size dispersion than CNC-U and CNF with an average particle size of 122 nm. CNC-H microstructures demonstrated homogeneous network structure with smaller nanometer dimensions (15–30 nm width and 60–400 nm length). However, the CNC-H showed lower thermal stability compared to CNC-U and CNF. Larger average pore size (16.32 nm), pore volume (0.42 cc/g) and high specific surface area (> 100 m{sup 2} g{sup −1}) in CNC-H aerogel were obtained. Graphical Abstract: Suspensions of nanocellulose (NC) were prepared by different mechanical methods: Homogenizing, Ultrasonic and grinding. The NC products were investigated and their differences in morphology and other characteristics were studied. The aerogels were prepared from the nanocellulose hydrogels. The nitrogen physisorption was used to study the pore characteristics of the aerogels. .

36 MATERIALS SCIENCE↗
DOE OSTI2013

DISFRAC Version 2.0 Users Guide

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

Cochran, Kristine B.↗
DOE OSTI2018

Densification, Microstructural Evolution, Mechanical Properties and Oxidation Study of CrB{sub 2} + EuB{sub 6} Composite

This paper reports the results of investigation on densification, microstructural evolution, mechanical properties and oxidation study of CrB{sub 2} + EuB{sub 6} composite. CrB{sub 2} + EuB{sub 6} (10 and 20 wt.%) composites have been fabricated by hot pressing at a temperature of 1700 °C and 35 MPa pressure. The hardness and flexural strength were measured in the range of 21.25-24.48 GPa and 171-199 MPa, respectively. The fracture toughness increased from 3.3 to 4.01 MPa m{sup 1/2} by the addition of 20% EuB{sub 6}. Microstructural evolution revealed the uniform distribution of EuB{sub 6} and absence of any reaction product. Fracture surface analysis confirmed the presence of transgranular mode of fracture. Oxidation study at 1200 °C revealed that the developed composites have good oxidation resistance and followed the parabolic rate of oxidation.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Microstructure and micro-texture evolution during large strain deformation of Inconel alloy IN718

The hot deformation behaviour of Inconel alloy IN718 was studied in the temperature range of 950–1100 °C and at strain rates of 0.01 and 1 s{sup −1} with a view to understand the microstructural evolution as a function of strain rate and temperature. For this purpose, a single hit, hot isothermal plane strain compression (PSC) technique was used. The flow curves obtained during PSC exhibited weak flow softening at higher temperatures. Electron backscattered diffraction analysis (EBSD) of the PSC tested samples at the location of maximum strain revealed dynamic recrystallisation occurring at higher temperatures. Based on detailed microstructure and microtexture analyses, it was concluded that single step, large strain deformation has a distinct advantage in the thermo-mechanical processing of Inconel alloy IN718. - Highlights: • Plane strain compression (PSC) on IN718 was conducted. • Evolution of microstructure during large strain deformation was studied. • Flow curves exhibited weak softening at higher temperatures and dipping of the flow curve at a strain rate of 1 s{sup −1}. • Optimization of microstructure and process parameter for hot rolling possible by plane strain compression testing • Dynamic recrystallisation occurs in specimens deformed at higher temperatures and lower strain rates.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructural evolution of an aluminide coating on alloy 625 during wet air exposure at 900 °C and 1000 °C

The microstructural changes of the aluminized alloy 625 during cyclic oxidation in air + 6% H 2 O at 900 °C and 1000 °C were analyzed using optical metallography (OM), scanning electron microscopy (SEM) with energy and wave length dispersive X-ray analysis (EDX/WDX) as well as electron backscatter diffraction (EBSD). An in-house developed thermodynamic-kinetic procedure was employed to predict the microstructural evolution of aluminized alloy 625 during high temperature exposure by considering simultaneously occurring surface oxidation and interdiffusion processes. Because of the lack of mobility data for the relevant alloying elements in the σ-phase, assumptions for the mobilities were made based on the value of the mobilities in α-Cr. Despite these assumptions, the calculated results were found to be in good agreement with experimental observations. The complete depletion of β-NiAl in the coating observed during exposure at 1000 °C was correctly predicted by the model. The model was also able to infer dissolution of the precipitate phases α-Cr and σ in the interdiffusion zone during exposures at 900 °C and 1000 °C. The model was yet unable to predict the formation of the μ-phase in the alloy after 1000 h of exposure at 1000 °C. The developed modelling method offers the potential to predict microstructural changes of aluminized nickel base alloys thus reducing cost and time consuming experimental efforts.

36 MATERIALS SCIENCE↗
DOE OSTI2016

In situ {sup 1}H-TD-NMR: Quantification and microstructure development during the early hydration of alite and OPC

An in situ framework for {sup 1}H time-domain nuclear magnetic resonance analysis was developed and applied on alite and OPC hydration. Highly time-resolved quantitative data on the evolution of proton reservoirs during hydration was collected for up to 40 h. Reservoirs could be clearly assigned to mobile (mix water), intermediate (C-S-H) and rigid fractions (CH, ettringite). Comparison of determined fraction quantities with data from in situ XRD measurements and heat flow calorimetry show very good agreement. During alite hydration at 23 °C, a bulk water content of 4 H{sub 2}O in C{sub 1.7}SH{sub x} was confirmed. T2 relaxation times of the mobile fraction shifted towards shorter times from the start of the main reaction until the maximum of the heat flow. Microstructure evolution is nearly finished at that point in time. T2 relaxation times are severely shortened for iron-containing OPC, but are still evaluable.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Fabrication and Analysis of Tri-layer YBa{sub 2}Cu{sub 3}O{sub 7−δ} Thick Films by Low-Fluorine MOD Method

Improving the thickness of superconducting layer in coated conductors is an effective way to enhance its critical current. In this work, tri-layer YBCO/YBCO/YDyBCO films were successfully deposited on buffered Hastelloy substrate using the multi-coating lowfluorine metal-organic decomposition (LF-MOD) method and the thickness of the films can be up to 2.4 μ m. The effects of high-temperature annealing time on microstructures and superconducting properties of the films were systematically studied. Energy dispersive X-ray spectroscopy (EDS) results reveal that there remains a large amount of F element in the upper layer of the film when the annealing time is too short. With increasing the annealing time, the fluoride-containing precursor converts to YBCO grains completely. But the coarsening of grains appeared, and the critical current density (J{sub c}) of the film dropped slightly when the annealing time is too long. The cross-sectional scanning electron microscope (SEM) image and EDS plane analysis were applied to investigate the microstructure and element distribution of the final triple-layer YBCO films, respectively. The critical current of the final YBCO superconducting film could reach 316 A (77 k, self-field) for 1.2-cm-wide tapes with the optimal annealing conditions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2021

Dual microscopy to explore enhanced atmospheric ice nucleation on multi-component aerosols

Using an optical microscopy setup adapted to in-situ studies of ice formation at ambient pressure, we examined a specific multicomponent mineral, microcline, with the ultimate aim of gaining a more realistic understanding of ice nucleation in Earth’s atmosphere. We focused on a perthitic feldspar, microcline, to test the hypothesis that co-existence in some feldspars of K-rich and Na-rich phases are contributing to enhanced ice nucleation. On a sample deliberately chosen to contain lamella, a typical perthitic microstructure, and flat surface regions next to each other, we performed a series of ice formation experiments. We found microcline to promote ice formation, causing a large number of ice nucleation events at around - 27°C. The number of ice nuclei decreased from experimental run to experimental run, indicating surface aging upon repeated exposure to humidity. An analysis of 10 experimental runs of identical conditions did not reveal an obvious enhancement of ice formation at the lamellar microstructure. Instead, we find efficient nucleation at various surface sites that produce orientationally aligned ice crystallites with asymmetric shape. Based on this observation we propose that surface steps running along select directions produce microfacets of an orientation that is favorable to enhanced ice nucleation, similar to previously reported for K-rich feldspars.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Unraveling the implications of finite specimen size on the interpretation of dynamic experiments for polycrystalline aluminum through direct numerical simulations

Normal and Pressure-shear plate impact (NPI and PSPI) experiments are popular experimental techniques for studying the mean-field macroscopic behavior of polycrystalline metals under high-rate dynamic loading. However, since both configurations rely upon geometry for subjecting the specimen to high strain rates, these experiments often involve a limited specimen size. Moreover, because of the inherent heterogeneities present within polycrystalline metals, it is difficult to ascertain if the size of the specimen and/or regions where measurements are made are sufficiently large for making representative inferences about the mean-field macroscopic properties from single-point velocity measurements. In the present study, we quantify the expected measurement variability on observable point measurements in NPI and PSPI experiments by carrying out direct numerical simulations (DNS) of statistically representative polycrystalline microstructures subjected to dynamic compression and compression-shear loading. In particular, we consider the role of specific material heterogeneities (e.g. the grain-to-grain difference in size, crystallographic orientation) on dispersion in the normal and transverse particle velocity records and on local fluctuations in key state variables (e.g. velocity, accumulated plastic strain) by incorporating these effects directly into a representative synthetic microstructure geometry and crystalline description of pure polycrystalline aluminum. The form of the present study is a large parametric investigation, consisting of ten ensembles of one hundred simulations. Each of the thousand simulations reflects a randomly realized synthetic microstructure in one of five cases of decreasing average grain size for the two loading configurations. Our analysis of the DNS results demonstrates that for both of these experimental configurations, the grain size directly correlates with the coefficient of variation (CV) in simulated point measurements, showing a convergent decrease in CV to zero (i.e. particle velocity record approaches the mean-field value) with decreasing grain size. Remarkably, the magnitude of variations in the particle velocity record is shown to be largest where the deviatoric stresses are most significant. In the case of NPI, this occurs at the elastic and plastic wavefront, whereas, in the case of PSPI, the magnitude of fluctuations are approximately constant throughout the experimental window time. The reasoning for the scatter in particle velocity due to the heterogeneous microstructure is demonstrated to be dependent on the mechanisms for accommodating deformation and on the interaction of reflection waves generated at sites of heterogeneities occurring at the scale of grains. Lastly, we develop a power-law description for the magnitude of scattering versus characteristic length, which provides a statistical framework for assessing the required number of grains per characteristic specimen dimension for minimizing scatter within these two experimental configurations (NPI, PSPI).

36 MATERIALS SCIENCE↗
DOE OSTI2023

Probing rutile solid-phase crystallization of atomically mixed Mn-alloyed TiO 2 coatings through XANES analysis

Phase transformation via dopant introduction is an emerging strategy for tuning the electronic and catalytic properties of oxides. However, developing a general theory of ternary alloys and their microstructure evolution remains challenging due to the knowledge gaps in how point defects such as dopants lead to the formation of complex or metastable phases. We investigate the influence of Mn concentration and annealing temperature on the microstructure evolution of amorphous Mn-alloyed TiO 2 synthesized via Atomic Layer Deposition. In conclusion, our findings reveal a new crystallization pathway resulting in a direct amorphous TiO 2 to rutile transformation without an intermediate anatase phase and our multi-parameter thermal processing conditions show potential for AI-assisted data acquisition and analysis for studying complex oxide coatings.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Structural and electrical properties of ternary Ru-AlN thin films prepared by plasma-enhanced atomic layer deposition

Highlights: Black-Right-Pointing-Pointer Ru-AlN thin films were grown by plasma-enhanced atomic layer deposition (PEALD). Black-Right-Pointing-Pointer Structural properties were systematically investigated by XRD, BF-STEM and EDX. Black-Right-Pointing-Pointer A drastic decrease in resistivity was due to the microstructural change of the films. -- Abstract: Ruthenium-aluminum-nitride (Ru-AlN) thin films were grown by plasma-enhanced atomic layer deposition (PEALD) at 300 Degree-Sign C. The Ru intermixing ratio of Ru-AlN thin films was controlled by the number of Ru unit cycles, while the number of AlN unit cycles was fixed to one cycle. The electrical resistivity of Ru-AlN thin film decreased with increasing the Ru intermixing ratio, but a drastic decrease in electrical resistivity was observed when the Ru intermixing ratio was around 0.58-0.78. Bright-field scanning transmission electron microscope (BF-STEM) and energy-dispersive X-ray spectroscopy (EDX) element mapping analysis revealed that the electrical resistivity of Ru-AlN thin film was strongly dependent on the microstructures as well as on the Ru intermixing ratio. Although the electrical resistivity of Ru-AlN thin films decreased with increasing the Ru intermixing ratio, a drastic decrease in electrical resistivity occurred where the electrical paths formed as a result of the coalescence of Ru nanocrystals.

36 MATERIALS SCIENCE↗