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All sources NASA NTRS DOE OSTI

DOE OSTI2021

Synergic grain boundary segregation and precipitation in W- and W-Mo-containing high-entropy borides

The structures of W- and W-Mo-containing high-entropy borides (HEBs) are systematically studied by combining atomic-resolution transmission electron microscopy imaging, electron diffraction, and chemical analysis. Here, we reveal that W or W-Mo addition in HEBs leads to segregation of these elements to the grain boundaries (GBs). In the meantime, W- or W-Mo-rich precipitates also form along the GBs. Crystallographic analysis and atomic-scale imaging show that the GB precipitates in both W- and W-Mo-containing HEBs have a cube-on-cube orientation relationship with the matrix. With further strain analysis, the coherency of the precipitate/matrix interface is validated. Nanoindentation tests show that the simultaneous GB segregation and coherent precipitation, as a supplement to the grain hardening, provide additional hardening of the HEBs. Our work provides an in-depth understanding of the GB segregation and precipitation behaviors of HEBs. It suggests that GB engineering could be potentially used for optimizing the performance of high-entropy ceramics.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

NASA NTRS2003

Aging Optimization of Aluminum-Lithium Alloy C458 for Application to Cryotank Structures

Compared with aluminum alloys such as 2219, which is widely used in space vehicle for cryogenic tanks and unpressurized structures, aluminum-lithium alloys possess attractive combinations of lower density and higher modulus along with comparable mechanical properties. These characteristics have resulted in the successful use of the aluminum-lithium alloy 2195 (Al-1.0 Li-4.0 Cu-0.4 Mg-0.4 Ag-0.12 Zr) for the Space Shuttle External Tank, and the consideration of newer U.S. aluminum-lithium alloys such as L277 and C458 for future space vehicles. These newer alloys generally have lithium content less than 2 wt. % and their composition and processing have been carefully tailored to increase the toughness and reduce the mechanical property anisotropy of the earlier generation alloys such 2090 and 8090. Alloy processing, particularly the aging treatment, has a significant influence on the strength-toughness combinations and their dependence on service environments for aluminum-lithium alloys. Work at NASA Marshall Space Flight Center on alloy 2195 has shown that the cryogenic toughness can be improved by employing a two-step aging process. This is accomplished by aging at a lower temperature in the first step to suppress nucleation of the strengthening precipitate at sub-grain boundaries while promoting nucleation in the interior of the grains. Second step aging at the normal aging temperature results in precipitate growth to the optimum size. A design of experiments aging study was conducted for plate. To achieve the T8 temper, Alloy C458 (Al-1.8 Li-2.7 Cu-0.3 Mg-0.08 Zr-0.3 Mn-0.6 Zn) is typically aged at 300F for 24hours. In this study, a two-step aging treatment was developed through a comprehensive 2(exp 4) full factorial design of experiments study and the typical one-step aging used as a reference. Based on the higher lithium content of C458 compared with 2195, the first step aging temperature was varied between 175F and 250F. The second step aging temperatures was varied between 275F and 325F, which is in the range of the single-step aging temperature. The results of the design of experiments used for the T8 temper as well as a smaller set of experiments for the T6 temper will be presented. The process of selecting the optimum aging treatment, based on the measured mechanical properties at room and cryogenic temperature as well as the observed deformation mechanisms, will be presented in detail. The implications for the use of alloy C458 in cryotanks will be discussed.

Sova, B. J.↗

NASA NTRS2003

Aging Optimization of Aluminum-Lithium Alloy C458 for Application to Cryotank Structures

Compared with aluminum alloys such as 2219, which is widely used in space vehicle for cryogenic tanks and unpressurized structures, aluminum-lithium alloys possess attractive combinations of lower density and higher modulus along with comparable mechanical properties. These characteristics have resulted in the successful use of the aluminum-lithium alloy 2195 (Al-1.0 Li-4.0 Cu-0.4 Mg-0.4 Ag-0.12 Zr) for the Space Shuttle External Tank, and the consideration of newer U.S. aluminum-lithium alloys such as L277 and C458 for future space vehicles. These newer alloys generally have lithium content less than 2 wt. % and their composition and processing have been carefully tailored to increase the toughness and reduce the mechanical property anisotropy of the earlier generation alloys such 2090 and 8090. Alloy processing, particularly the aging treatment, has a significant influence on the strength-toughness combinations and their dependence on service environments for aluminum-lithium alloys. Work at NASA Marshall Space Flight Center on alloy 2195 has shown that the cryogenic toughness can be improved by employing a two-step aging process. This is accomplished by aging at a lower temperature in the first step to suppress nucleation of the strengthening precipitate at sub-grain boundaries while promoting nucleation in the interior of the grains. Second step aging at the normal aging temperature results in precipitate growth to the optimum size. A design of experiments aging study was conducted for plate. To achieve the T8 temper, Alloy C458 (Al-1.8 Li-2.7 Cu-0.3 Mg- 0.08 Zr-0.3 Mn-0.6 Zn) is typically aged at 300 F for 24 hours. In this study, a two-step aging treatment was developed through a comprehensive 24 full factorial design of experiments study and the typical one-step aging used as a reference. Based on the higher lithium content of C458 compared with 2195, the first step aging temperature was varied between 175 F and 250 F. The second step aging temperatures was varied between 275 F and 325 F, which is in the range of the single-step aging temperature. The results of the design of experiments used for the T8 temper as well as a smaller set of experiments for the T6 temper will be presented. The process of selecting the optimum aging treatment, based on the measured mechanical properties at room and cryogenic temperature as well as the observed deformation mechanisms, will be presented in detail. The implications for the use of alloy C458 in cryotanks will be discussed.

Sova, B. J.↗

DOE OSTI2022

Phase transformation and growth mechanism of RF sputtered ferroelectric lead scandium tantalate (PbSc 0.5 Ta 0.5 O 3 ) films

Lead scandium tantalate (PbSc 0.5 Ta 0.5 O 3 , PST), an order/disorder ferroelectric, is a potential candidate for electrocaloric cooling and pyroelectric infrared (IR) detector. In this work, we report the phase transformation kinetics from two series of samples containing pure amorphous and mixture of amorphous and pyrochlore to desired perovskite phase using postdeposition rapid thermal processing (RTP) as well as growth mechanism of RF sputtered PST thin films using excess lead target on platinized silicon (Pt/Ti/SiO 2 /Si) substrates. We find that small changes in the temperature ramp have a large effect on the degree of perovskite conversion (ferroelectric phase), orientation (crystallographic texture), and long-range order parameter (< S 111 >). Through isothermal annealing, we obtained optimal perovskite phase at ≥700°C temperature. The phase transformation is characterized by spontaneous formation of center-type in-plane radial rosette-like structures revealed by scanning electron microscopy. The PST perovskite crystallites were found to coexist with pyrochlore in RTP annealed films. The volume fractions for perovskite and pyrochlore phase were obtained from the analysis of “rosettes” and respective X-ray diffraction intensities which helped to determine various parameters associated with phase kinetics (n, k, and activation energy, Ea) and accompanying growth. The effective activation energies of perovskite transition and growth were found to be 332 ± 11 kJ/mol (345 ± 11 kJ/mol) and 114 ± 10 kJ/mol (122 ± 10 kJ/mol), respectively, for pure amorphous only (and mixed amorphous and pyrochlore) phase following nucleation-growth controlled Avrami's equation. A linear growth rate (n~1) for the perovskite phase indicates predominant interface-controlled process and diffusion-limited phenomena thus inhibiting rosette size owing to reactant depletion and soft impingement at the grain boundary. However, the growth behavior is isotropic in two-dimension parallel to the plane of the substrates for both sample series. Furthermore, lead loss was severe for in-situ growth and RTP combined with conventional furnace annealing than those of RTP only films, which were closer to stoichiometric albeit with excess lead and marginal oxygen vacancies (V o ).

36 MATERIALS SCIENCE↗

DOE OSTI2016

Room temperature neutron diffraction and magnetic studies of multiferroic Pb{sub 0.9}Bi{sub 0.1}Fe{sub 0.55}Nb{sub 0.45}O{sub 3} solid solution

The Pb{sub 0.9}Bi{sub 0.1}Fe{sub 0.55}Nb{sub 0.45}O{sub 3} (PBFNO) solid solution was synthesized by single step solid state reaction method and the optimized parameters are 700°C for 2hr (calcination) and 800°C for 3hr (sintering). The formation of desired material was confirmed using X-Ray Diffraction (XRD) and Neutron Diffraction (ND) studies. The structural and magnetic properties of the sintered pellets were investigated at room temperature (RT) through XRD, ND and Magnetic (M-H) studies. The structural analysis was carried out by Rietveld refinement through the Full Prof program. Rietveld refined XRD and ND patterns confirms the monoclinic structure with Cm space group and obtained cell parameters from the ND data are a = 5.651(2) Å, b = 5.658(2) Å, c = 4.005(1) Å and α = 90°, β = 89.98(1)°, γ = 90°. RT M-H curve studies have been carried out. It shows the clear opening of hysteresis (M–H) loop, is evidenced as the existence of weak ferromagnetism at RT. The M-H data shows existence weak ferromagnetism embedded in an antiferromagnetic matrix structure. The dielectric constant with frequency shows the formation of barrier layers at the grain and grain boundary interfaces gives rise to interfacial space charge polarization.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2012

Nanocrystalline non-stoichiometric SBT: Effect of milling duration on structural and electrical characteristics

In the present work, nanocrystalline specimens of non-stoichiometric Strontium Bismuth Tantalate (SBT) ferroelectric ceramics were synthesized by mechanical activation process using a high energy planetary ball mill. The powders were milled for different milling durations (5, 10, 20 h) keeping the milling speed fixed at 300 rpm. Microstructural characterizations have been performed using X-ray diffraction, scanning electron microscopy, electron diffraction and transmission electron microscopy. Nanocrystallites with average grain size in the range of 30-50 nm are observed to be formed. Grain size is observed to decrease with increasing milling duration. Detailed dielectric study as a function of temperature has been carried out. It is observed that dielectric constant increases and dielectric loss decreases with increasing milling duration. The observed characteristics have been explained in terms of increased number of grain boundaries due to the reduction of granular size. - Highlights: Black-Right-Pointing-Pointer In the present work nano crystalline non-stoichiometric SBT has been synthesized. Black-Right-Pointing-Pointer The technique involved is mechanical activation (high energy ball milling). Black-Right-Pointing-Pointer The milling duration has been optimized. Black-Right-Pointing-Pointer Sr0.8Bi2.2Ta2O9 milled for 20 hours exhibit enhanced electrical characteristics.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Solid Electrolyte Bimodal Grain Structures for Improved Cycling Performance

Here, the application of solid-state electrolytes in Li batteries is hampered by the occurrence of Li-dendrite-caused short circuits. To avoid cell failure, the electrolytes can only be stressed with rather low current densities, severely restricting their performance. As grain size and pore distributions significantly affect dendrite growth in ceramic electrolytes such as Li 7 La 3 Zr 2 O 12 and its variants; here, a “detour and buffer” strategy to bring the superiority of both coarse and fine grains into play, is proposed. To validate the mechanism, a coarse/fine bimodal grain microstructure is obtained by seeding unpulverized large particles in the green body. The rearrangement of coarse grains and fine pores is fine-tuned by changing the ratio of pulverized and unpulverized powders. The optimized bimodal microstructure, obtained when the two powders are equally mixed, allows, without extra interface decoration, cycling for over 2000 h as the current density is increased from 1.0 mA·cm -2 , and gradually, up to 2.0 mA·cm -2 . The “detour and buffer” effects are confirmed from postmortem analysis. The complex grain boundaries formed by fine grains discourage the direct infiltration of Li. Simultaneously, the coarse grains further increase the tortuosity of the Li path. This study sheds light on the microstructure optimization for the polycrystalline solid-state electrolytes.

25 ENERGY STORAGE↗

DOE OSTI2017

Metallic Nanocomposites as Next-Generation Thermal Interface Materials

Thermal interface materials (TIMs) are an integral and important part of thermal management in electronic devices. The electronic devices are becoming more compact and powerful. This increase in power processed or passing through the devices leads to higher heat fluxes and makes it a challenge to maintain temperatures at the optimal level during operation. Herein, we report a free standing nanocomposite TIM in which boron nitride nanosheets (BNNS) are uniformly dispersed in copper matrices via an organic linker, thiosemicarbazide. Integration of these metal-organic-inorganic nanocomposites was made possible by a novel electrodeposition technique where the functionalized BNNS (f-BNNS) experience the Brownian motion and reach the cathode through diffusion, while the nucleation and growth of the copper on the cathode occurs via the electrochemical reduction. Once the f-BNNS bearing carbonothioyl/thiol groups on the terminal edges come into the contact with copper crystals, the chemisorption reaction takes place. We performed thermal, mechanical, and structural characterization of these nanocomposites using scanning electron microcopy (SEM), diffusive laser flash (DLF) analysis, phase-sensitive transient thermoreflectence (PSTTR), and nanoindentation. The nanocomposites exhibited a thermal conductivity ranging from 211 W/mK to 277 W/mK at a filler mass loading of 0-12 wt.percent. The nanocomposites also have about 4 times lower hardness as compared to copper, with values ranging from 0.27 GPa to 0.41 GPa. The structural characterization studies showed that most of the BNNS are localized at grain boundaries - which enable efficient thermal transport while making the material soft. PSTTR measurements revealed that the synergistic combinations of these properties yielded contact resistances on the order of 0.10 to 0.13 mm2K/W, and the total thermal resistance of 0.38 to 0.56 mm2K/W at bondline thicknesses of 30-50 um. The coefficient of thermal expansion (CTE) of the nanocomposite is 11 ppm/K, which lies between the CTEs of aluminum (22 ppm/K) and silicon (3 ppm/K), which are common heat sink and heat source materials, respectively. The nanocomposite can also be deposited directly on to heat sink which will simplify the packaging processes by removing one possible element to assemble. These unique properties and ease of assembly makes the nanocomposite a promising next-generation TIM.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Metallic Nanocomposites as Next-Generation Thermal Interface Materials: Preprint

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2009

Microhardness Testing of Aluminum Alloy Welds

A weld is made when two pieces of metal are united or fused together using heat or pressure, and sometimes both. There are several different types of welds, each having their own unique properties and microstructure. Strength is a property normally used in deciding which kind of weld is suitable for a certain metal or joint. Depending on the weld process used and the heat required for that process, the weld and the heat-affected zone undergo microstructural changes resulting in stronger or weaker areas. The heat-affected zone (HAZ) is the region that has experienced enough heat to cause solid-state microstructural changes, but not enough to melt the material. This area is located between the parent material and the weld, with the grain structure growing as it progresses respectively. The optimal weld would have a short HAZ and a small fluctuation in strength from parent metal to weld. To determine the strength of the weld and decide whether it is suitable for the specific joint certain properties are looked at, among these are ultimate tensile strength, 0.2% offset yield strength and hardness. Ultimate tensile strength gives the maximum load the metal can stand while the offset yield strength gives the amount of stress the metal can take before it is 0.2% longer than it was originally. Both of these are good tests, but they both require breaking or deforming the sample in some way. Hardness testing, however, provides an objective evaluation of weld strengths, and also the difference or variation in strength across the weld and HAZ which is difficult to do with tensile testing. Hardness is the resistance to permanent or plastic deformation and can be taken at any desired point on the specimen. With hardness testing, it is possible to test from parent metal to weld and see the difference in strength as you progress from parent material to weld. Hardness around grain boundaries and flaws in the material will show how these affect the strength of the metal while still retaining the sample. This makes hardness testing a good test for identifying grain size and microstructure.

Bohanon, Catherine↗

DOE OSTI2024

Nuclear Fuel and Pu Redox Studies from The Glenn T. Seaborg Institute at Idaho National Laboratory

The Glenn T. Seaborg Institute at Idaho National Laboratory (INL-GTSI) focuses on advancing fundamental research in the actinide sciences by providing unique opportunities to early career scientists and engineers to gain experience studying the actinide elements and their associated systems. The INL-GTSI is built from three focus areas that are based on the expertise and supporting infrastructure at INL and include solid state chemistry and physics, solution phase chemistry and physics, and forensic and isotope science. INL is the lead Laboratory for nuclear energy research and development in the U. S. and the research on nuclear fuels performed under the INL-GTSI gives good examples of solid state studies. Uranium-Molybdenum (U-Mo) alloys are leading fuel candidates for conversion of high performance research and test reactors to low-enriched fuels. During irradiation, generated fission gas accumulates into bubbles and self-organizes into a gas bubble superlattice (GBS) that effectively stores fission gases and inhibits fuel swelling. A study on the early self- organizing behavior of the GBS shows that not only grain boundaries but the interfaces between the U-Mo matrix and uranium carbide (UC) impurities are important to GBS formation.[1] In solution, understanding the complex redox behavior of plutonium in aqueous environments is critical for establishing optimized nuclear waste reprocessing solvent systems and storage tank environments. INL-GTSI researchers have produced an experimentally validated multi-scale model of the gamma radiation induced behavior of plutonium ions in concentrated aqueous HNO3 solutions.[2] Here, gamma radiation effected only minimal steady state changes in the redox distribution of the plutonium oxidation states. The redox cycling between Pu(IV) and Pu(III) is demonstrated to be mediated by the •OH/NO3• radical oxidation of Pu(III) and the H2O2/HNO3 driven reduction of Pu(IV). The INL-GTSI offers young researchers the unique chance to work directly with actinide bearing materials in a U. S. National Laboratory environment. Further topical areas of interest to the INL-GTSI include, but are not limited to, fundamental actinide properties, structure/property (electronic, magnetic, thermal) relations, actinide quantum criticality, f- electron interactions, electron correlations, computational studies, new phases, defect effects, interface interactions, isotope production and separation, forensic analytical chemistry, structure and dynamic properties of actinides in non-aqueous media, separations chemistry and kinetics for advanced nuclear fuel cycles, radiation effects, and innovative and advanced ligand design for complexation of the actinides.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2018

Spatially Resolved Recombination Analysis of CuIn $_\text{x}$ Ga $_\text{1-x}$ Se $_{2}$ Absorbers With Alkali Postdeposition Treatments

In this contribution, we probe spatial variations in charge-carrier recombination in CuIn x Ga 1-x Se 2 (CIGS) absorbers grown on soda-lime glass (SLG) and alkali-free sapphire substrates with NaF and KF postdeposition treatments (PDTs). Temperature-and illumination-dependent device measurements are used to track interface recombination and recombination in the quasi-neutral region. The analysis of these data reveals that the benefit of alkali PDTs depends on the substrate: interface recombination is reduced in devices grown on sapphire substrates, whereas recombination in the quasi-neutral regions is reduced in devices grown on SLG substrates. Cathodoluminescence (CL) spectrum imaging is used to study the spatial distribution of recombination with respect to the grain structure. The grain-boundary CL contrast is similar in films with no PDT, NaF PDT, or KF PDT. A reduced grain-boundary contrast is observed with a NaF + KF PDT; however, suggesting a reduced recombination strength at the grain boundaries (GBs) for combined NaF + KF treatment. CL spectra indicate band tailing, consistent with the fluctuating potential model. Fluctuating potentials are believed to reduce open-circuit voltage, but their spatial distribution has not been studied. Here, CL spectrum imaging data are used to generate maps of the root-mean-square value of the potential energy fluctuations-γ. These maps reveal a bimodal ..gamma.. distribution for all samples: ..gamma.. is generally in the range ~15-50 meV or ~100-180 meV. The higher ..gamma.. range is more significantly affected by the PDTs; after the PDTs, it is strongly correlated with GBs. The lower ..gamma.. range is correlated with higher emission intensity regions, typically grain interiors, and increases in area fraction after the PDTs. These results demonstrate how spatially resolved luminescence and device characterization measurements can be used to monitor changes in recombination in CIGS films and photovoltaic devices. Such measurements can complement empirical device optimization and help improve device performance.

14 SOLAR ENERGY↗

DOE OSTI2017

Computational design and performance prediction of creep-resistant ferritic superalloys

Ferritic superalloys containing the B2 phase with the parent L21 phase precipitates in a disordered solid-solution matrix, also known as a hierarchical-precipitate-strengthened ferritic alloy (HPSFA), had been developed for high-temperature structural applications in fossil-energy power plants. These alloys were designed by adding Ti into a previously-studied NiAl-strengthened ferritic alloy (denoted as FBB8 in this study). Following with the concept of HPSFAs, in the present research, a systematic investigation on adding other elements, such as Hf and Zr, and optimizing the Ti content within the alloy system, has been conducted, in order to further improve the creep resistance of the model alloys. Studies include advanced experimental techniques, first-principles calculations on thermodynamic and mechanical properties, and numerical simulations on precipitation hardening, have been integrated and conducted to characterize the complex microstructures and excellent creep resistance of alloys. The experimental techniques include transmission-electron microscopy (TEM), scanning-electron microscopy (SEM), neutron diffraction (ND), and atom-probe tomography (APT), which provide the detailed microstructural information of the model alloys. Systematic tension/compression creep tests have also been conducted in order to verify the creep resistance of the potential alloy compositions. The results show that when replacing Ti with Hf and Zr, it does not form the L21 phase. Instead, the hexagonal Laves phase forms and distributes majorly along the grain boundary, or large segregation within grains. Since the Laves phase does not form parent to the B2-phase precipitates, it cannot bring the strengthening effect of HPSFAs. As a result, the FBB8 + 2 wt. % Hf and FBB8 + 2 wt. % Zr alloys have similar mechanical properties to the original FBB8. The FBB8 + Ti series alloys had also been studied, from the creep tests and microstructural characterizations, the FBB8 + 3.5 wt.% Ti possesses the greatest creep resistance, with the L21/B2 phase ratio of 4 (80% of the precipitates is the L21 phase, and 20% is the B2 phase). First-principles calculations include thermodynamics, elastic properties, and interfacial properties, which have been conducted for the understanding of the thermodynamic and mechanical properties of HPSFAs. In addition to the systematic experimental approach and first-principles calculations, a series of numerical tools and algorithms, which assist in the optimization of creep properties of ferritic superalloys, are utilized and developed. These numerical simulation results are compared with the available experimental data and previous first-principles calculations, providing the deep insight of creep mechanisms of the creep-resistant ferritic superalloys. To conclude the present research, we’ve found that (1) only FBB8 + Ti alloys have the potential of forming HPSFA, and FBB8 + Hf and FBB8 + Zr do not work. Therefore, only FBB8 + Ti alloys have desirable creep resistance, (2) the optimum composition for the FBB8 + Ti alloys is FBB8 + 3.5% Ti, which has the greatest creep resistance (218.8 MPa as the threshold stress at 700 oC), (3) first-principle calculations obtained results that could not be obtained in experiments, which are relevant to develop ferritic superalloys with the improved creep resistance, and (4) two-dimensional dislocation-dynamics simulations investigate effects of factors like precipitate volume fractions and precipitate radii in the alloy systems, which helps in developing the most desirable microstructure with greatest strengthening.

20 FOSSIL-FUELED POWER PLANTS↗

DOE OSTI2021

Bifunctional nanoprecipitates strengthen and ductilize a medium-entropy alloy

Single-phase high- and medium-entropy alloys with face-centred cubic (fcc) structure can exhibit high tensile ductility and excellent toughness, but their room-temperature strengths are low. Dislocation obstacles such as grain boundaries, twin boundaries, solute atoms and precipitates can increase strength. However, with few exceptions, such obstacles tend to decrease ductility. Interestingly, precipitates can also hinder phase transformations. Here, using a model, precipitate-strengthened, Fe–Ni–Al–Ti medium-entropy alloy, we demonstrate a strategy that combines these dual functions in a single alloy. The nanoprecipitates in our alloy, in addition to providing conventional strengthening of the matrix, also modulate its transformation from fcc-austenite to body-centred cubic (bcc) martensite, constraining it to remain as metastable fcc after quenching through the transformation temperature. During subsequent tensile testing, the matrix progressively transforms to bcc-martensite, enabling substantial increases in strength, work hardening and ductility. This use of nanoprecipitates exploits synergies between precipitation strengthening and transformation-induced plasticity, resulting in simultaneous enhancement of tensile strength and uniform elongation. Further, our findings demonstrate how synergistic deformation mechanisms can be deliberately activated, exactly when needed, by altering precipitate characteristics (such as size, spacing, and so on), along with the chemical driving force for phase transformation, to optimize strength and ductility.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Frequency-Dependent Properties of Magnetic Nanoparticle Crystals

In the proposed research program we will investigate the time- and frequency-dependent behavior of ordered nanoparticle assemblies, or nanoparticle crystals. Magnetostatic interactions are long-range and anisotropic, and this leads to complex behavior in nanoparticle assemblies, particularly in the time- and frequency-dependent properties. We hypothesize that the high frequency performance of composite materials has been limited because of the range of relaxation times; if a composite is a dipolar ferromagnet at a particular frequency, it should have the advantages of a single phase material, but without significant eddy current power losses. Arrays of surfactant-coated monodomain magnetic nanoparticles can exhibit long-range magnetic order that is stable over time. The magnetic domain size and location of domain walls is governed not by structural grain boundaries but by the shape of the array, due to the local interaction field. Pores or gaps within an assembly pin domain walls and limit the domain size. Measurements of the magnetic order parameter as a function of temperature showed that domains can exist at high temoerature, and that there is a collective phase transition, just as in an exchange-coupled ferromagnet. Dipolar ferromagnets are not merely of fundamental interest; they provide an interesting alternative to exchange-based ferromagnets. Dipolar ferromagnets made with high moment metallic particles in an insulating matrix could have high permeability without large eddy current losses. Such nanocomposites could someday replace the ferrites now used in phase shifters, isolators, circulators, and filters in microwave communications and radar applications. We will investigate the time- and frequency-dependent behavior of nanoparticle crystals with different magnetic core sizes and different interparticle barrier resistances, and will measure the magnetic and electrical properties in the DC, low frequency (0.1 Hz - 1 kHz), moderate frequency (10 Hz - 500 MHz), and high frequency (up to 20 GHz) regimes. Our results will demonstrate whether a DC dipolar ferromagnet shows collective frequency-dependent reponse similar to that of an exchange-based ferromagnet, and will provide data for comparison of optimal nanocomposite properties with those of ferrites used in high frequency applications. Both the magnetic and electronic response of the composites will be examined in order to determine the frequency range where hopping conductivity leads to significant eddy current power losses. In the high frequency regime we will look for evidence of spin wave quantization and the resulting decrease in non-linear spin wave processes that could affect the performance of high frequency magnetic devices.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Exploring the relationship between deposition method, microstructure, and performance of Nb/Si-based superconducting coplanar waveguide resonators

Superconducting quantum circuits (SQC) are one of the most promising hardware platforms for quantum computing, yet their performance is currently limited by the presence of various structural defects inside the circuit's structure. Despite impressive progress in the past decade, a precise understanding of the origin of these defects from various fabrication processes and their impact on coherence is still lacking. Here, in this study, we performed a comprehensive investigation on the microstructure, superconductivity, and resonator quality factor of Nb films deposited by high-power impulse magnetron sputtering (HiPIMS) and direct current (DC) magnetron sputtering. A suite of characterization techniques, including electron microscopy with spectroscopy, secondary ion mass spectrometry, magneto-optical microscopy, and pump-probe reflectivity spectroscopy is used. We reveal that niobium (Nb) resonators fabricated using HiPIMS exhibit a smaller average grain size, thicker surface oxide with larger thickness variations (rougher surface), and a thicker amorphous Nb/Si interface layer compared to samples deposited by DC sputtering. We identified that the amorphous Nb oxides (mainly located at the Nb surface and along the grain boundaries) and Nb-Si amorphous layers (at the Nb/Si interface) are major and potential sources of two-level system (TLS), while off-stochiometric oxides and suboxides of Nb close to the surface, crystalline defects (i.e., dislocations at grain boundary, point defects introduced during deposition) are main contributors of non-TLS sources. Our findings clarify the relationship between different defects and coherence loss mechanisms, highlighting the importance of material microstructure control on performance optimization in SQC.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Recent Advances in Analytical Electron Microscopy for Irradiated Materials

Analytical electron microscopy (AEM) in the scanning transmission electron microscope (STEM) has long been a staple of post-irradiation examination (PIE) and materials development campaigns. Recently, new advances in both STEM hardware and post-processing data-analysis software, along with ancillary advances such as in focused ion beam (FIB) sample preparation, has led to exciting advances in the quantity and quality of data that can be obtained. This talk will summarize recent experiments performed at Oak Ridge National Laboratory (ORNL), especially work on neutron-irradiated materials and fuels taking advantage of a newly-installed latest-generation AEM tool in the ORNL irradiated materials laboratories. ORNL installed a new FEI Talos F200X microscope, a 200 keV, high-brightness Schottky emission AEM system optimized for high-speed, high-efficiency X-ray mapping experiments. The F200X features the FEI 'SuperX' four-sector silicon drift detector (SDD) X-ray detector, which provides 0.9 sr solid angle of collection. By combining the high-brightness electron source, latest-generation electron optics, and fast computers and pulse processors, X-ray mapping speed is increased by a factor of 50-100 x compared to the previous-generation instruments. In addition to improvements in hardware, data mining via multivariate statistical analysis (MVSA) allows for maximum insight to the data obtained from the new hardware. MVSA data mining of the X-ray maps allows, for instance, unbiased computational identification of the phases present, and discovery of small phases or precipitates not expected by the human analyst. This talk will present examples of experiments performed using the most modern AEM tools and software. Silicon carbide is a major candidate for next-generation nuclear applications. Nano-infiltration by transient eutectic (NITE) SiC requires low sintering temperatures. X-ray mapping of the NITE structure find pockets of different oxides, such as Zr-Y-oxide, Y-Al-oxide, and yttria. MVSA data mining finds the regions where different oxides are present and indicates that Y additions preferentially wet grain boundaries, where Zr additions are preferentially concentrated at grain triple points. SiC coatings from AGR-I experiment TRISO particles were found to contain significant quantities of fission products (e.g., Pd) as well as actinides (U, Pu). MVSA data mining found complex precipitates and grain boundary films of the fission products and actinides deep (∼several microns) into the SiC layer. Advanced AEM methods, combined with MVSA data mining, makes possible both rapid and detailed PIE. Ferritic alloys, such as accident-tolerant FeCrAl grades, benefit greatly from advanced AEM examination. Neutron-irradiated FeCrAl precipitates the detrimental Cr-rich α' phase. Because the SuperX SDD system has four detectors, it is possible to obtain high X-ray count rates even on a highly tilted specimen, as might be needed to obtain STEM images of dislocation loops. Results on neutron-irradiated FeCrAl indicates that α' size and number density can be obtained by AEM, and MVSA results determine that minor elements (such as Si) has complex radiation-induced segregation behavior at grain boundaries. We have also developed and validated computer models of the AEM experiment, allowing different microstructures' X-ray map results to be simulated for different STEM instruments. This allows X-ray mapping to be more quantitative, such as by estimating what size nanoclusters in an oxide-dispersion strengthened steel would be visible or invisible in STEM. In summary, new advanced AEM technology provides a major leap forward in experiments possible in PIE of irradiated materials. (authors)

36 MATERIALS SCIENCE↗

NASA NTRS1990

Characterization of Iridium Coated Rhenium Used in High-Temperature, Radiation-Cooled Rocket Thrusters

Materials used for radiation-cooled rocket thrusters must be capable of surviving under extreme conditions of high-temperatures and oxidizing environments. While combustion efficiency is optimized at high temperatures, many refractory metals are unsuitable for thruster applications due to rapid material loss from the formation of volatile oxides. This process occurs during thruster operation by reaction of the combustion products with the material surface. Aerojet Technical Systems has developed a thruster cone chamber constructed of Re coated with Ir on the inside surface where exposure to the rocket exhaust occurs. Re maintains its structural integrity at high temperature and the Ir coating is applied as an oxidation barrier. Ir also forms volatile oxide species (IrO2 and IrO3) but at a considerably slower rate than Re. In order to understand the performance limits of Ir-coated Re thrusters, we are investigating the interdiffusion and oxidation kinetics of Ir/Re. The formation of iridium and rhenium oxides has been monitored in situ by Raman spectroscopy during high temperature exposure to oxygen. For pure Ir, the growth of oxide films as thin as approximately 200 A could be easily detected and the formation of IrO2 was observed at temperatures as low as 600 C. Ir/Re diffusion test specimens were prepared by magnetron sputtering of Ir on Re substrates. Concentration profiles were determined by sputter Auger depth profiles of the heat treated specimens. Significant interdiffusion was observed at temperatures as low as 1000 C. Measurements of the activation energy suggest that below 1350 C, the dominant diffusion path is along defects, most likely grain boundaries, rather than bulk diffusion through the grains. The phases that form during interdiffusion have been examined by x ray diffraction. Analysis of heated test specimens indicates that the Ir-Re reaction produces a solid solution phase of Ir dissolved in the HCP structure of Re.

Stulen, R. H.↗