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DOE OSTI2019

Atomically imaged crystal structure and normal-state properties of superconducting C a 10 P t 4 A s 8 ( ( F e 1 – x P t x ) 2 A s 2 ) 5

Superconducting Ca 10 Pt 4 As 8 (Fe 2 As 2 ) 5 is rare because optimal superconducting transition temperature is achieved without chemical doping or pressure. Furthermore, the unclear crystal structure limits our ability to understand the structure-property relationship. Using atomically resolved scanning transmission electron microscopy and electron diffraction, we directly determine the structure of this superconductor: it forms a monoclinic structure (space group P 2 1 /n) with lattice parameters a = b = 8.76Å, c = 20.18Å, and γ = 90.5°. Compared with previously reported structures derived from diffraction experiments, the c-lattice constant is doubled due to alternating stacking of Pt 4 As 8 layers, which induces a high density of stacking faults. With the establishment of the crystal structure, stacking faults, and chemical composition, the distinctive normal-state electrical and thermal transport properties of our superconducting Ca 10 Pt 4 As 8 ((Fe 1–x Pt x ) 2 As 2 ) 5 (x ~ 0.05) single crystals can be explained.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2017

Magnetic and magnetocaloric properties of HoCr O 3 tuned by selective rare-earth doping

Rare-earth chromites ( R Cr O 3 ) are an important subclass of functional materials with interesting magnetic, electrical, and catalytic properties that make them promising for various applications. In this paper, we report comparisons on the structural and magnetic properties of HoCr O 3 with those of H o 0.67 T m 0.33 Cr O 3 and H o 0.67 G d 0.33 Cr O 3 powder samples, which were doped by T m 3 + (or G d 3 + ) ions at the A -site with ionic radius smaller (or larger) than that of H o 3 + ion. The structural properties of the samples were characterized by x-ray diffraction, Raman spectroscopy, and scanning electron microscopy carried out at ambient. The band gaps of the three samples were determined by analyzing their ultraviolet Vis spectra. Magnetic studies carried out from 5 K to 300 K show that the Néel temperature ( T N Cr , where C r 3 + ions order) increases with an increase in the average A -site ( R -site) ionic radius, tolerance factor, and Cr1-O1-Cr1 bond angle but decreases with an increase in the orthorhombic strain factor. In addition, the application of external hydrostatic pressure was found to enhance T N Cr of HoCr O 3 , similar to the effect observed by doping HoCr O 3 with G d 3 + ions. These changes in T N Cr with A -site doping and hydrostatic pressure are related to changes in C r 3 + - C r 3 + exchange coupling resulting from changes in the Cr1-O1-Cr1 bond angle and Cr1-O1 bond lengths, respectively. Temperature dependent paramagnetic susceptibility data of the samples was fitted to the modified Curie-Weiss law that included the Dzyloshinskii-Moriya interaction. Isothermal magnetization data showed that the magnetic behavior of the samples changes from canted antiferromagnetic at low temperatures to paramagnetic at higher temperatures. The large magnetocaloric entropy change was observed in HoCr O 3 , which was enhanced by Gd doping but lowered by Tm doping, showing its tunability by A -site doping. Correlation between magnetoelectric properties and magnetization is discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Nanoscale symmetry fluctuations in ferroelectric barium titanate, BaTiO 3

Crystal charge density is a ground-state electronic property. In ferroelectrics, charge is strongly influenced by lattice and vice versa , leading to a range of interesting temperature-dependent physical properties. However, experimental determination of charge in ferroelectrics is challenging because of the formation of ferroelectric domains. Demonstrated here is the scanning convergent-beam electron diffraction (SCBED) technique that can be simultaneously used for imaging ferroelectric domains and identifying crystal symmetry and its fluctuations. Results from SCBED confirm the acentric tetragonal, orthorhombic and rhombohedral symmetry for the ferroelectric phases of BaTiO 3 . However, the symmetry is not homogeneous; regions of a few tens of nanometres retaining almost perfect symmetry are interspersed in regions of lower symmetry. While the observed highest symmetry is consistent with the displacive model of ferroelectric phase transitions in BaTiO 3 , the observed nanoscale symmetry fluctuations are consistent with the predictions of the order–disorder phase-transition mechanism.

Chemistry↗

DOE OSTI2016

Calcium-Iron Oxide as Energy Storage Medium in Rechargeable Oxide Batteries

Rechargeable oxide batteries (ROB) comprise a regenerative solid oxide cell (rSOC) and a storage medium for oxygen ions. A sealed ROB avoids pumping loss, heat loss, and gas purity expenses in comparison with conventional rSOC. However, the iron oxide base storage medium degrades during charging–discharging cycles. In comparison, CaFe 3 O 5 has improved cyclability and a high reversible oxygen storage capacity of 22.3 mol%. In this paper, we analyzed the redox mechanism of this compound. After a solid-state synthesis of CaFe 3 O 5 , we verified the phase composition and studied the redox reaction by means of X-ray diffraction, Mössbauer spectrometry, and scanning electron microscopy. Finally, results show a great potential to operate the battery with this storage material during multiple charging–discharging cycles.

25 ENERGY STORAGE↗

DOE OSTI2021

Relationship of Chemical Composition and Moisture Sensitivity in LiNi x Mn y Co 1-x-y O 2 for Lithium-Ion Batteries

Chemical composition–moisture sensitivity relationship of LiNi x Mn y Co 1-x-y O 2 (NMC) cathode materials was investigated by exploring crystal structures, surface properties, and electrochemical performance behaviors of various commercial NMC powders: LiNi 1/3 Mn 1/3 Co 1/3 O 2 (NMC111), LiNi 0.5 Mn 0.3 Co 0.2 O 2 (NMC532), LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622), and LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811). The NMC powders were stored in different moisture conditions: moisture-free, humidified air, or immersed in water. Rietveld refinement analysis of X-ray diffraction (XRD) data and scanning electron microscopy (SEM) were used to characterize the crystal structure changes and the evolution of particle surfaces morphologies. The effect of moisture contamination on the electrochemical properties of NMC cathodes was studied by galvanostatic cycling and electrochemical impedance spectroscopy (EIS). The moisture contamination resulted in either structural disorder or unwanted surficial deposition products, which increased a charge-transfer impedance and consequent performance degradation of battery cells. The results showed that NMC’s moisture vulnerability increased with Ni content (x) despite protective coatings on commercial particles, which stressed the necessity of alternative surface passivation strategies of Ni-rich NMC for broad applications such as electric vehicles and electrified aircraft propulsion.

25 ENERGY STORAGE↗

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

Development of High-Performance Ni-base Alloys for Gas Turbine Wheels Using a Coprecipitation Approach (Final Technical Report)

In this project, a synergistic approach involving experiments informed by modelling was used to develop γ'/γ'' coprecipitation-strengthened Ni-base superalloys for land-based gas turbine wheels. In thick sections of such turbine wheels, the slow cooling rate normally observed, as well as variations in cooling rate could potentially result in drastically inhomogeneous and coarsened microstructure. Thus, ten alloy compositions were selected based on coprecipitation and sluggish γ’ growth and coarsening during three iterations of alloy development, assisted by extensive CALPHAD modeling. Phase equilibrium calculations, informed by the characterization of early alloys, were successful in predicting suitable aging treatments to obtain bimodal coprecipitate distribution in several alloys. These aging treatments were applied to the subsequent round of alloys and the resulting microstructures were characterized in detail. Two different cooling rates were used during each of these heat treatments to simulate the range of cooling rates observed in a thick section forging. The microstructures were used to calibrate a multi-phase field model (MPF), which was used to study the formation mechanisms of various coprecipitate morphologies observed in the experiments. Following this, the most promising alloys in each round were selected and studied using high temperature tensile and creep tests. Considering that a slower cooling rate would lead to a strength debit, while a faster cooling rate might lead to a decline in creep rupture life of a full-scale wheel, tensile tests were carried out for slower cooled samples, while creep tests were carried out for faster cooled samples. The deformation microstructures were then characterized using advanced characterization techniques such as Diffraction Contrast-Scanning Transmission Electron Microscopy (DC-STEM) and Electron Channeling Contrast Imaging (ECCI). Further, a mean-field creep model was developed and calibrated using these experimental findings to predict long-term creep behavior of these coprecipitation-strengthened alloys.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Scale-Up of Lithium Iron & Aluminum Nickelate Advanced Cathode and Fabrication of A Battery Pack Comprising The Same

Global battery manufacturers are increasingly worried about the serious supply chain constraint caused by rapid fluctuations in cobalt prices over the years. We present a novel cobalt-free, nickel-rich layered cathode material called NFA class (LiNixFeyAlzO2) to tackle this challenge. Spherical NFA(OH)2 precursors were successfully synthesized by incorporating Ni, Fe, and Al elements using a co-precipitation reaction in a continuous stirred tank reactor. The LiNFAO2 cathode, composed of LiNi0.85Fe0.05Al0.1O2, was synthesized and analyzed using X-Ray diffraction, Mössbauer spectroscopy, and scanning electron microscopy (SEM). The material's electrochemical behavior was evaluated through various techniques at different lithiation/delithiation states in two voltage ranges. The cobalt-free material exhibits a high capacity of 190 mAh/g at 0.1C within the voltage range of 3V-4.5V, as demonstrated by electrochemical performance evaluations. Rate and cycling evaluations showed good rate capability and cycling stability, with 88% capacity retention after 100 cycles at C/3 within the voltage range of 3V-4.3V. Our research shows the great potential of cobalt-free NFA cathodes as a feasible option for developing cost-effective lithium-ion batteries.

25 ENERGY STORAGE↗

DOE OSTI2024

Scale-Up of Lithium Iron & Aluminum Nickelate Advanced Cathode and Fabrication of A Battery Pack Comprising The Same

25 ENERGY STORAGE↗

DOE OSTI2022

Nanoindentation Investigation of Chloride-Induced Stress Corrosion Crack Propagation in an Austenitic Stainless Steel Weld

Transgranular chloride-induced stress corrosion cracking (TGCISCC) is a mounting concern for the safety and longevity of arc welds on austenitic stainless steel (AuSS) nuclear waste storage canisters. Recent studies have shown the key role of crystallography in the susceptibility and propagation of TGCISCC in SS weldments. Given that crystallography underlies mechanical heterogeneities, the mechanical-crystallographic relationship during TGCISCC growth must be understood. In this study, welded SS 304L coupons are loaded in four-point bend fixtures and then boiled in magnesium chloride to initiate TGCISCC. Nanoindentation mapping is paired with scanning electron microscopy (SEM) electron backscatter diffraction (EBSD) to understand the correlation between grain orientation, grain boundaries, and hardening from TGCISCC propagation. The nanoindentation hardness of individual grains is found to not be a controlling factor for TGCISCC propagation. However, intragranular hardness is generally highest immediately around the crack due to localized strain hardening at the crack tip. This work shows that nanoindentation techniques can be useful in understanding CISCC behaviors when paired with electron microscopy.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Effect of Ni-Content on the Transformation Temperatures in NiTi-20 at. % Zr High Temperature Shape Memory Alloys

The effect of Ni-content on phase transformation behavior of NiTi-20 at. % Zr high temperature shape memory alloy (HTSMA) is investigated over a small composition range, i.e., 49.8, 50.0 and 50.2 at. % Ni, by differential scanning calorimetry (DSC), high-energy synchrotron radiation X-ray diffraction (SR-XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). All samples show a monoclinic B19' martensitic structure at room temperature. It is shown that even with these small variations in Ni-content, the alloy shows vastly different transformation temperatures and responds in a drastically different manner to aging treatments at 550 and 600 °C. Lastly, a discussion on H-phase composition with respect to bulk composition is presented.

36 MATERIALS SCIENCE↗

NASA NTRS1975

Interaction of hydrogen chloride with alumina

The influence of outgas conditions and temperature on the adsorptive properties of two aluminas Alon-c and Al6sG were studied using adsorption isotherm measurements. Alon-C and Al6SG were characterized using X-ray powder diffraction, thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and BET nitrogen surface areas. Some of these techniques were applied to two other aluminas but no isotherm data was obtained. Isotherm data and techniques applied to each alumina are summarized in tabular form.

Bailey, R. R.↗

NASA NTRS1977

Analysis of ablation debris from natural and artificial iron meteorites

Artificial ablation studies were performed on iron and nickel-iron samples using an arc-heated plasma of ionized air. Experiment conditions simulated a meteoroid traveling about 12 km/sec at an altitude of 70 km. The artificially produced fusion crusts and ablation debris show features very similar to natural fusion crusts of the iron meteorites Boguslavka, Norfork, and N'Kandhla and to magnetic spherules recovered from Mn nodules. X-ray diffraction, electron microprobe, optical, and scanning electron microscope analyses reveal that important mineralogical, elemental, and textural changes occur during ablation. Some metal is melted and ablated. The outer margin of the melted rind is oxidized and recrystallizes as a discontinuous crust of magnetite and wustite. Adjacent to the oxidized metallic ablation zone is an unoxidized metallic ablation zone in which structures such as Widmannstatten bands are obliterated as the metal is transformed to unequilibrated alpha 2 nickel-iron. Volatile elements are vaporized and less volatile elements undergo fractionation.

Blanchard, M. B.↗

NASA NTRS1985

Oxidation of silicon nitride sintered with rare-earth oxide additions

The effects of rare-earth oxide additions on the oxidation of sintered Si3N4 were examined. Insignificant oxidation occurred at 700 and 1000 C, with no evidence of phase instability. At 1370 C, the oxidation rate was lowest for Y2O3 and increased for additions of La2O3, Sm2O3, and CeO2, in that order. Data obtained from X-ray diffraction, electron microprobe analysis, and scanning electron microscopy indicate that oxidation occurs via diffusion of cationic species from Si3N4 grain boundaries.

Mieskowski, D. M.↗

NASA NTRS1986

Oxidation and emittance of superalloys in heat shield applications

Recently developed superalloys that form alumina coatings have a high potential for heat shield applications for advanced aerospace vehicles at temperatures above 1095C. Both INCOLOY alloy MA 956 (of the Inco Alloys International, Inc.), an iron-base oxide-dispersion-strengthened alloy, and CABOT alloy No. 214 (of the Cabot Corporation), an alumina-forming nickel-chromium alloy, have good oxidation resistance and good elevated temperature strength. The oxidation resistance of both alloys has been attributed to the formation of a thin alumina layer (alpha-Al2O3) at the surface. Emittance and oxidation data were obtained for simulated Space Shuttle reentry conditions using a hypersonic arc-heated wind tunnel. The surface oxides and substrate alloys were characterized using X-ray diffraction and scanning and transmission electron microscopy with an energy-dispersive X-ray analysis unit. The mass loss and emittance characteristics of the two alloys are discussed.

Wiedemann, K. E.↗

NASA NTRS1988

Synthesis and characterization of high-T(sub c) screen-printed Y-Ba-Cu-O films on alumina

Thick films of YBa2Cu3O(sub 7-x) have been deposited on highly polished alumina substrates by the screen printing technique. To optimize the post-printing heat treatment, the films were baked at various temperatures for different lengths of time and oxygen-annealed at a lower temperature. The resulting films were characterized by electrical resistivity measurements, x-ray diffraction, and optical and scanning electron microscopy. Properties of the films were found to be highly sensitive to the post-printing thermal treatment. Films baked for 15 min at 1000 C in oxygen were hard, adherent, near single phase, and superconducting with T(sub c)(onset) approx 96 K, T(sub c)(zero) approx 66 K and Delta T sub c (10 to 90 percent) approx 10 K.

Bansal, Narottam P.↗

NASA NTRS1988

Synthesis and characterization of high-T(c) screen-printed Y-Ba-Cu-O films on alumina

Thick films of YBa2Cu3O(sub 7-x) have been deposited on highly polished alumina substrates by the screen printing technique. To optimize the post-printing heat treatment, the films were baked at various temperatures for different lengths of time and oxygen-annealed at a lower temperature. The resulting films were characterized by electrical resistivity measurements, X-ray diffraction, and optical and scanning electron microscopy. Properties of the films were found to be highly sensitive to the post-printing thermal treatment. Films baked for 15 min at 1000 C in oxygen were hard, adherent, near single phase, and superconducting with T(sub c) (onset) approx 96 KK, T(sub c) (zero) approx 66 K and Delta T sub c (10 to 90 percent) approx 10 K.

Bansal, Narottam P.↗

NASA NTRS2017

Basalt Weathering in a Cold and Icy Climate: Three Sisters, Oregon as an Analog for Early Mars

There is abundant evidence for liquid water on early Mars, but the debate remains whether early Mars was warm and wet or cold and icy with punctuated periods of melting. To further investigate the hypothesis of a cold and icy early Mars, we collected rocks and sediments from the Collier and Diller glacial valleys in the Three Sisters volcanic complex in Oregon. We analyzed rocks and sediments with X-ray diffraction (XRD), scanning and transmission electron microscopies with energy dispersive spectroscopy (SEM, TEM, EDS), and visible, short-wave infrared (VSWIR) and thermal-IR (TIR) spectroscopies to characterize chemical weathering and sediment transport through the valleys. Here, we focus on the composition and mineralogy of the weathering products and how they compare to those identified on the martian surface. Phyllosilicates (smectite), zeolites, and poorly crystalline phases were discovered in pro- and supra-glacial sediments, whereas Si-rich regelation films were found on hand samples and boulders in the proglacial valleys. Most phyllosilicates and zeolites are likely detrital, originating from hydrothermally altered units on North Sister. TEM-EDS analyses of the <2 um size fraction of glacial flour samples demonstrate a variety of poorly crystalline (i.e., no long-range crystallographic order) phases: iron oxides, devitrified volcanic glass, and Fe-Si-Al phases. The CheMin XRD on the Curiosity rover in Gale crater has identified significant amounts of X-ray amorphous materials in all samples measured to date. The amorphous component is likely a combination of silicates, iron oxides, and sulfates. Although we have not yet observed amorphous sulfate in the samples from Three Sisters, the variety of poorly crystalline weathering products found at this site is consistent with the variable composition of the X-ray amorphous component identified by CheMin. We suggest that these amorphous phases on Mars could have formed in a similarly cold and icy environment.

Rampe, E. B.↗