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At least 1,027 records · Page 57
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

MULTI-TECHNIQUE CHARACTERIZATION OF SUPERCONDUCTING MATERIALS FOR PARTICLE ACCELERATOR APPLICATIONS

We investigated the performance limitations of superconducting radio-frequency (SRF) cavities and materials using multiple experimental techniques. In particular, this study focuses on understanding the surface properties of nitrogen-doped Nb cavities and super?conducting thin films with higher Tc such as Nb3Sn. The main goal of this work is to use different techniques to better understand each aspect of the complex loss mechanism in superconductors to further improve the already highly efficient SRF cavities. Nitrogen doping applied to a Nb SRF cavity significantly improves the quality factor Q0 compared to a conventional Nb cavity, at an expense of reduced maximum accelerating gradient. The early quench mechanism was analyzed by using temperature maps before and during the quenching. The temperature maps revealed insignificant heating before the quench, and we concluded that nitrogen doping reduces critical magnetic fields in local regions, leading to premature quenching. To understand the origin of the increasing Q0 with the rf field, the density of states (DOS) of cold spots from nitrogen-doped and standard cavities were measured and analyzed using scanning tunneling microscopy. The results suggested that nitrogen doping reduces the spatial inhomogeneity of superconducting properties and shrinks the metallic suboxide layers, which tunes the DOS in such a way as to produce the field-induced reduction in the surface resistance. To characterize SRF thin films, an experimental setup for measuring a coplanar waveguide (CPW) resonator was developed and tested. A surface impedance measurement of the Nb film showed good agreement with the BCS calculation. The preliminary results from measurements of Nb3Sn and NbTiN films are also presented here. The nonlinear Meissner effect was investigated in Nb3Sn film CPW resonators by mea?suring the resonant frequency as a function of a parallel magnetic field. Contrary to a conventional quadratic dependence of the penetration depth ?(B) on the applied magnetic field B, as expected in s-wave superconductors, nearly a linear increase of ?(B) with B was observed. It was concluded that this behavior of ?(B) is due to weakly linked grain bound?aries on the polycrystalline Nb3Sn films, which can mimic the NLME expected in a clean d-wave superconductor.

Makita, Junki↗
DOE OSTI2024

Experimental and Numerical Characterization of High Temperature Deformation Behavior of 347H Stainless Steel

This study investigates how temperature affects the plasticity and thermal creep behavior of 347H stainless steel under uniaxial tension. The research combined experimental testing with advanced computational modeling. Two types of experiments were conducted: uniaxial tensile tests at temperatures from 100°C to 750°C using strain rates of ~10⁻⁴ s⁻¹, and creep tests at temperatures between 600°C and 750°C under various stress levels. These experimental results were used to develop and validate a new integrated mechanistic model that can predict material behavior under any loading condition while accounting for both stress and temperature effects. The model was implemented using a polycrystalline microstructure simulation framework based on elasto-viscoplastic Fast Fourier Transform (EVPFFT). It incorporates three key deformation mechanisms: thermally activated dislocation glide, dislocation climb, and vacancy diffusional creep. The model accounts for internal stress distribution within single crystals and considers how precipitates and solute atoms (both interstitial and substitutional) affect dislocation movement. After validation against experimental data, the model was used to generate Ashby-Weertman deformation mechanism maps for 347H steel, providing new insights into how microstructure influences the activation of different creep mechanisms.

Joy, Jobin K.↗
DOE OSTI2022

Crystalline Orientation–Dependent Spin Hall Effect in Epitaxial Platinum

We report on the spin Hall effect in epitaxial Pt films with well-defined crystalline (200), (220), and (111) orientations and smooth surfaces. The magnitude of the spin Hall effect has been determined by spin–torque ferromagnetic resonance measurements on epitaxial Pt/Py heterostructures. We observed a 54% enhancement of the charge-to-spin conversion efficiency of the epitaxial Pt when currents are applied along the in-plane <002> direction. Temperature-dependent harmonic measurements on epitaxial Pt/Co/Ni heterostructures compared to a polycrystalline Pt/Co/Ni suggest the extrinsic mechanism underlying spin Hall effect in epitaxial Pt. Our work contributes to the development of energy-efficient spintronic devices by engineering the crystalline anisotropy of non-magnetic metals.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2022

Critical Shape for the Growth of Grain Boundary Twin Embryos in Mg and Mg Alloys: Crystal Plasticity Modeling

Application of polycrystalline hexagonal close packed (HCP) metals in engineering designs has been constrained by their anisotropic responses due to twinning and limited plasticity. In deformation, twins most often initiate at grain boundaries (GBs), and thicken and propagate across the grain. In this work, the GB twin embryos in Mg and Mg alloys, and the conditions that influence their propagation are investigated. Using a micromechanical crystal plasticity model, the role of embryo shape on the driving forces prevailing at the embryo boundaries that could support its expansion is studied. The modeled embryos are either planar, extending more in the shear direction than normal to the twin plane, or equiaxed. Results show that the thinner the embryo, the greater the driving forces for both thickening and forward propagation. Alloys with low prismatic-to-basal critical resolved shear stress (CRSS) ratios promote embryo thickening and large CRSS values for the slip mode that primarily accommodates the twin shear encourage propagation. The neighboring grains with orientations that enable local accommodation of the embryo twin shear by pyramidal slip promote forward propagation but have little effect on thickening. When two like embryos lie along the same GB, their paired interaction promotes forward propagation but hinders thickening.

36 MATERIALS SCIENCE↗
DOE OSTI2021

In Situ X-ray Measurements to Follow the Crystallization of BaTiO 3 Thin Films during RF-Magnetron Sputter Deposition

Here, we report on adding an important dimension to the fundamental understanding of the evolution of the thin film micro structure evolution. Thin films have gained broad attention in their applications for electro-optical devices, solar-cell technology, as well storage devices. Deep insights into fundamental functionalities can be realized via studying crystallization microstructure and formation processes of polycrystalline or epitaxial thin films. Besides the fundamental aspects, it is industrially important to minimize cost which intrinsically requires lower energy consumption at increasing performance which requires new approaches to thin film growth in general. Here, we present a state of the art sputtering technique that allows for time-resolved in situ studies of such thin film growth with a special focus on the crystallization via small angle scattering and X-ray diffraction. Focusing on the crystallization of the example material of BaTiO 3 , we demonstrate how a prototypical thin film forms and how detailed all phases of the structural evolution can be identified. The technique is shaped to enable a versatile approach for understanding and ultimately controlling a broad variety of growth processes, and more over it demonstrate how to in situ investigate the influence of single high temperature sputtering parameters on the film quality. It is shown that the whole evolution from nucleation, diffusion adsorption and grain growth to the crystallization can be observed during all stages of thin film growth as well as quantitatively as qualitatively. This can be used to optimize thin-film quality, efficiency and performance.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Atomistic Investigation of Plastic Deformation and Dislocation Motion in Uranium Mononitride

Uranium mononitride (UN) is a promising advanced nuclear fuel due to its high thermal conductivity and high fissile density. However, many aspects of its mechanical behavior, particularly at reactor-relevant conditions, remain unclear. In this study, molecular dynamics (MD) simulations were employed to investigate the deformation behavior and dislocation motion in UN. We found that the Kocevski potential predicts the principal slip system as $\frac{1}{2}$ $\langle110\rangle${110}, aligning with experimental data. On the other hand, the Tseplyaev potential predicts slip to primarily occur on $\frac{1}{2}$ $\langle110\rangle${111}. MD simulations of stress–strain behavior were used to estimate the nanoindentation hardness, revealing that the Kocevski potential accurately predicts hardness even though it fails to model dynamic plasticity. Complete dislocation mobility functions have been fitted for the edge and screw dislocations in both the thermally activated and phonon-drag regimes. The 300 K linear mobility of the edge dislocation using the Tseplyaev potential was found to be 817 Pa -1 ·s -1 , whereas that of the screw dislocation using the Kocevski potential was found to be 4546 Pa -1 ·s -1 . At intermediate stresses, we observed that the subsonic steady-state motion of the edge dislocation in UN is intermittently interrupted by velocity jumps, reaching the average sound velocity. Finally, the threshold Schmid stress is calculated as 179–197 MPa, which gives an upper-limit estimate of the uniaxial yield stress of polycrystalline UN of 548–603 MPa. These findings, including the fitted dislocation mobility function, provide essential input for future plasticity and dislocation dynamics models of nuclear fuels.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Comparison of Hafnium Dioxide and Zirconium Dioxide Grown by Plasma-Enhanced Atomic Layer Deposition for the Application of Electronic Materials

We report the growth of nanoscale hafnium dioxide (HfO 2 ) and zirconium dioxide (ZrO 2 ) thin films using remote plasma-enhanced atomic layer deposition (PE-ALD), and the fabrication of complementary metal-oxide semiconductor (CMOS) integrated circuits using the HfO 2 and ZrO 2 thin films as the gate oxide. Tetrakis (dimethylamino) hafnium (Hf[N(CH 3 ) 2 ] 4 ) and tetrakis (dimethylamino) zirconium (IV) (Zr[N(CH 3 ) 2 ] 4 ) were used as the precursors, while O 2 gas was used as the reactive gas. The PE-ALD-grown HfO 2 and ZrO 2 thin films were analyzed using X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and high-resolution transmission electron microscopy (HRTEM). The XPS measurements show that the ZrO 2 film has the atomic concentrations of 34% Zr, 2% C, and 64% O while the HfO 2 film has the atomic concentrations of 29% Hf, 11% C, and 60% O. The HRTEM and XRD measurements show both HfO 2 and ZrO 2 films have polycrystalline structures. n-channel and p-channel metal-oxide semiconductor field-effect transistors (nFETs and pFETs), CMOS inverters, and CMOS ring oscillators were fabricated to test the quality of the HfO 2 and ZrO 2 thin films as the gate oxide. Current-voltage (IV) curves, transfer characteristics, and oscillation waveforms were measured from the fabricated transistors, inverters, and oscillators, respectively. The experimental results measured from the HfO 2 and ZrO 2 thin films were compared.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2020

Crystallographic Orientation Dependence of Mechanical Responses of FeCrAl Micropillars

Iron-chromium-aluminum (FeCrAl) alloys are used in automobile exhaust gas purifying systems and nuclear reactors due to its superior high-temperature oxidation and excellent corrosion resistance. Single-phase FeCrAl alloys with a body centered cubic structure plastically deform through dislocation slips at room temperature. Here, we investigated the orientation dependence of mechanical responses of FeCrAl alloy through testing single-crystal and bi-crystal micropillars in a scanning electron microscopy at room temperature. Single-crystal micropillars were fabricated with specific orientations which favor the activity of single slip system or two slip systems or multiple slip systems. The strain hardening rate and flow strength increase with increasing the number of activated slip system in micropillars. Bi-crystal micropillars with respect to the continuity of slip systems across grain boundary were fabricated to study the effect of grain boundary on slip transmission. The high geometrical compatibility factor corresponds to a high flow strength and strain hardening rate. Experimental results provide insight into understanding mechanical response of FeCrAl alloy and developing the mechanisms-based constitutive laws for FeCrAl polycrystalline aggregates.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Nanocrystalline Materials: Synthesis, Characterization, Properties, and Applications

Nanostructuring is a commonly employed method of obtaining superior mechanical properties in metals and alloys. Compared to conventional polycrystalline counterparts, nanostructuring can provide remarkable improvements in yield strength, toughness, fatigue life, corrosion resistance, and hardness, which is attributed to the nano grain size. In this review paper, the current state-of-the-art of synthesis methods of nanocrystalline (NC) materials such as rapid solidification, chemical precipitation, chemical vapor deposition, and mechanical alloying, including high-energy ball milling (HEBM) and cryomilling was elucidated. More specifically, the effect of various process parameters on mechanical properties and microstructural features were explained for a broad range of engineering materials. This study also explains the mechanism of grain strengthening using the Hall-Petch relation and illustrates the effects of post-processing on the grain size and subsequently their properties. This review also reports the applications, challenges, and future scope for the NC materials.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Synthesis, Crystal and Electronic Structures, Nonlinear Optical Properties, and Magnetic Properties of Two Thiophosphates: KInP 2 S 7 and KCrP 2 S 7

Two thiophosphates, KInP 2 S 7 and KCrP 2 S 7 , were structurally characterized without investigating any optical properties. Herein in this work, KInP 2 S 7 and KCrP 2 S 7 were revisited to investigate their optical and magnetic properties, respectively. Pure polycrystalline samples and crystals of KInP 2 S 7 and KCrP 2 S 7 were grown by high temperature solid state reactions, where mm-sized crystals of KCrP 2 S 7 were collected. KCrP 2 S 7 is isostructural to KInP 2 S 7 , which features a layered structure. KInP 2 S 7 and KCrP 2 S 7 possess close relationship to the layered thiophosphate M 2 P 2 S 6 (M = Fe, Co, Zn, etc.). The bonding pictures of KInP 2 S 7 were studied using the electron localization function (ELF) coupled with crystal orbital Hamilton population (COHP) calculations. The intrinsically distorted [PS 4 ] tetrahedra and [InS 6 ] octahedra are made by strong covalent P-S interactions and ionic In-S interactions, respectively. Electronic structure analysis confirmed that the optical properties of KInP 2 S 7 are mainly contributed to by [PS 4 ] tetrahedra together with small amounts of the contributions coming from [InS 6 ] octahedra. Magnetic measurement on mm-sized crystals of KCrP 2 S 7 verified that there is an antiferromagnetic transition around 21 K, and the Cr atoms are trivalent. KInP 2 S 7 is predicated to be an indirect bandgap semiconductor of 2.38 eV, which is confirmed by the UV-Vis measurement of 2.4(1) eV. KInP 2 S 7 is not a type-I phase-matching material and exhibits moderate second harmonic generation (SHG) response (0.51 × AgGaS 2 , sample of particle size of 100 µm). The laser damage threshold (LDT) of KInP 2 S 7 is very high of 5.2 × AgGaS 2 . Bandgap engineering were undergone to enhance the SHG response of KInP 2 S 7 .

36 MATERIALS SCIENCE↗
DOE OSTI2023

Phase Transformation Pathway of DyPO4 to 21.5 GPa

Interest in the deformation behavior and phase transformations of rare earth orthophosphates (REPO4s) spans several fields of science—from geological impact analysis to ceramic matrix composite engineering. In this study, the phase behavior of polycrystalline, xenotime DyPO4 is studied up to 21.5(16) GPa at ambient temperature using in situ diamond anvil cell synchrotron X-ray diffraction. This experiment reveals a large xenotime–monazite phase coexistence pressure range of 7.6(15) GPa and evidence for the onset of a post-monazite transformation at 13.9(10) GPa to scheelite. The identification of scheelite as the post-monazite phase of DyPO4, though not definitive, is consistent with REPO4 phase transformation pathways reported in both the experimental and the computational literature.

Sharma, Jai (ORCID:0000000339034534)↗
DOE OSTI2023

Double-Layer Kagome Metals Pt 3 Tl 2 and Pt 3 In 2

The connectivity and inherent frustration of the kagome lattice can produce interesting electronic structures and behaviors in compounds containing this structural motif. Here we report the properties of Pt 3 X 2 (X = In and Tl) that adopt a double-layer kagome net structure related to that of the topologically nontrivial high-temperature ferromagnet Fe 3 Sn 2 and the density wave hosting compound V 3 Sb 2 . We examined the structural and physical properties of single crystal Pt 3 Tl 2 and polycrystalline Pt 3 In 2 using X-ray and neutron diffraction, magnetic susceptibility, heat capacity, and electrical transport measurements, along with density functional theory calculations of the electronic structure. Our calculations show that Fermi levels lie in pseudogaps in the densities of states with several bands contributing to transport, and this is consistent with our Hall effect, magnetic susceptibility, and heat capacity measurements. Although electronic dispersions, characteristic of simple kagome nets with nearest-neighbor hopping, are not clearly seen, likely due to the extended nature of the Pt 5d states, we do observe moderately large and non-saturating magnetoresistance values and quantum oscillations in the magnetoresistance and magnetization associated with the kagome nets of Pt.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Microscopic Characterization of Pb 10−x Cu x (PO 4 ) 6 O by 31 P and 63/65 Cu NMR Measurements

The report of the first room-temperature, ambient-pressure superconductivity in copper-doped lead apatite Pb 10−x Cu x (PO 4 ) 6 O has attracted lots of attention. However, subsequent studies revealed the presence of numerous impurity phases in the polycrystalline sample, and the sharp superconducting-like transition is not due to a superconducting transition but most likely due to a reduction in resistivity caused by the first-order structural phase transition of Cu 2 S at around 385 K from the β phase at high temperature to the γ phase at low temperature. Before now, only bulk measurements have been performed on a Pb 10−x Cu x (PO 4 ) 6 O powder sample, which could be affected by the impurity phases, masking the intrinsic properties of Pb 10−x Cu x (PO 4 ) 6 O. In this study, 31 P and 63/65 Cu nuclear magnetic resonance (NMR) measurements have been performed on a Pb 10−x Cu x (PO 4 ) 6 O powder sample to investigate its physical properties from a microscopic point of view. Our NMR data evidence the non-magnetic insulating nature of Pb 10−x Cu x (PO 4 ) 6 O without any trace of electron correlation effects. Furthermore, the 63/65 Cu NMR results suggest that no copper or very little copper is substituted for Pb in Pb 10 (PO 4 ) 6 O prepared by sintering Pb 2 SO 5 and Cu 3 P.

lead apatite↗
DOE OSTI2021

ZrN Phase Formation, Hardening and Nitrogen Diffusion Kinetics in Plasma Nitrided Zircaloy-4

Plasma nitridation was conducted to modify the surfaces of Zircaloy-4. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman analysis were used to characterize microstructures and phases. Surface indentation and cross-sectional indentation were performed to evaluate mechanical property changes. Nitridation forms a thin layer of ZrN phase, followed by a much deeper layer affected by nitrogen diffusion. The ZrN phase is confirmed by both TEM and Raman characterization. The Raman peaks of ZrN phase show a temperature dependence. The intensity increases with increasing nitridation temperatures, reaches a maximum at 700 °C, and then decreases at higher temperatures. The ZrN layer appears as continuous small columnar grains. The surface polycrystalline ZrN phase is harder than the bulk by a factor of ~8, and the nitrogen diffusion layer is harder by a factor of ~2–5. The activation energy of nitrogen diffusion was measured to be 2.88 eV. The thickness of the nitrogen-hardened layer is controllable by changing the nitridation temperature and duration.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Real-Time Observation of Nanoscale Kink Band Mediated Plasticity in Ion-Irradiated Graphite: An In Situ TEM Study

Graphite IG-110 is a synthetic polycrystalline material used as a neutron moderator in reactors. Graphite is inherently brittle and is known to exhibit a further increase in brittleness due to radiation damage at room temperature. To understand the irradiation effects on pre-existing defects and their overall influence on external load, micropillar compression tests were performed using in situ nanoindentation in the Transmission Electron Microscopy (TEM) for both pristine and ion-irradiated samples. While pristine specimens showed brittle and subsequent catastrophic failure, the 2.8 MeV Au2+ ion (fluence of 4.378 × 1014 cm−2) irradiated specimens sustained extensive plasticity at room temperature without failure. In situ TEM characterization showed nucleation of nanoscale kink band structures at numerous sites, where the localized plasticity appeared to close the defects and cracks while allowing large average strain. We propose that compressive mechanical stress due to dimensional change during ion irradiation transforms buckled basal layers in graphite into kink bands. The externally applied load during the micropillar tests proliferates the nucleation and motion of kink bands to accommodate the large plastic strain. The inherent non-uniformity of graphite microstructure promotes such strain localization, making kink bands the predominant mechanism behind unprecedented toughness in an otherwise brittle material.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Investigation of the Effect of Atmospheric Plasma Treatment in Nanofiber and Nanocomposite Membranes for Piezoelectric Applications

In this work, we report the effect of steady-state atmospheric plasma (Corona discharge) in nanofibers and nanocomposite membranes for piezoelectric applications. The investigation was performed in PVDF (Poly vinylidene fluoride) nanofibers, CNT (Carbon Nanotubes)-reinforced PVDF nanocomposites, and PAN (Poly acrylonitrile) nanofiber membranes. Steady-state plasma was generated with a high voltage power source with 1 mA discharge current output and 6 kV discharge voltage, and the gap between tip and the material was maintained to be 1 cm. For the fabrication of nanofibers and nanocomposite membranes, an electrospinning method was used. The electrospinning parameters, such as flow rate and voltage, were optimally tuned for obtaining uniform nanofibers and nanomembranes. Along with the plasma treatment, heat treatment above the glass transition temperature was also conducted on the nanofiber membranes. Using a Scanning Electron Microscope (SEM), the morphology of the nanofibers was observed. X-ray Diffraction (XRD) demonstrated the polycrystallinity of the nanofibers. Fourier Transform Infrared Spectroscopy (FTIR) analysis of the PVDF nanofibers shows a peak at 796 cm−1 representing α-phase (C-H rocking) in the control sample which is absent in the treated samples. Raman spectroscopy of PVDF nanofibers identifies a Raman shift from 873 cm−1 to 877 cm−1 (denoting β-phase) for plasma-treated samples only. Electron Paramagnetic Resonance (EPR) concludes that the intensity of the free radicals increases from 1.37 to 1.46 (a.u.) after plasma treatment. Then, sensors were fabricated from the PVDF nanofibers, MWCNT-reinforced PVDF nanofibers, and PAN nanofibers to characterize their piezoelectric properties. The impact test results showed that the atmospheric plasma and heat-treated samples had 86%, 277%, and 92% increases of the d33 value (piezoelectric coefficient) in the case of PVDF nanofibers, MWCNT-reinforced nanofibers, and PAN nanofibers, respectively. It was also observed that the capacitance of the nanofiber membranes has increased due to the plasma treatment.

Biochemistry & Molecular Biology↗
DOE OSTI2025

Sound Velocities in Vanadium Reveal Complex Elastic Behavior at High Pressures

Compressional (VP) and shear (VS) wave velocities of polycrystalline vanadium were measured simultaneously up to 11.5 GPa at room temperature using ultrasonic interferometry in a multi-anvil press. Complex softening behavior in VS and resulting shear moduli are discovered, possibly revealing a precursor to the reported phase transition within 30–60 GPa. The current data enables a comprehensive assessment of the elastic and mechanical properties of vanadium at high pressures, including bulk and shear moduli, Young’s modulus, Poisson’s ratio, and Pugh’s ratio. Through fitting to the 3rd-order finite strain equations, the elastic moduli and their pressure derivatives were determined to be K S0 = 151 (2) GPa, G 0 = 46.9 (8) GPa, K$^{’}_{S0}$ = 3.47 (5), and G$^{’}_{0}$ = 0.62 (1). These experimental results allow us to compare with and benchmark the existing Steinberg–Guinan models for extrapolations to extreme pressure and temperature conditions.

36 MATERIALS SCIENCE↗
DOE OSTI2020

X-ray Laue Microdiffraction and Raman Spectroscopic Investigation of Natural Silicon and Moissanite

Moissanite, SiC, is an uncommon accessory mineral that forms under low oxygen fugacity. Here, we analyze natural SiC from a Miocene tuff-sandstone using synchrotron Laue microdiffraction and Raman spectroscopy, in order to better understand the SiC phases and formation physics. The studied crystals of SiC consist of 4H- and 6H-SiC domains, formed from either, continuous growth or, in one case, intergrown, together with native Si. The native Si is polycrystalline, with a large crystal size relative to the analytical beam dimensions (>1–2 μm). We find that the intergrown region shows low distortion or dislocation density in SiC, but these features are comparatively high in Si. The distortion/deformation observed in Si may have been caused by a mismatch in the coefficients of thermal expansion of the two materials. Raman spectroscopic measurements are discussed in combination with our Laue microdiffraction results. Our results suggest that these SiC grains likely grew from an igneous melt.

58 GEOSCIENCES↗