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At least 649 records · Page 36
All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Superconducting NbTiN thin films for superconducting radio frequency accelerator cavity applications

Current superconducting radio frequency technology, used in various particle accelerator facilities across the world, is reliant upon bulk niobium superconducting cavities. Due to technological advancements in the processing of bulk Nb cavities, the facilities have reached accelerating fields very close to a material-dependent limit, which is close to 50 MV/m for bulk Nb. One possible solution to improve upon this fundamental limitation was proposed a few years ago by Gurevich [Appl. Phys. Lett. 88, 012511 (2006)], consisting of the deposition of alternating thin layers of superconducting and insulating materials on the interior surface of the cavities. The use of type-II superconductors with Tc > Tc Nb and H c > HcNb, (e.g., Nb 3 Sn, NbN, or NbTiN) could potentially greatly reduce the surface resistance (Rs) and enhance the accelerating field, if the onset of vortex penetration is increased above Hc Nb , thus enabling higher field gradients. Although Nb 3 Sn may prove superior, it is not clear that it can be grown as a suitable thin film for the proposed multilayer approach, since very high temperature is typically required for its growth, hindering achieving smooth interfaces and/or surfaces. On the other hand, since NbTiN has a smaller lower critical field (H c1 ) and higher critical temperature (T c ) than Nb and increased conductivity compared to NbN, it is a promising candidate material for this new scheme. Here, the authors present experimental results correlating filmmicrostructure with superconducting properties on NbTiN thin film coupon samples while also comparing filmsgrown with targets of different stoichiometry. In conclusion, it is worth mentioning that the authors have achieved thin films with bulk-like lattice parameter and transition temperature while also achieving H c1 values larger than bulk for films thinner than their London penetration depths.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Meso-scale magnetic signatures for nuclear reactor steel irradiation embrittlement monitoring

Verifying the structural integrity of passive components in light water and advanced reactors will be necessary to ensure safe, long-term operations of the existing U.S. nuclear fleet. This objective can be achieved through nondestructive condition monitoring techniques, which can be integrated with plant operations to quantify the “state of health” of structural materials in real-time. While nondestructive methods for monitoring many classes of degradation (such as fatigue or stress corrosion cracking) are relatively advanced, this is not the case for degradation caused by irradiation. The development of nondestructive evaluation technologies for these types of degradation will require advanced materials characterization techniques and tools that enable comprehensive understanding of nuclear reactor material microstructural and behavioral changes under extreme operating environments. Irradiation-induced degradation of reactor steels causes changes in their microstructure that impacts their micro-magnetic properties. In this paper, we describe preliminary results of integrating advanced material characterization techniques with meso-scale computational models. In the future, this will help to provide an interpretive understanding of the state of degradation in structural materials. Microstructural data are presented from monocrystalline Fe and are correlated with variable-field magnetic force microscopy and micro-magnetic measurements. Ongoing research is focused on extending the measurements and models on thin films to gain insights into the structural state of irradiated materials and the resulting impact on magnetic properties. Preliminary conclusions from these correlations are presented, and next steps described.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2015

Annealing effect on the magnetic induced austenite transformation in polycrystalline freestanding Ni-Co-Mn-In films produced by co-sputtering

Ni-Co-Mn-In freestanding films, with a magneto-structural transformation at room temperature were successfully produced by co-sputtering and post-annealing methods leading to film composition mastering. For a post-annealing temperature of 700 °C, the phase transformation occurs slightly above room temperature, with a twisted martensitic microstructure phase observed at 300 K by Field Emission Scanning Electron Microscopy. Magnetization measurements on a polycrystalline film showed a phase transformation from a weakly magnetic martensite to a magnetic austenite phase. Moreover, an inverse magnetocaloric effect with an entropy variation of 4 J/kg K under 5 T was also measured. A simple magneto-actuation experiment based on the magnetic induced austenite transformation was also successfully completed. The possibility to insert such films in microsystems is clearly demonstrated in this work.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Corrosion properties of phase reversion induced nano/ultrafine grained AISI 304 metastable austenite stainless steel

Highlights: • AISI 304 stainless steel was cold rolled under 3 cryogenic temperatures and room temperature, after annealing bulk nano/ultrafine grained material was obtained. • Microstructure of samples was studied by TEM, −120 °C rolled sample had an equiaxed microstructure. • Corrosion resistance of samples was studied by polarization curve, EIS, and Mott-Schottky plot, −120 °C rolled sample had the best corrosion performance. • The distinctive polarization curve of −120 °C rolled sample indicated its passive film had peculiar feature, the M-S plot showed its abnormal semiconductor character. - Abstract: AISI 304 metastable austenite stainless steel was cold rolled under cryogenic temperature and transformed into martensite completely, after reverse transformation by annealing, bulk nano/ultrafine grained material was obtained. The material’s microstructure was observed by TEM, and the corrosion resistance was studied by polarization curve, EIS, and Mott-Schottky plot. Results showed that samples cold rolled at −120 °C had an equiaxed microstructure and displayed the best corrosion performance. The distinctive polarization curve shape indicated that its passive film had a peculiar feature, and the M-S plot showed its abnormal semiconductor character. XPS measurements are used to directly characterize the composition of passive film formed on specimens. Heterogeneous microstructures might help with the improvement on corrosion resistance of the nano/ultrafine grained stainless steel.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Sandy Soil Microaggregates: Rethinking Our Understanding of Hydraulic Function

Core Ideas Sandy soil microaggregates are comprised of a solid sand core encrusted with fines. Thick films control a significant proportion of water retention in coarse sandy soil. Three water pools drain sequentially: capillary water, thick films, and adsorptive films. Film seepage rates should be considered when irrigating sandy soil. This study investigated the peculiar structure of microaggregates in coarse sandy soils that exhibit only external porosity and investigated their control on soil hydrology. The microstructure underpins a hydrologic existence that differs from finer textured soils where aggregates have internal porosity. Understanding the impact of these microaggregates on soil hydrology will permit improved agricultural irrigation management and estimates associated with ecosystem capacity and resiliency. Microstructure was investigated using a digital microscope, and aspects of the structure were quantified by sedimentation and computed microtomography. Sandy soil microaggregates were observed to be comprised of a solid sand‐grain core that is coated with fines, presumably cemented by organic media. This microstructure leads to three distinct water pools during drainage: capillary water, followed by thick films (1–20 μm) enveloping the outer surfaces of the crusted microaggregates, followed by adsorbed thin films (<1 μm). The characteristics of the thick films were investigated using an analytical model. These films may provide as much as 10 to 40% saturation in the range of plant‐available water. Using lubrication theory, it was predicted that thick film drainage follows a power law function with an exponent of 2. Thick films may also have a role in the geochemical evolution of soils and in ecosystem function because they provide contiguous water and gas phases at relatively high moisture contents. And, because the rough outer crust of these microaggregates can provide good niches for microbial activity, biofilm physics will dominate thick film processes, and consequently hydrologic, biologic, and geochemical functions for coarse sandy soils.

Paradiś, Ashley↗
DOE OSTI2020

Combinatorial Exploration and Mapping of Phase Transformation in a Ni–Ti–Co Thin Film Library

Combinatorial synthesis and high-throughput characterization of a Ni–Ti–Co thin film materials library are reported for exploration of reversible martensitic transformation. The library was prepared by magnetron co-sputtering, annealed in vacuum at 500 °C without atmospheric exposure, and evaluated for shape memory behavior as an indicator of transformation. Composition, structure, and transformation behavior of the 177 pads in the library were characterized using high-throughput wavelength dispersive spectroscopy (WDS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and four-point probe temperature-dependent resistance (R(T)) measurements. A new, expanded composition space having phase transformation with low thermal hysteresis and Co > 10 at. % is found. Unsupervised machine learning methods of hierarchical clustering were employed to streamline data processing of the large XRD and XPS data sets. Through cluster analysis of XRD data, we identified and mapped the constituent structural phases. Finally, composition–structure–property maps for the ternary system are made to correlate the functional properties to the local microstructure and composition of the Ni–Ti–Co thin film library.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Electron emission of Au nanoparticles embedded in ZnO for highly conductive oxide

We investigated the effect of embedded Au nanoparticles (Au NPs) on electrical properties of zinc oxide (ZnO) for highly conductive oxide semiconductor. Au NPs in ZnO films influenced both the structural and electrical properties of the mixture films. The electrical resistivity decreases by as much as five orders of magnitude. This is explained by the electron emission from Au NPs to the ZnO matrix. Temperature-dependent Hall effect measurements show that an electron emission mechanism changes from tunneling to thermionic emission at T = 180 K. The electron mobility in the mixture film is mainly limited by the grain boundaries at lower temperature (80-180 K), and the Au/ZnO heterogeneous interface at higher temperature (180-340 K). In addition to the electron emission, embedded Au NPs alter the ZnO matrix microstructure and improve the electron mobility. Compared to the undoped ZnO film, the carrier concentration of the Au NP-embedded ZnO film can be increased by as much as six orders of magnitude with a small change in the carrier mobility. This result suggests a way to circumvent the inherent tradeoff between the carrier concentration and the carrier mobility in transparent conductive oxide (TCO) materials.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Tungsten Incorporation into Gallium Oxide: Crystal Structure, Surface and Interface Chemistry, Thermal Stability and Interdiffusion

Tungsten (W) incorporated gallium oxide (Ga2O3) (GWO) thin films were deposited by radio-frequency magnetron co-sputtering of W-metal and Ga2O3-ceramic targets. Films were produced by varying sputtering power applied to the W-target in order to achieve variable W-content (0-12 at%) into Ga2O3 while substrate temperature was kept constant at 500 °C. Chemical composition, chemical valence states, microstructure and crystal structure of as-deposited and annealed GWO films were evaluated as a function of W-content. The structural and chemical analyses indicate that the samples deposited without any W-incorporation are stoichiometric, nanocrystalline Ga2O3 films, which crystallize in β-phase monoclinic structure. While GWO films also crystallize in monoclinic β-Ga2O3 phase, W-incorporation induces surface amorphization as revealed by structural studies. The chemical valence state of Ga ions probed by X-ray photoelectron spectroscopic (XPS) analyses is characterized by the highest oxidation state i.e., Ga3+. No changes in Ga chemical state are noted for variable W-incorporation in the range of 0-12 at%. Rutherford backscattering spectrometry (RBS) analyses indicate the uniform distribution of W-content in the GWO films. However, XPS analyses indicate the formation of mixed valence states for W ions, which may be responsible for surface amorphization in GWO films. GWO films were stable up to 900 oC, at which point thermally induced secondary phase (W-oxide) formation was observed. A transition to mesoporous structure coupled with W interdiffusion occurs due to thermal annealing as derived from the chemical analyses at the GWO films’ surface as well as depth-profiling towards the GWO-Si interface. A model has been formulated to account for the mechanism of W-incorporation, thermal stability and interdiffusion via pore formation in GWO films.

Chemical composition↗
DOE OSTI2018

Ensuring combination of strength, ductility and toughness in medium-manganese steel through optimization of nano-scale metastable austenite

Highlights: • Medium-Mn steel was innovatively designed for medium to heavy steel plates. • Three intercritical annealing processes were adopted to ensure TRIP effect. • Austenite-martensite submicro-laminate structure was obtained after annealing. • The reversed austenite with different stability led to improved ductility. • TRIP effect induced by metastable austenite contributed excellent impact properties. - Abstract: Medium-Mn steel was innovatively designed in terms of alloying elements for medium to heavy steel plates to obtain combination of high strength, good ductility, and excellent low temperature toughness. Martensite was the dominant microstructure in the directly quenched steel plate because of high hardenability obtained by the addition of 5.6 wt% Mn. Three intercritical annealing processes were adopted to ensure transformation-induced-plasticity (TRIP) effect through optimization of the volume fraction, morphology, and C and Mn-enriched reversed austenite. On annealing, the dislocation density of martensite plate was decreased because of recovery and recrystallization, and metastable austenite film nucleated at the interface. Both thermal and mechanical stability of austenite decreased with increase in annealing temperature. The high yield strength of 840 MPa, good elongation after fracture of 24.3%, and excellent toughness at − 60 °C of 130.3 J was obtained at intermediate annealing temperature of 650 °C, and the volume fraction of reversed austenite at room temperature and − 80 °C was 22% and 17%, respectively. The reversed austenite exhibited different stability with increased tensile strain, leading to improved ductility and delayed necking. Moreover, the crack initiation energy and crack propagation energy were increased via dynamic stress partitioning and relaxation together with the transformation of metastable austenite. Thus, significant degree of TRIP effect induced by moderate stability of austenite played an important role in governing mechanical properties.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2019

Fundamental Relationship of Microstructure and Ionic Conductivity of Amorphous LLTO as Solid Electrolyte Material

All-solid-state Li-ion batteries (ASSLiB) attracted lots of attention mainly due to their higher safety compared with commercial Li-ion batteries. The research of solid electrolyte is critical for the development of ASSLiB, and among all the candidates of solid electrolyte materials, amorphous Lithium Lanthanum Titanate Oxide (LLTO) is promising because of its outstanding electrochemical stability up to 12V. However, the fundamental relationship among the ionic conductivity, microstructure, and mechanism of Li ion transport is still unrevealed. In this study, both amorphous LLTO thin film and LLTO powder were successfully prepared by sol-gel process. In order to determine the relationship between microstructure and ionic conductivity, various annealing time at 500°C were applied. This work shows that the ionic conductivity increases from 2.32 × 10 -8 S/cm to 9.01 × 10 -6 S/cm with the annealing time before LLTO starts to crystallize and decreases back to ~1.6 × 10 -9 S/cm after the formation of crystal phase. The absolute value of difference is close to 3 orders of magnitude. Furthermore, the morphology of the thin film changes accordingly, solvent evaporation, surface refinement and crystallization phases would occur sequentially, and this indicates that there is an optimal synthesis condition for the LLTO film. However, the changes of structure, morphology and ionic conductivity does not affect activation energy. This will help researchers to find optimized synthesis condition of amorphous LLTO and potentially search for and design other solid electrolyte materials.

25 ENERGY STORAGE↗
DOE OSTI2018

Facile synthesis and photocatalytic activity of La-doped BiOCl hierarchical, flower-like nano-/micro-structures

Highlights: • Novel La-doped BiOCl flower-like hierarchical films. • Greatly enhanced photocatalytic degradation effect on dyes. • Specific growth mechanism was proposed. • Photocatalysis mechanism was proposed. - Abstract: A series of La-doped BiOCl hierarchical, flower-like nano-/micro-structures (NMFs) with ginkgo-leaf-like “petals” were prepared by etching La-doped Bi{sub 2}O{sub 3} films in HCl solution at room temperature. For the La-doped Bi{sub 2}O{sub 3} films, they were fabricated through hot-dipping Bi{sub 2}O{sub 3} thin films in La{sub 2}O{sub 3} powder at 650 °C. Microstructure examination revealed that the ginkgo-leaf-like La-doped BiOCl petals have a multilayered structure consisting of several ultra-thin nanosheets with different radii due to the external-to-internal etching process. The investigation on their formation mechanism revealed that the La-doped BiOCl hierarchical NMFs grew anisotropically through Ostwald ripening mechanism. Besides, the photodegradation of rhodamine B under simulated sunlight irradiation revealed that the La-doped BiOCl hierarchical NMFs possessed higher performance than pure BiOCl sample. And the active species trapping tests indicated that the photogenerated holes were the main active radicals for the degradation of rhodamine B.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Effect of Minor Er on the Microstructure and Properties of Al-6.0Mg-0.4Mn-0.1Cr-0.1Zr Alloys

As-cast Al-6.0Mg-0.4Mn-0.1Cr-0.1Zr alloys containing different additions of Er were prepared. Then, the specimens were carried out homogenization heat treatment, hot rolling, cold rolling, and annealing. The effects of minor Er on the microstructure and properties of Al-6.0Mg-0.4Mn-0.1Cr-0.1Zr alloy were investigated. Results show that addition of Er can refine the microstructure and improve the mechanical properties of the alloys. As for the annealed alloys, the addition of 0.33%Er can increase the tensile strength by 29 MPa. Strength increment is mainly attributed to refinement and the precipitation of Al{sub 3}Er and Al{sub 3}(Er, Zr). Additionally, the minor Er can improve the corrosion resistance of the alloys, which can be attributed to the compact composite oxide film of Er-O and Al-O, purification, and modification.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Controlling Solvate Intermediate Growth for Phase-Pure Organic Lead Iodide Ruddlesden–Popper (C 4 H 9 NH 3 ) 2 (CH 3 NH 3 ) n -1 Pb n I 3 n +1 Perovskite Thin Films

The growth of Ruddlesden-Popper perovskite thin films is complicated by the existence of multiple crystallization pathways available to precursors in solution. During conventional thin film growth processes, such as spin-coating or blade-coating, solvents can evaporate too quickly to clearly resolve different reaction intermediates and products that form during crystallization. Here, we resolve multiple reaction products and intermediates that form during Ruddlesden-Popper phase growth by studying drop-cast precursor solutions in situ through the evolution of X-ray diffraction, photoluminescence, and optical micrographs over long timescales in a thin film geometry. We found that methylammonium-rich solvate intermediates play a crucial role in directing the bulk optical properties of the films, and form simultaneously with smaller regions of Ruddlesden-Popper phases during growth. The microstructure and optical properties of these sub-phases were characterized during growth and after annealing, revealing that discrepancies between thin film and single-crystal optical properties originate from solvate intermediates. These lower band-gap solvate-mediated minority phases dominate the optical emission spectrum by means of rapid energy migration, and contribute to sub-band-gap electronic states in photovoltaic devices. Processing routes to yield thin films with optical properties similar to single crystals of Ruddlesden-Popper phases were developed by tuning the precursor stoichiometry and deposition kinetics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Enhanced magnetism in lightly doped manganite heterostructures: strain or stoichiometry?

Lattice mismatch induced epitaxial strain has been widely used to tune functional properties in complex oxide heterostructures. Apart from the epitaxial strain, a large lattice mismatch also produces other effects including modulations in microstructure and stoichiometry. However, it is challenging to distinguish the impact of these effects from the strain contribution to thin film properties. Here, we use La 0.9 Sr 0.1 MnO 3 (LSMO), a lightly doped manganite close to the vertical phase boundary, as a model system to demonstrate that both epitaxial strain and cation stoichiometry induced by strain relaxation contribute to functionality tuning. The thinner LSMO films are metallic with a greatly enhanced T C which is 97 K higher than the bulk value. Such anomalies in T C and transport cannot be fully explained by the epitaxial strain alone. Detailed microstructure analysis indicates La deficiency in thinner films and twin domains formation in thicker films. Our results have revealed that both epitaxial strain and strain relaxation induced stoichiometry/microstructure modulations contribute to the modified functional properties in lightly doped manganite perovskite thin films.

36 MATERIALS SCIENCE↗
NASA NTRS1951

A Specially Constructed Metallograph for Use at Elevated Temperatures

A Metallographic microscope was developed with provision for heating a specimen to 1800 F in protective atmospheres, that is, vacuum or gas. A special objective was constructed of reflecting elements with an unusually long working distance (7/16 in.) and a high numerical aperture (0.5). Changes in specimen microstructure were observed and recorded on 35-millimeter motion-picture film. The resulting pictures were projected as motion pictures and individual frames were cut and enlargements made for close observation. Structural changes upon heating a 0.35-percent annealed carbon steel and a 5-percent tin phosphor bronze specimen were observed and recorded. Newly formed microstructure were revealed by selective vacuum etching and specimen relief resulting from recrystallization and varying grain orientation.

INSTRUMENTS, LABORATORY↗
DOE OSTI2021

Microstructure and heteroatom dictate the doping mechanism and thermoelectric properties of poly(alkyl-chalcogenophenes)

Heteroatom substitution can favorably alter electronic transport in conductive polymers to improve their thermoelectric performance. Here we report the spectroscopic, structural, and thermoelectric properties of poly(3–(3',7'-dimethyloctyl) chalcogenophenes) or P3RX doped with 2,3,5,6-tetrafluoro-7,7,8,8-tetracyanoquinodimethane (F4TCNQ), where the heteroatom [X = thiophene (T), selenophene (Se), tellurophene (Te)], the doping methodology, and extent of doping are systematically varied. Spectroscopic measurements reveal that while all P3RX polymers are appreciably doped, the doping mechanism is inherently different. Poly(3-hexylthiophene) (P3HT, used as a control) and poly(3–(3',7'-dimethyloctyl)tellurophene) (P3RTe) are doped primarily via integer charge transfer (ICT), whereas poly(3–(3',7'-dimethyloctyl)selenophene) (P3RSe) and poly(3–(3',7'-dimethyloctyl)thiophene) (P3RT) are doped via charge transfer complex (CTC) mechanisms. Despite these differences, all polymers saturate with roughly the same number of F4TCNQ counterions (1 dopant per 4 to 6 heterocycles), reinforcing the idea that the extent of charge transfer varies with the doping mechanism. Grazing incidence wide-angle x-ray scattering measurements provide insight into the structural driving forces behind different doping mechanisms—P3RT and P3RSe have similar microstructures in which F4TCNQ intercalates between the π-stacked backbones resulting in CTC doping (localized carriers), while P3HT and P3RTe have microstructures in which F4TCNQ intercalates in the alkyl side chain region, giving rise to ICT doping (delocalized carriers). These structural and spectroscopic observations shed light on why P3HT and P3RTe obtain electrical conductivities ca. 3 S/cm, while P3RT and P3RSe have conductivities <10–3 S/cm under the same thin film processing conditions. Ultimately, this work quantifies the effects of heteroatom, microstructural ordering, extent of doping, and doping mechanism, thereby providing rational guidance for designing future thermoelectric polymer-dopant systems.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Charge storage and tunneling mechanism of Ni nanocrystals embedded HfO{sub x} film

A nano-floating gate memory structure based on Ni nanocrystals (NCs) embedded HfO{sub x} film is deposited by means of radio-frequency magnetron sputtering. Microstructure investigations reveal that self-organized Ni-NCs with diameters of 4-8 nm are well dispersed in amorphous HfO{sub x} matrix. Pt/Ni-NCs embedded HfO{sub x}/Si/Ag capacitor structures exhibit voltage-dependent capacitance-voltage hysteresis, and a maximum flat-band voltage shift of 1.5 V, corresponding to a charge storage density of 6.0 × 10{sup 12} electrons/cm{sup 2}, is achieved. These capacitor memory cells exhibit good endurance characteristic up to 4 × 10{sup 4} cycles and excellent retention performance of 10{sup 5} s, fulfilling the requirements of next generation non-volatile memory devices. Schottky tunneling is proven to be responsible for electrons tunneling in these capacitors.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2024

Extending the Takagi-Taupin equations for x-ray nanobeam Bragg coherent diffraction

We present an approach for simulating x-ray nanobeam Bragg coherent diffraction patterns based on the Takagi-Taupin equations. Compared to conventional methods, the current approach can be universally applied to any weakly strained system including semi-infinite crystals that diffract dynamically. It addresses issues such as the curved wave front and redivergence of the focused incident beam. In conclusion, we show excellent agreement with experimental data for a strained La 0.7 ⁢Sr 0.3⁢ MnO 3 thin film on a SrTiO 3 substrate and a path to extracting physical information using automatic differentiation.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗