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At least 631 records · Page 35
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Twinned nanostructure of VO 2 thin films grown on r-cut sapphire

Due to strong electron-phonon interactions, strain engineering is a powerful tool to control quantum critical phenomena in strongly correlated oxides. Exploring this possibility requires understanding the nanoscale structure of quantum materials and the role it plays in forming the strain landscape. In this work, we used a combination of x-ray nanoimaging and reciprocal space mapping to study the nanostructure of the archetypal Mott insulator VO 2 featuring an insulator-to-metal and structural phase transitions. We found that VO 2 thin films grown on r-cut sapphire consist of two intertwined crystal lattices, permanently inclined with respect to each other. This persistent pattern of twin domains stands out from the symmetry breaking induced by the structural phase transition and conceivably originates from the post-growth strain relaxation process. We propose a model explaining the formation of twin domains and the emergence of anisotropy in the film nanostructure. Our work suggests using miscut substrates to suppress either one or the other twin that can serve as a new tool to control strain in VO 2 films.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Oxygen vacancy induced photoluminescence and ferromagnetism in SrTiO{sub 3} thin films by molecular beam epitaxy

SrTiO{sub 3} thin films were epitaxially grown on (100) SrTiO{sub 3} substrates using molecular beam epitaxy. The temperature for growth of the films was optimized, which was indicated by x-ray diffraction and further confirmed by microstructural characterization. Photoluminescence spectra show that oxygen-vacancy contributes to red and blue luminescence of oxygen-deficient post-annealed films, and a red shift was observed in blue region. On the other hand, ferromagnetism in film form SrTiO{sub 3} was observed from 5 K to 400 K and could be further enhanced with decreasing oxygen plasma partial pressure in annealing processes, which might be explained by the theory involving d{sup 0} magnetism related to oxygen-vacancy. From the cooperative investigations of optical and magnetic properties, we conclude that intrinsic defects, especially oxygen-vacancy, can induce and enhance luminescence and magnetism in SrTiO{sub 3} films.

36 MATERIALS SCIENCE↗
DOE OSTI2024

ZnO-Au Hybrid Metamaterial Thin Films with Tunable Optical Properties

ZnO-Au nanocomposite thin films have been previously reported as hybrid metamaterials with unique optical properties such as plasmonic resonance properties and hyperbolic behaviors. In this study, Au composition in the ZnO-Au nanocomposites has been effectively tuned by target composition variation and thus resulted in microstructure and optical property tuning. Specifically, all the ZnO-Au nanocomposite thin films grown through the pulsed laser deposition (PLD) method show obvious vertically aligned nanocomposite (VAN) structure with the Au nanopillars embedded in the ZnO matrix. Moreover, the average diameter of Au nanopillars increases as Au concentration increases, which also leads to the redshifts in the surface plasmon resonance (SPR) wavelength and changes in the hyperbolic behaviors of the films. As a whole, this work discusses how strain-driven tuning of optical properties and microstructure resulted through a novel Au concentration variation approach which has not been previously attempted in the ZnO-Au thin film system. These highly ordered films present great promise in the areas of sensing, waveguides, and nanophotonics to name a few.

Bhatt, Nirali A.↗
DOE OSTI2014

Mono-textured nanocrystalline thin films with pronounced stress-gradients: On the role of grain boundaries in the stress evolution

The origins of residual stress gradients in nanocrystalline thin films, especially the role of grain size and texture gradients, are still not fully understood. In this work, the stress evolution in exemplary nanocrystalline TiN thin films with one and two fiber texture components as well as in homogeneous amorphous SiO{sub x} films is analyzed using wafer curvature as well as laboratory and synchrotron cross-sectional nanobeam X-ray diffraction techniques. The stress evolution across the film thickness is attributed to the evolutionary nature of microstructural development at the individual growth stages. While the effect of the smooth crystallographic texture changes during growth is only of minor importance, as this does not significantly affect the dominant stress formation mechanisms, the change in the grain size accompanied by a change of the volume fraction of grain boundaries plays a decisive role in the stress development across the film thickness. This is demonstrated on the monotextured thin films, where the residual stresses scale with the apparent grain size. These findings are validated also by the investigations of stress profiles in homogeneous amorphous SiO{sub x} films exhibiting no grain boundaries.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Film Growth Dynamics During Pulsed Sputter Deposition (LDRD Final Report)

Novel materials synthesis and development using physical vapor deposition require our fundamental understanding of plasma conditions and film growth dynamics. A central theme is to control materials microstructure. Over the last few decades, the difficulty of thick heavy metal coatings has been one of the major bottlenecks limiting our studies of the important family of inertial-confinement-fusion (ICF) designs with colliding-shell targets. Our previous attempts to fabricate such coatings by conventional DC magnetron sputtering (DCMS) has had limited success due to the inherent complexity and our limited understanding of the deposition process. In this project, we have investigated the physics of a novel and promising pulsed sputter deposition process. We expanded the scientific foundation of sputter deposition processes through a combination of well-posed experiments and state-of-the-art characterizations. The following important scientific milestones have been achieved: (1) Successfully installed and tested a high-power impulse magnetron sputtering (HiPIMS) system; (2) Deployed a novel set of in-situ diagnostics during pulsed deposition, including a multibeam optical stress sensor (MOSS) system for real-time stress measurement, and Langmuir probe for the measurements of plasma physical properties. This allows us to monitor dynamically plasma conditions, ion flux and energy distributions, and film stress; (3) Investigated and obtained a fundamental understanding of HIPIMS on microstructure and stress control; (4) Successfully synthesized and demonstrated record-breaking strength nanocrystalline-nanotwinned (nnt) metals; (5) Successfully obtained high-quality, leak-proof Cr metal shells via HiPIMS method. The outcomes of this project could have transformational scientific and programmatic impacts, enabling novel materials synthesis and an experimental campaign with colliding shell target designs. The basic understanding of the deposition process has important implications to a broad range of industrial applications.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Enhancing Modulation of Thermal Conduction in Vanadium Dioxide Thin Film by Nanostructured Nanogaps

Efficient thermal management at the nanoscale is important for reducing energy consumption and dissipation in electronic devices, lab-on-a-chip platforms and energy harvest/conversion systems. For many of these applications, it is much desired to have a solid-state structure that reversibly switches thermal conduction with high ON/OFF ratios and at high speed. We describe design and implementation of a novel, all-solid-state thermal switching device by nanostructured phase transformation, i.e., modulation of contact pressure an d area between two poly-silicon surfaces activated by microstructural change of a vanadium dioxide (VO 2 ) thin film. Our solid-state devices demonstrate large and reversible alteration of cross-plane thermal conductance as a function of temperature, achieving a conductance ratio of at least 2.5. This new approach using nanostructured phase transformation provides new opportunities for applications that require advanced temperature and heat regulations.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Evaluation of the Mechanical Properties of Naturally Grown Multilayered Oxides Formed on HCM12A Using Small Scale Mechanical Testing

The microstructure and mechanical integrity of protective multilayered oxide films grown in liquid metal on F/M steel HCM12A was investigated utilizing Raman spectroscopy, nanoindentation and micro-cantilever testing methods. Here, the Raman spectra showed a Fe3O4 outer layer and a Cr-rich spinel structure inner layer. The nanoindentation results showed a higher hardness value for the inner layer than for the outer layer. In addition, the hardness of the diffusion layer in between the inner layer and the bulk steel was measured. Quantitative fracture properties were obtained of the steel/oxide interface and within the oxide layers utilizing microcantilever testing. Furthermore the strength and elastic properties of the multilayered oxide film were measured and it was found that the porous structure in the inner Fe–Cr oxide limits the integrity of the steel/oxide interface.

14 SOLAR ENERGY↗
DOE OSTI2014

Enhancement of the photocatalytic property of TiO{sub 2} columnar nanostructured films by changing deposition angle

Highlights: • Isolated and inclined columnar TiO{sub 2} nanostructures were obtained by sputtering Ti, and subsequently annealing. • The film performed photocatalytic decolorization effectively under UV irradiation. • The photocatalytic efficiency increased with deposition angle, which results in a more porous micro structure of the films. - Abstract: Isolated and inclined columnar nanostructured TiO{sub 2} films were obtained by sputtering titanium with glancing angle deposition method and subsequently annealing in air. Compared with flat film, TiO{sub 2} film fabricated with this method has higher porosity; compared with TiO{sub 2} powder, it overcomes the obstacles of immobilization and recycling. The TiO{sub 2} photocatalysis was evaluated by the degradation of methyl orange under UV light. It was indicated that the photocatalytic performance increased with deposition angle, which changed the porosity of the films. The relationship between deposition angle (the angle between the target and substrate surface) and the TiO{sub 2} columnar inclination angle (the angle between TiO{sub 2} columnar and substrate normal) was discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Numerical analysis of micro-/nanoscale gas-film lubrication of sliding surface with complicated structure

It has been reported that the friction between a partially polished diamond-coated surface and a metal surface was drastically reduced to zero when they are slid at a few m/s. Since the sliding was noiseless, it seems that the diamond-coated surface was levitated over the counter surface and the sliding mechanism was the gas film lubrication. Recently, the mechanism of levitation of a slider with a micro/nanoscale surface structure on a rotating disk was theoretically clarified [S. Yonemura et al., Tribol. Lett., (2014), doi:10.1007/s11249-014-0368-2]. Probably, the partially polished diamond-coated surface may be levitated by high gas pressure generated by the micro/nanoscale surface structure on it. In this study, in order to verify our deduction, we performed numerical simulations of sliding of partially polished diamond-coated surface by reproducing its complicated surface structure using the data measured by an atomic force microscope (AFM). As a result, we obtained the lift force which is large enough to levitate the slider used in the experiment.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

Structural and magnetic properties of (111) oriented annealed ultrathin Co/Pt multilayers

The effect of annealing on the structural and magnetic properties of Co/Pt multilayers was studied as a function of annealing temperature. The ultrathin layers of Pt and Co were deposited to make [Pt 1nm/Co 1nm]{sub x20} multilayer on Si (100) substrate using MBE technique. The structural, magnetic and electronic properties were recorded using XRD, SQUID and XPS techniques, respectively. M-H loop of as deposited sample shows soft magnetic nature with coercivity value of 350 Oe which increases to 974 Oe in 500°C annealed film. When studied at low temperature (5 K), the coercivity of 592 Oe is obtained in the as deposited sample which increases to 1626 Oe after annealing. In addition, as revealed by X-ray photoelectron spectroscopy, modifications in core level and valance band are observed. The observed changes in magnetic and electronic properties are attributed to structural modifications in correlation with the changes in (111) orientation of the films seen by X-ray diffraction.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2026

Mechanical and Microstructural Study of Neutron-Irradiated Novel Alloy Systems

Generation IV nuclear reactors require structural materials capable of withstanding high temperatures, corrosion, and radiation damage. Refractory high entropy alloys (RHEAs) show potential due to their resistance to irradiation damage, reduced void swelling, and microstructural stability. However, most previous studies have focused on thin films and ion irradiation, leaving the neutron irradiation response of bulk RHEAs largely unexplored. Mechanical behavior results show brittle behavior before and after irradiation. The addition of Zr led to an increase in hardness due to Zr-rich precipitates in the bulk microstructure. Lastly, hardness results showed an increase in hardening after irradiation indicating irradiation induced hardening has occurred.

36 - MATERIALS SCIENCE↗
DOE OSTI2019

Effect of the Temperature of Photonic Annealing on the Structural and Optical Properties of ZnO Films Synthesized by Dual Magnetron-Assisted Sputtering

Zinc-oxide films 1.4 μm in thickness are deposited onto glassy substrates by the dual magnetron-assisted sputtering of zinc targets in an argon and oxygen gas atmosphere. The dependences of the structural and optical characteristics of the ZnO films on the temperature of postdeposition photonic annealing are studied. It is established that an increase in the annealing temperature yields an increase in the degree of crystallinity of the films. Electron microscopy shows that the deposited ZnO coatings are columnar in structure and the microstructure density and crystallite size increase upon annealing. It is found that, at an annealing temperature of 450–650°C, the optical transmittance increases to >90% in the spectral range 400–1100 nm. The experimental results show that the temperature of vacuum photonic annealing has the most profound effect on the final properties of ZnO coatings.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2013

Effect of Cr doping in the microstructure, electrical and magnetic properties of In{sub 2−x}Cr{sub x}O{sub 3} system (x=0.1 and x=0.2)

In this paper a sol-gel method followed by a spin coating technique have been used to fabricate In{sub 2−x}Cr{sub x}O{sub 3} thin films with x=0.1 and 0.2. The structural analysis using an x-ray diffractometer showed that films have bixibyte cubic structure with good orientations to (222) directions. Microstructure analysis using atomic force microscope showed that sample with x=0.1 has clear pores and the particles tend to agglomerate and collect together with some holes seen on surface at x=0.2. The structure analysis using transmission electron microscope showed that the average grain size is 7.9 nm and 5.6 nm for samples x=0.1 and 0.2, respectively. The electrical measurements were carried out using Hall effect measurement system. The resistivity, carrier concentration and mobility for sample with x=0.1 is 27ohm.cm, 8.1×1016 cm{sup −3} and 1.9 cm{sup 2}V{sup −1}S{sup −1}, respectively and for higher dopant the film became insulator. The film with x=0.1 has metallic like behavior at 80-165K while semiconducting like behavior observed at 170-300K. Thermal activated conduction band and hoping conduction models have been used to estimate conducting mechanism in semiconducting part. Both samples show magnetic behavior at room temperature. The magnetic moment decreased from 6.7 emu/cm{sup 3} for x=0.1 to 2.8 emu/cm{sup 3} for x=0.2 while the coercivity increased from 85 Oe for x=0.1 to 120 Oe for x=0.2.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Improved ferroelectric polarization of V-doped Bi{sub 6}Fe{sub 2}Ti{sub 3}O{sub 18} thin films prepared by a chemical solution deposition

We prepared V-doped Bi{sub 6}Fe{sub 2}Ti{sub 3}O{sub 18} thin films on Pt/Ti/SiO{sub 2}/Si (100) substrates by using a chemical solution deposition route and investigated the doping effect on the microstructure, dielectric, leakage, and ferroelectric properties of Bi{sub 6}Fe{sub 2}Ti{sub 3}O{sub 18} thin films. The Bi{sub 5.97}Fe{sub 2}Ti{sub 2.91}V{sub 0.09}O{sub 18} thin film exhibits improved dielectric properties, leakage current, and ferroelectric properties. The incorporation of vanadium resulted in a substantially enhanced remnant polarization (2P{sub r}) over 30 μC/cm{sup 2} in Bi{sub 5.97}Fe{sub 2}Ti{sub 2.91}V{sub 0.09}O{sub 18} thin film compared with 10 μC/cm{sup 2} in Bi{sub 6}Fe{sub 2}Ti{sub 3}O{sub 18} thin film. It is demonstrated that the improved properties may stem from the improvement of crystallinity of the films with the contribution of suppressed oxygen vacancies and decreased mobility of oxygen vacancies caused by the V-doping. The results will provide a guidance to optimize the ferroelectric properties in Bi{sub 6}Fe{sub 2}Ti{sub 3}O{sub 18} thin films by chemical solution deposition, which is important to further explore single-phase multiferroics in the n = 5 Aurivillius thin films.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2015

Microstructure evolution of Al-doped zinc oxide and Sn-doped indium oxide deposited by radio-frequency magnetron sputtering: A comparison

The microstructure and morphology evolution of Al-doped zinc oxide (AZO) and Sn-doped indium oxide (ITO) thin films on borosilicate glass substrates deposited by radio-frequency magnetron sputtering at room temperature (RT) and 300 °C were investigated by X-ray diffraction and atomic force microscopy (AFM). One-dimensional power spectral density (1DPSD) functions derived from the AFM profiles, which can be used to distinguish different growth mechanisms, were used to compare the microstructure scaling behavior of the thin films. The rms roughness R{sub q} evolves with film thickness as a power law, R{sub q} ∼ d{sub f}{sup β}, and different growth exponents β were found for AZO and ITO films. For AZO films, β of 1.47 and 0.56 are obtained for RT and 300 °C depositions, respectively, which are caused by the high compressive stress in the film at RT and relaxation of the stress at 300 °C. While for ITO films, β{sub 1} = 0.14 and β{sub 2} = 0.64 for RT, and β{sub 1} = 0.89 and β{sub 2} = 0.3 for 300 °C deposition are obtained, respectively, which is related to the strong competition between the surface diffusion and shadowing effect and/or grain growth. Electrical properties of both materials as a function of film thickness were also compared. By the modified Fuchs-Sondheimer model fitting of the electrical transport in both materials, different nucleation states are pointed out for both types of films.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Controlling swelling in mixed transport polymers through alkyl side-chain physical cross-linking

Semiconducting conjugated polymers bearing glycol side chains can simultaneously transport both electronic and ionic charges with high charge mobilities, making them ideal electrode materials for a range of bioelectronic devices. However, heavily glycolated conjugated polymer films have been observed to swell irreversibly when subjected to an electrochemical bias in an aqueous electrolyte. The excessive swelling can lead to the degradation of their microstructure, and subsequently reduced device performance. An effective strategy to control polymer film swelling is to copolymerize glycolated repeat units with a fraction of monomers bearing alkyl side chains, although the microscopic mechanism that constrains swelling is unknown. Here we investigate, experimentally and computationally, a series of archetypal mixed transporting copolymers with varying ratios of glycolated and alkylated repeat units. Experimentally we observe that exchanging 10% of the glycol side chains for alkyl leads to significantly reduced film swelling and an increase in electrochemical stability. Through molecular dynamics simulation of the amorphous phase of the materials, we observe the formation of polymer networks mediated by alkyl side-chain interactions. When in the presence of water, the network becomes increasingly connected, counteracting the volumetric expansion of the polymer film.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Safe, Low-Cost, High Energy-Density, Solid-State Li-Ion Batteries

We developed intrinsically safe, robust, low-cost, high-energy-density solid-state Li-ion batteries, by integrating high conductivity garnet-type solid Li ion electrolytes and several different cathodes in tailored microstructures, fabricated by low-cost supported thin-film ceramic techniques, to overcome the primary technological barriers to next generation battery technology. In this ARPA-E project we employed Li-garnet solid-state electrolytes pioneered by one of the co-investigators (Thangadurai) which has room temperature (RT) conductivity of ~10 -3 S cm -1 . The highly stable garnet SSE allowed the use of S, NMC, and other cathodes with Li metal anodes without stability or flammability concerns. We studied the garnet’s stability when exposed to CO 2 and humidity (with or without an ALD coating) and showed that the material can be processed in ambient air for most steps prior to battery assembly, significantly reducing production costs. We extensively studied and scaled up the synthesis of the powder and explored external suppliers of garnet to determine the best pathway for commercial success. We used low-cost and scalable tapecasting fabrication methods to create porous-dense-porous “trilayer” solid electrolyte microstructures with a ~20 μm separating dense layer, and >70% porosity porous layers to host the electrodes. These scalable multilayer ceramic fabrication techniques, without need for dry rooms or vacuum equipment, also provide for dramatically reduced manufacturing costs. The tailored microstructured electrode supports (scaffold) increased interfacial area ~50x, overcoming the high impedance typical of planar geometry SSLiBs, resulting in record-setting 10 mA/cm 2 lithium cycling in a symmetric cell. We expanded our tapecasting ability and showed tapes >25m in length by the end of the project. We demonstrated the ability to sinter garnet without the use of a garnet powderbed, which could have been a major obstacle and waste of material at scale. At the same time, we expanded the size of our trilayers from coin cells (0.7 cm 2 ) to the full format design (30 cm 2 ). To develop full cells, we demonstrated 250 Wh/kg at room temperature with commercial NMC electrode films in a bilayer configuration. Similarly, we demonstrated 280 Wh/kg trilayer Li-S cells at room temperature with >90% capacity retention over 300 cycles. At 90°C we demonstrated 350 Wh/kg with a Li-S trilayer. The high thermal stability of the garnet electrolyte also enabled extended cycling (400 cycles) of a Li-TiS 2 cell at 150 °C, showcasing the exceptional safety and nonflammability of the solid-state trilayer batteries. Ion Storage Systems has taken this technology and knowledge to produce trilayer garnet electrolytes and is building out facilities to commercialize high performance solid state batteries. ISS has hired a strong staff, identified and communicated with a large number of potential partners, and successfully secured follow-on funding.

25 ENERGY STORAGE↗