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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 343 records · Page 19
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Combinatorial sputter deposition of ultrathick Au-Bi alloy films

We report gold-bismuth alloys are of interest as catalysts and catalytic sensing systems, electrochemical sensors, superconductors, and hohlraums for magnetically assisted inertial confinement fusion implosions. Radiation-hydrodynamics simulations with the Lasnex code of laser-driven hohlraums predict higher x-ray drive from Au-Bi alloys compared with cases of Au-Ta or pure Au and Bi hohlraums. Here, we use direct current magnetron sputtering in Ar gas, with co-sputtering from two elemental targets, to deposit Au-Bi alloys with Bi content of 9–77 at.% and thicknesses up to ~20 µm. Films are characterized by a combination of x-ray diffraction, Rutherford backscattering, scanning electron microscopy, substrate-curvature-based residual stress, and electronic transport measurements. Experiments are complemented by Monte Carlo simulations of ballistic sputtering and gas phase transport of depositing species and Ar gas atoms. Results show that all films are polycrystalline, with three distinct compositional regimes dominated by Au, Au 2 Bi, and Bi crystallographic phases. A metallic behavior of the temperature dependence of electrical resistivity is observed for all the films. Films with Bi content above ~30 at.% exhibit porosity, which is tolerable to hohlraum x-ray drive based on Lasnex simulations.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Optimized oxygen deprived low temperature sputtered WO3 thin films for crystalline structures

In this work, we report a detailed analysis on the effects of processing parameters for sputtered tungsten trioxide (WO 3 ) thin nanoscale films on their structural, vibrational and electrical properties. The research aims to understand the fundamental aspects of WO3 sputtering at relatively low temperatures and in an oxygen deprived environment targeting applications of temperature and oxygen sensitive substrates. Structural analysis indicates that films deposited at room temperature, or substrate temperatures at or below 400 degrees C with low oxygen partial pressure are amorphous. Furthermore, crystallization of the films was observed with distinct Raman peaks when the films were annealed at 300 degrees C or above using rapid thermal annealing for 10 min. Films revealed monoclinic phases of WO 3 with the presence of W-O-W stretching, bending and lattice vibrational modes in the Raman spectra. Interestingly, a change of transport behavior from insulating to semiconducting was observed for as deposited films on post annealing. Annealed films revealed stoichiometric WO 3 phases with no external defects detected. The present study adopts a route to intercalate WO 3 in a variety of applications from electrochromic coloration to a nanocrystalline thin film for electronic devices sensitive to higher temperatures and gas flow in the sputtering system.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2020

Large anisotropic magnetocaloric effect in all-sputtered epitaxial terbium thin films

We present an experimental investigation of the magnetic and magnetocaloric properties of sputtered epitaxial and amorphous Tb thin films. We grew epitaxial Nb (50-nm)/Tb (100-nm) bilayer thin films on Al 2 O 3 $(11\bar{2}0)$ substrate using DC magnetron sputtering at high temperature, with excellent crystalline quality of the hcp Tb(0001) layer. While the amorphous Tb thin film exhibits more isotropic magnetocaloric properties, we show that the epitaxial Tb thin film displays large anisotropic magnetocaloric properties, with a large maximum magnetic entropy change of 6.27 J kg -1 K -1 at the Néel temperature as well as a large relative cooling power of 225 J kg -1 with a magnetic field change ΔH = 20 kOe applied along the in-plane direction. These large and anisotropic magnetocaloric properties are much larger than those measured for the amorphous Tb thin film, or previously reported for Tb-based thin-film structures. Our findings highlight the opportunities for growing epitaxial rare-earth thin films using sputtering techniques and demonstrate the importance of crystallographic control on the magnetocaloric effect in Tb thin films.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Microstructural and Superconducting Radiofrequency Properties of Multilayer Sequentially Sputtered Nb 3 Sn films

Nb 3 Sn is considered as a potential candidate for superconducting radiofrequency cavities for particle acceleration due to its higher transition temperature of 18.3 K and higher superheating field of 400 mT. Nb 3 Sn films can be grown inside the surface of a Nb cavity by sequentially sputtering multiple layers of Nb and Sn thin films followed by annealing at 950 °C for 3 h. We report on the properties of Nb 3 Sn films grown on Nb substrates by magnetron sputtering. The films’ crystal structure, surface morphology, and composition were characterized by X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The films had a polycrystalline Nb 3 Sn structure with a fine-grain surface and an atomic Sn composition of ~23%. The RF surface resistance of the films was measured for different temperatures at 7.4 GHz to understand the feasibility of this method for the SRF application. The RF surface resistance of the films was 5 mΩ at 12 K, which is about 2 orders of magnitude higher than 60 μΩ previously measured in Nb 3 Sn films grown by Sn vapor diffusion. Finally, the sputtered film had a superconducting transition at 17.2 K, which is also lower than 17.9 K observed in Nb 3 Sn film prepared by vapor diffusion.

43 PARTICLE ACCELERATORS↗
DOE OSTI2012

Electrochemical properties of sputter-deposited MoO{sub 3} films in lithium microbatteries

Molybdenum oxide (MoO{sub 3}) films were prepared by magnetron sputtering using an Mo target. The films were sputtered in the reactive atmosphere of an argon-oxygen gas mixture under various substrate temperatures, T{sub s}, and oxygen partial pressures, p(O{sub 2}). The effects of the growth conditions on the microstructure were examined using reflection high-energy electron diffraction and x-ray photoelectron spectroscopy. The analyses indicate that stoichiometric and polycrystalline MoO{sub 3} films were obtained at T{sub s} = 445 Degree-Sign C and p(O{sub 2}) = 61%. The applicability of the sputtered MoO{sub 3} films for lithium microbattery application has been demonstrated. The discharge-charge profiles, the kinetics of lithium intercalation process in the film, and the cycling behavior have been investigated in detail to understand the effect of microstructure on the electrochemical performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Effect of target-substrate distance on properties of flexible InZnSnO films grown by linear facing target sputtering

The authors have investigated the effect of target-to-substrate distance (TSD) on the electrical, optical, and structural properties of flexible InZnSnO (IZTO) films grown on polyethylene terephthalate substrates using linear facing target sputtering (LFTS) at room temperature. The electrical and optical properties of IZTO film grown by LFTS were significantly influenced by TSD while the structural and surface properties of IZTO film were not affected by TSD, unlike conventional magnetron sputtering. Regardless of TSD, all IZTO film showed completely amorphous structure with very low root mean square roughness of 0.33 nm, due to the low kinetic energy of sputtered IZTO atoms and a substrate position that did not directly face the targets. Based on the figure of merit value, the optimized TSD for deposition of flexible IZTO films is 2.5 cm. At optimized conditions, the IZTO film showed a sheet resistance of 23.1 {Omega}/sq and an optical transmittance of 80%.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Negative oxygen ion formation in reactive magnetron sputtering processes for transparent conductive oxides

Reactive d.c. magnetron sputtering in Ar/O{sub 2} gas mixtures has been investigated with energy-resolved mass spectrometry. Different metal targets (Mg, Ti, Zn, In, InSn, and Sn), which are of importance for transparent conductive oxide thin film deposition, have been used to study the formation of negative ions, mainly high-energetic O{sup -}, which are supposed to induce radiation damage in thin films. Besides their energy distribution, the ions have been particularly investigated with respect to their intensity in comparison of the different target materials. To realize the comparability, various calibration factors had to be introduced. After their application, major differences in the negative ion production have been observed for the target materials. The intensity, especially of O{sup -}, differs by about two orders of magnitude. It is shown that this difference results almost exclusively from ions that gain their energy in the target sheath. Those may gain additional energy from the sputtering process or reflection at the target. Low-energetic negative ions are, however, less affected by changes of the target material. The results concerning O{sup -} formation are discussed in term of the sputtering rate from the target and are compared to models for negative ion formation.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Process monitoring during AlN{sub x}O{sub y} deposition by reactive magnetron sputtering and correlation with the film's properties

In this work, AlN{sub x}O{sub y} thin films were deposited by reactive magnetron sputtering, using an aluminum target and an Ar/(N{sub 2}+O{sub 2}) atmosphere. The direct current magnetron discharge parameters during the deposition process were investigated by optical emission spectroscopy and a plasma floating probe was used. The discharge voltage, the electron temperature, the ion flux, and the optical emission lines were recorded for different reactive gas flows, near the target and close to the substrate. This information was correlated with the structural features of the deposits as a first step in the development of a system to control the structure and properties of the films during reactive magnetron sputtering. As the target becomes poisoned, the discharge voltage suffers an important variation, due to the modification of the secondary electron emission coefficient of the target, which is also supported by the evolution of the electron temperature and ion flux to the target. The sputtering yield of the target was also affected, leading to a reduction of the amount of Al atoms arriving to the substrate, according to optical emission spectroscopy results for Al emission line intensity. This behavior, together with the increase of nonmetallic elements in the films, allowed obtaining different microstructures, over a wide range of compositions, which induced different electrical and optical responses of films.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Hysteresis-free high rate reactive sputtering of niobium oxide, tantalum oxide, and aluminum oxide

This work reports on experimental studies of reactive sputtering from targets consisting of a metal and its oxide. The composition of the targets varied from pure metal to pure oxide of Al, Ta, and Nb. This combines features from both the metal target and oxide target in reactive sputtering. If a certain relation between the metal and oxide parts is chosen, it may be possible to obtain a high deposition rate, due to the metal part, and a hysteresis-free process, due to the oxide part. The aim of this work is to quantify the achievable boost in oxide deposition rate from a hysteresis-free process by using a target consisting of segments of a metal and its oxide. Such an increase has been previously demonstrated for Ti using a homogeneous substoichiometric target. The achievable gain in deposition rate depends on transformation mechanisms from oxide to suboxides due to preferential sputtering of oxygen. Such mechanisms are different for different materials and the achievable gain is therefore material dependent. For the investigated materials, the authors have demonstrated oxide deposition rates that are 1.5–10 times higher than what is possible from metal targets in compound mode. However, although the principle is demonstrated for oxides of Al, Ta, and Nb, a similar behavior is expected for most oxides.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Method to control deposition rate instabilities—High power impulse magnetron sputtering deposition of TiO{sub 2}

The authors describe how changes in shutter state (open/closed) affect sputter plasma conditions and stability of the deposition rate of Ti and TiO{sub 2} films. The films were grown by high power impulse magnetron sputtering in pure Ar and in Ar/O{sub 2} mixture from a metallic Ti target. The shutter state was found to have an effect on the pulse waveform for both pure Ar and reactive sputtering of Ti also affecting stability of TiO{sub 2} deposition rate. When the shutter opened, the shape of pulse current changed from rectangular to peak-plateau and pulse energy decreased. The authors attribute it to the change in plasma impedance and gas rarefaction originating in geometry change in front of the magnetron. TiO{sub 2} deposition rate was initially found to be high, 1.45 Å/s, and then dropped by ∼40% during the first 5 min, while for Ti the change was less obvious. Instability of deposition rate poses significant challenge for growing multilayer heterostructures. In this work, the authors suggest a way to overcome this by monitoring the integrated average energy involved in the deposition process. It is possible to calibrate and control the film thickness by monitoring the integrated pulse energy and end growth when desired integrated pulse energy level has been reached.

42 ENGINEERING↗
DOE OSTI2015

Spatially resolved electron density and electron energy distribution function in Ar magnetron plasmas used for sputter-deposition of ZnO-based thin films

Langmuir probe and trace rare gases optical emission spectroscopy were used to analyze the spatial structure of the electron density and electron energy distribution function (EEDF) in a cylindrical Ar magnetron plasma reactor used for sputter-deposition of ZnO-based thin films. While a typical Bessel (zero order) diffusion profile was observed along the radial direction for the number density of charged particles at 21 cm from the ZnO target, a significant rise of these populations with respect to the Bessel function was seen in the center of the reactor at 4 cm from the magnetron surface. As for the EEDF, it was found to transform from a more or less Maxwellian far from the target to a two-temperature Maxwellian with a depletion of high-energy electrons where magnetic field confinement effects become important. No significant change in the behavior of the electron density and EEDF across a wide range of pressures (5–100 mTorr) and self-bias voltages (115–300 V) was observed during magnetron sputtering of Zn, ZnO, and In{sub 2}O{sub 3} targets. This indicates that sputtering of Zn, In, and O atoms do not play a very significant role on the electron particle balance and electron heating dynamics, at least over the range of experimental conditions investigated.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Sputtered carbon as a corrosion barrier for x-ray detector windows

Sputtered amorphous carbon thin films were explored as corrosion resistant coatings on aluminum thin films to be incorporated into x-ray detector windows. The requirements for this application include high corrosion resistance, low intrinsic stress, high strains at failure, and high x-ray transmission. Low temperature sputtering was used because of its compatibility with the rest of the window fabrication process. Corrosion resistance was tested by exposure of carbon coated and uncoated Al thin films to humidity. Substrate curvature and bulge testing measurements were used to determine intrinsic stress and ultimate strain at failure. The composition and bonding of the carbon films were further characterized by electron energy loss spectroscopy, Raman spectroscopy, and carbon, hydrogen, and nitrogen elemental analyses. Samples had low compressive stress (down to.08 GPa), a high strain at failure (3%), and a low fraction of sp{sup 3} carbon–carbon bonds (less than 5%). The high breaking strain and excellent x-ray transmission of these sputtered carbon films indicate that they will work well as corrosion barriers in this application.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Characterization of Cu2ZnSnS4 Thin Films Prepared by the Sulfurization of Co-sputtered Metal Precursors

In this work, we report on the synthesis and characterization of Cu2ZnSnS4 (CZTS) thin films prepared by annealing of co-sputtered metal precursors in sulfur atmosphere. Radio-frequency magnetron sputtering was applied to deposit the metal layers from single metal targets on Mo-coated soda-lime glass substrates. The chemical composition of the precursors was controlled by varying the sputtering working power, resulting in films with various compositions. X-ray fluorescence was used to determine the elemental concentration of these metal films. The metal precursors were then converted into CZTS in a tube furnace using different sulfurization conditions to investigate the effect of the annealing process on the properties of the final CZTS films. Film structural characterization and phase identification results were supported by X-ray diffraction (XRD) and Raman spectroscopy. Surface and cross-sectional film morphology was carried out by scanning electron microscopy (SEM). For the sulfurized films, significant Sn loss was noticed. However, the loss of Sn was successfully controlled by depositing precursors with an excess of Sn. After optimizing the composition of the metal precursor, XRD and Raman scattering results revealed single-phase CZTS films without clear signs of secondary phases. SEM showed improved morphology in the form of dense structures and smooth surfaces for the films sulfurized at 600 degrees C. Our first solar cell, based on a CZTS film originating from a precursor sulfurized at 550 degrees C for 60 min, showed an open-circuit voltage of 471 mV, a short-circuit current density of 9.92 mA/cm-2, a fill factor of 36.9%, and an efficiency of 1.72%.

14 SOLAR ENERGY↗
DOE OSTI2018

Phase Formation and Electronic Structure Peculiarities in the Al{sub 1–} {sub x}Si{sub x} Film Composites under the Conditions of Magnetron and Ion-Beam Sputtering

The peculiarities of the phase composition and electronic structure of aluminum–silicon composite films near the Al{sub 0.75}Si{sub 0.25} composition obtained by the magnetron and ion-beam sputtering methods on a Si(100) silicon substrate are studied using the X-ray diffraction techniques and ultrasoft X-ray emission spectroscopy. In addition to silicon nanocrystals of about 25 nm in size, an ordered solid solution corresponding to the previously unknown Al{sub 3}Si phase is formed in magnetron sputtering on a polycrystalline Al matrix. Films obtained by ion-beam sputtering of the composite target are found to be monophasic and contained only one phase of an ordered solid solution of aluminum silicide Al{sub 3}Si of the Pm3m cubic system with the primitive cell parameter a = 4.085 Å. However, subsequent pulsed photon annealing of the composite with different radiation doses from 145 to 216 J/cm{sup 2} gives rise to the partial decomposition of the Al{sub 3}Si phase with the formation of free metallic aluminum and silicon nanocrystals with sizes in the range from 50 to 100 nm, depending on the pulsed photon radiation dose.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Calculation of Self-Sputtering Yield under Ion Bombardment of Solids: Computer Simulation and Theory

We developed a computer simulation program for investigation of solid self-sputtering under ion bombardment. The program is based on binary collision approximation, truncated Coulomb potential, and the model of local inelastic losses proportional to energy. As a result of simulation, the self-sputtering yield is calculated as a function of atomic number and ion energy. To verify the cascade simulation code, we created a self-sputtering theory for the case of hard sphere potential. Simulation results show good agreement with both experimental data and theory.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

Oxygen Reduction Reaction Activity of Nanocolumnar Platinum Thin Films by High Pressure Sputtering

Nanocolumnar platinum thin films (Pt-TFs) were produced by high pressure sputtering (HIPS) and investigated as oxygen reduction reaction electrocatalysts for polymer electrolyte membrane fuel cells. Conventional high-density Pt-TF prepared by low pressure sputtering was also studied for comparison. Pt-TFs were deposited on a microporous layer (MPL)-like surface composed of carbon particles to mimic catalyst-coated gas diffusion electrodes. Electron microscopy imaging revealed that HIPS Pt-TFs developed a cauliflower-like columnar microstructure, which originated from a shadowing effect during HIPS. This shadowing effect is enhanced on the rough surface of the MPL-like carbon that leads to the nano-cauliflower formation. With this approach, we also aimed to relate the catalyst performance obtained by benchtop tests directly to membrane electrode assembly test results. The electrochemically active surface area of Pt-TFs increased from 10 to 19 m 2 /g with increasing sputter pressure. Specific activity of conventional high-density and nanocolumnar films were similar at ~600 μA/cm 2 , which is likely due to their similar crystal grain sizes, >5 nm. On the other hand, mass-specific (MA) activity values increased from ~0.06 A/mgPt for conventional Pt-TF to ~0.13 A/mgPt for HIPS Pt-TFs, which is consistent with the columnar microstructure of HIPS films providing a better catalyst utilization compared to conventional Pt-TF.

08 HYDROGEN↗
DOE OSTI2016

Bandgap Engineering of Cu(In 1-x Gax)Se 2 Absorber Layers Fabricated using CuInSe 2 and CuGaSe 2 Targets for One-Step Sputtering Process

Here we have demonstrated that the bandgap of Cu(In 1-x Ga x )Se 2 (CIGS) absorber layers was readily controlled by using a one-step sputtering process. CIGS thin-film sample libraries with different Ga/(In + Ga) ratios were synthesized on soda-lime glass at 550 °C using a combinatorial magnetron sputtering system employing CuInSe 2 (CIS) and CuGaSe 2 (CGS) targets. Energy-dispersive X-ray fluorescence spectrometry (EDS-XRF) confirmed that the CIGS films had different Ga/(In + Ga) ratios, which were varied by the sample configuration on the substrate and ranged from 0.2 to 0.9. X-ray diffraction and Raman spectroscopy revealed that the CIGS films had a pure chalcopyrite phase without any secondary phase such as Cu-Se or ordered vacancy compound (OVC), respectively. Furthermore, we found that the optical bandgap energies of the CIGS films determined by transmittance measurements ranged from 1.07 eV to 1.53 eV as the Ga/(In + Ga) ratio increased from 0.2 to 0.9, demonstrating that the one-step sputtering process using CIS and CGS targets is another simple route to control the bandgap energy of the CIGS absorber layer.

14 SOLAR ENERGY↗
DOE OSTI2017

Ultra‐low Mass Sputtered and Conventional Catalyst Layers on Plasma‐etched Nafion for PEMFC Applications

Abstract This paper presents performance results for the use of plasma‐etched Nafion membranes to suppress polarization losses in proton exchange membrane fuel cells (PEMFCs) configured from 0.1 mg cm −2 conventional Pt/C dispersion and 0.02 mg cm −2 ultra‐thin sputter‐deposited Pt catalyst layers. Four MEA configurations, namely, etched membrane‐conventional electrode, pristine membrane‐conventional electrode, etched membrane‐sputter electrode, and pristine membrane‐sputter electrode cells were explored, and their respective maximum power densities were ∼514.6, 417.9, 170.1 and 138.3 mW cm −2 . The results demonstrated that independent of MEA fabrication approach, cells with O 2 plasma treated membranes had reduced ohmic resistances and delivered superior performance over their pristine counterparts, validating the utility of membrane etching for achieving improved PEMFC performance.

Omosebi, A.↗