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DOE OSTI2017

Tribological Properties of NiAl Matrix Composites Filled with Serpentine Powders

The unexplored tribological properties of NiAl matrix composites filled with serpentine powders are investigated using a reciprocating ball-on-disk configuration. Tribological test results reveal that increasing the serpentine concentration to some extent reduces the friction coefficients and wear rates of the composites. The best anti-friction and anti-wear performance is displayed by the NiAl matrix composite filled with 8 wt.% serpentine and 2 wt.% TiC (NAST). Microstructural analyses demonstrate that after adding serpentine, the self-lubricating films with different percentages of coverage form on the worn surfaces of the composites. A self-lubricating film with the highest percentage of coverage smears on the worn surface of NAST. This clearly suggests that serpentine can act as a new type of filler for NiAl matrix composites, whereas a combination of serpentine and TiC can enable serpentine to provide a full play to its excellent lubricating performance.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Hydrogen permeability and stability of palladium films in a high pressure reactor

Palladium (Pd) thin films were fabricated by colloidal spray deposition (CSD) on substrates of porous yttrium stabilized zirconium oxide (YSZ). The films were sintered at 1140–1160 °C for 2–3 h in argon and had thickness of 5–11 μm. The hydrogen (H 2 ) permeation flux for the Pd film was measured with simulated feed gases (90% H 2 /He, syn-gas/steam, or syn-gas/steam with H 2 S) flowing on the film side and sweep gas (Ar) flowing on the substrate side. Here, the hydrogen flux with the Pd film was obtained by adjusting the flow rate and pressure of the gas. Hydrogen flux values of 121–173 cm 3 min -1 cm -2 were measured at 388–596 °C (feed: 90% H 2 /He at 200 mL min -1 ; sweep: Ar at 1400 mL min -1 ; and ΔP = ~170 psi), and the permeability was calculated and compared with literature values. Because Pd is known to be sensitive to some gases, the stability of Pd films was evaluated by examining the microstructures of samples after their exposure to gas mixtures containing CO, CO 2 , H 2 O, and H 2 S. From the results of stability tests in H 2 S-containing atmospheres, the Pd/Pd 4 S phase boundary was determined, and this measured boundary was compared to the Pd/Pd 4 S boundary calculated from the thermodynamic data in the literature.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Welding of Semiconductor Nanowires by Coupling Laser-Induced Peening and Localized Heating

We demonstrate that laser peening coupled with sintering of CdTe nanowire films substantially enhances film quality and charge transfer while largely maintaining basic particle morphology. During the laser peening phase, a shockwave is used to compress the film. Laser sintering comprises the second step, where a nanosecond pulse laser beam welds the nanowires. Microstructure, morphology, material content and electrical conductivities of the films are characterized before and after treatment. The morphology results show that laser peening can decrease porosity and bring nanowires into contact and pulsed laser heating fuses those contacts. Multiphysics simulations coupling electromagnetic and heat transfer modules demonstrate that during pulsed laser heating, local EM field enhancement is generated specifically around the contact areas between two semiconductor nanowires, indicating localized heating. The characterization results indicate that solely laser peening or sintering can only moderately improve the thin film quality; however, when coupled together as laser peen sintering (LPS), the electrical conductivity enhancement is dramatic. LPS can decrease resistivity up to a factor of ~10,000, resulting in values on the order of ~10 5 Ω-cm in some cases, which is comparable to CdTe thin films. Our work demonstrates that LPS is an effective processing method to obtain high-quality semiconductor nanocrystal films.

Science & Technology - Other Topics↗

DOE OSTI2015

Interfacial development of electrophoretically deposited graphene oxide films on Al alloys

Adhesion between film and substrate is critical for electronic device and coating applications. Interfacial development between electrophoretically deposited graphene oxide films on Al 1100 and Al 5052 alloys were investigated using FT-IR and XPS depth profiling techniques. Obtained results suggest metal ion permeation from the substrates into deposited graphene oxide films. The interface between the films and the substrates were primarily composed of Al-O-C bonds from oxygenated defects on graphene oxide plane rather than expected Al-C formation. Films heat treated at 150 °C had change in microstructure and peak shifts in XPS spectra suggesting change in chemical structure of bonds between the films and the substrates.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2016

Cu-doped CdS and its application in CdTe thin film solar cell

Cu is widely used in the back contact formation of CdTe thin film solar cells. However, Cu is easily to diffuse from the back contact into the CdTe absorber layer and even to the cell junction interface CdS/CdTe. This phenomenon is generally believed to be the main factor affecting the CdTe solar cell stability. In this study Cu was intentionally doped in CdS thin film to study its effect on the microstructural, optical and electrical properties of the CdS material. Upon Cu doping, the V{sub Cd{sup −}} and the surface-state-related photoluminescence emissions were dramatically decreased/quenched. The presence of Cu atom hindered the recrystallization/coalescence of the nano-sized grains in the as-deposited CdS film during the air and the CdCl{sub 2} annealing. CdTe thin film solar cell fabricated with Cu-doped CdS window layers demonstrated much decreased fill factor, which was induced by the increased space-charge recombination near the p-n junction and the worsened junction crystalline quality. Temperature dependent current-voltage curve measurement indicated that the doped Cu in the CdS window layer was not stable at both room and higher temperatures.

36 MATERIALS SCIENCE↗

DOE OSTI2014

A close correlation between nanostructure formations and the thickness dependence of the critical current density in pure and BaSnO{sub 3}-added GdBa{sub 2}Cu{sub 3}O{sub 7-δ} films

A close correlation between the nanostructure formations and the thickness dependence of the in-field critical current density (J{sub c}) in GdBa{sub 2}Cu{sub 3}O{sub 7-δ} (GdBCO) films is reported. Pure and 2 wt. % BaSnO{sub 3} (BSO)-added GdBCO films with film thicknesses (d) ranging from 0.2 μm to 1.5 μm were deposited on SrTiO{sub 3} single-crystalline substrates by using a pulsed laser deposition technique. Magnetization data measured at 77 K with the magnetic field applied parallel to the c-axis of the films showed the general trend of decreasing in-field J{sub c} with increasing residual film thickness. The two special inversions, however, were observed at d ∼ 0.6 μm, for which the J{sub c}’s of both the pure and BSO-added GdBCO films were larger than those of the films with d ∼ 0.4 μm. A sequential ion-milling process and scanning electron microscopy studies were employed to examine the microstructural evolution in the 1.5- μm-thick GdBCO films. For the pure GdBCO films, nanosized dislocations were observed to start growing at intersections of perpendicularly connected a-axis-oriented grains in a residual film thickness (t) of ∼ 0.6 μm and the growth persisted to the top surface of the 1.5-μm-thick GdBCO film. For the BSO-added GdBCO films, the density of BSO nanorods was estimated to be decreased versus t with an increase found at t of ∼ 0.6 μm A reason for this inversions of J{sub c} might be the nanostructure formations at t ∼ 0.6 μm, which were proved to serve as effective pinning centers.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2018

Effect of Yb Substitution on Microstructure and Superconducting Properties of Y{sub 1−x}Yb{sub x}Ba{sub 2}Cu{sub 3}O{sub 7−δ} Films

The purpose of this study was to improve the critical current density (J{sub c}) of YBa{sub 2}Cu{sub 3}O{sub 7−δ} (YBCO) superconducting films at high magnetic fields. Thin Y{sub 1−x}Yb{sub x}Ba{sub 2}Cu{sub 3}O{sub 7−δ} (Y{sub 1−x}Yb{sub x}BCO) superconducting films on LaAlO{sub 3} substrates were prepared by modified low-fluorine metal organic deposition method (LF-MOD) in order to investigate the effect of Yb substitution on the microstructure and superconducting properties of a YBCO-coated conductor. In this study, single-phased, c-axial-aligned Y{sub 1−x}Yb{sub x}BCO films were obtained. Yb doping had a little effect on the critical temperature (T{sub c}) and transition width (ΔT) values of Y{sub 1−x}Yb{sub x}BCO films. An abnormal phenomenon was observed that the J{sub c} of Y{sub 1−x}Yb{sub x}BCO films at low field was smaller than that of the pure YBCO film, but the J{sub c} of Y{sub 1−x}Yb{sub x}BCO films at high field was much greater than that of the undoped YBCO film. Compared to pure YBCO film, the J{sub c} values of Y{sub 0.75}Yb{sub 0.25}BCO and Y{sub 0.25}Yb{sub 0.75}BCO films were enhanced by a factor of 8 at 8 T, 65 K, which meant that chemical substitution of Yb into the Y site could improve flux pinning significantly under the high magnetic field in Y{sub 1−x}Yb{sub x}BCO coated conductors.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Pulsed laser deposition and structural evolution of BaF 2 nanolayers in Eu-doped BaF 2 /Al 2 O 3 layered optical nanocomposite thin films

Here, we have developed a pulsed laser deposition (PLD) geometry for the growth of uniform BaF 2 nanoscale thin films, through control of the deposition conditions. Our goal is to use the BaF 2 layers with controllable structure as component layers in layered optical nanocomposites. The structure of the BaF 2 nanolayer evolves as a function of the layer thickness: BaF 2 grows via a layer-by-layer growth mode on Al 2 O 3 ; the layers are amorphous for a thickness < 3 nm, and then become nanocrystalline as the layer thickness increases. The BaF 2 nanocrystals have an FCC crystal structure with a weak < 111 > texture that becomes stronger for thicker films. We then demonstrate that our BaF2 films can be introduced into layered Al 2 O 3 /BaF 2 /EuO x nanocomposite films, which allows for control of the relative position of the Eu ions and the BaF 2 layer. Cross-section samples of the multilayered films show interfacial intermixing between the layers, which is related to implantation during the PLD process. This intermixing enables the incorporation of Eu ions into BaF 2 layers and form a thin Eu-doped BaF 2 nanolayer at the interface. The layered nanocomposite films show photoluminescence (PL) emission from Eu 3+ ions, and the PL intensity changes can be correlated with the crystallinity and crystal size changes in the BaF 2 layer. Our results provide guidance for achieving thin film nanocomposite materials with controllable structure and photoluminescence behavior for light emitting diodes, photovoltaics and other optical applications.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Creation of Self-Semi-Interpenetrating Network Structures in PIM-1 Membranes for Enhanced Physical Aging Resistance

A series of self-semi-interpenetrating network (ssIPN) thin films based on PIM-1 structure were developed by end-cross-linking telechelic PIM-1 oligomers end-capped with curable carboxylic acid groups to form model networks, which are penetrated by linear high-molecular-weight PIM-1 chains. ssIPN films with systematically varied network content ranging from 10 to 30 wt % were comprehensively examined on their microstructure and gas permeation properties. Fresh PIM-1 ssIPN films exhibited gas separation performances close to those of as-cast linear PIM-1, where the films closely followed the upper bound trade-off line, gaining as much selectivity as they lose gas permeability as the network content increases. This indicates that gas permeability is largely preserved despite cross-linking. Wide-angle X-ray scattering supported this observation, with peaks shifting toward lower d-spacing as oligomer content increased, suggesting tighter chain packing with higher cross-linkable oligomer loading. In physical aging studies over two months, all ssIPN films outperform linear PIM-1 for H 2 /CH 4 and O 2 /N 2 separations. Notably, the PIM-1 ssIPN with 10 wt % network content showed the best physical aging resistance, with negligible permeability loss even after one month. Finally, these findings highlight a promising macromolecular strategy for enhancing the physical aging resistance of microporous polymer membranes for gas separation.

PIM-1↗

NASA NTRS1991

Substrate effects on the epitaxial growth of ZnGeP2 thin films by open tube organometallic chemical vapor deposition

Epitaxial ZnGeP2-Ge films have been grown on (111)GaP substrates using MOCVD. The films grown with dimethylzinc to germane flow rate ratio R greater than 10 show mirror-smooth surface morphology. Films grown with R less than 10 show a high density of twinning, including both double position and growth twins. Compared to films grown on (001) GaP substrates, the layers on (111) GaP generally show a higher density of microstructural defects. TEM electron diffraction patterns show that the films grown on (111) GaP substrates are more disordered than films grown on (001) GaP under comparable conditions. The growth rate on (111) GaP substrates is about 2.5 times slower than that on (001) GaP, and films grown on Si substrates show extensive twinning formation. Both TEM and SEM examinations indicate that smooth epitaxial overgrowth may be easier on (111) Si substrates than on (001) Si.

Xing, G. C.↗

DOE OSTI2018

AFe{sub 2}O{sub 4}/(Pb{sub 0.80}Sr{sub 0.20})TiO{sub 3} (A = Mn, Ni and Co): a New Room-Temperature Magnetoelectric Multiferroic Bi-layered Composite Films

The room temperature and magnetic field-dependent dielectric, impedance and magnetoelectric (ME) coupling effect of polycrystalline AFe{sub 2}O{sub 4}/(Pb{sub 0.80}Sr{sub 0.20})TiO{sub 3} (A = Mn, Ni and Co) bi-layered composite films have been investigated. The structural and microstructural analyses using the X-ray diffraction (XRD), atomic force microscopy (AFM) and scanning electron microscopy (SEM) reveal the presence of homogenous growth of both tetragonal and spinel phases without any extra phase and diffusion in the AFO/PST20 bi-layered composite films. Our results show that all composite films exhibit ferroelectric as well as considerable magnetic, indicating magnetoelectric coupling effect. Our results show that the dielectric and impedance properties of AFO/PST20 bi-layered composite films can be manipulated by the magnetic field at room temperature, also indicating the existence of magnetoelectric coupling. The impedance (Z{sup ′} and Z{sup ″}) Nyquist plots show distinct electrical responses with the magnetic field. The maximum magnetoelectric coefficient (α) is found to be α{sub ME}∼ 239 and ∼ 195 mV/cm/Oe for the MFO/PST20 and CFO/PST20 bi-layered composite films, respectively. The above results show that the AFO/PST20 bi-layered composite films are room-temperature multiferroic material that can be potentially used in magnetoelectric devices.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2014

Role of the interface on radiation damage in the SrTiO{sub 3}/LaAlO{sub 3} heterostructure under Ne{sup 2+} ion irradiation

We systematically investigated the microstructural evolution of heteroepitaxial SrTiO{sub 3} (STO) thin films grown on a single crystal LaAlO{sub 3} (LAO) (001) substrate, focusing on the response of the STO/LAO interface to Ne{sup 2+} irradiation at room temperature. Cross sectional transmission electron microscope (TEM) analysis reveals that the LAO crystal amorphizes first after a relatively low dose of damage followed by the amorphization of the STO film after irradiation to a higher dose. While the critical dose to amorphize differs between each material, amorphization begins at the interface and proceeds outward in both cases. Thus, a crystalline/amorphous interface first forms at the STO/LAO interface by a dose of 1 dpa, and then an amorphous/amorphous interface forms when the dose reaches 3 dpa. Scanning TEM and x-ray energy dispersive spectroscopy indicate no significant heavy cation elemental diffusion, though electron energy loss spectroscopy reveals a redistribution of oxygen across the film/substrate interface after Ne{sup 2+} irradiation. Atomistic calculations are used to interpret the experimental findings in terms of the defect properties in each of the two component phases.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2020

Applications of plasma-enhanced metalorganic chemical vapor deposition

The use of plasma enhancement for growth of III-V compound semiconductor materials by metalorganic chemical vapor deposition (MOCVD) is examined, to improve control of microstructure, develop understanding of the underlying growth mechanisms, and expand the range of materials combinations for photovoltaic and solid-state lighting applications. Whereas plasma is commonly used with group-IV materials, such as silicon, few studies have examined the impact of plasma-enhanced MOCVD (PE-MOCVD) for III-V materials growth. PE-MOCVD provides improved decomposition of metalorganic precursors, which is driven by hydrogen plasma to augment hydride reactions and thermal pyrolysis, but plasma generation requires low reactor pressure. We have demonstrated elemental Al films grown by PE-MOCVD, which show distinct crystallographic texturing, and assume epitaxial microstructure upon post-growth annealing. We also demonstrate PE-MOCVD of GaAs at temperatures as low as 300 °C. With increasing radio-frequency power, the GaAs growth rate shows a transition from power limited to mass-transport limited. PE-MOCVD grown Ga 0.5 In 0.5 P shows no detectable spontaneous atomic ordering, which offers a mechanism to form order/disorder unicompositional heterostructures, without temperature change or impurity incorporation. In its current implementation, PE-MOCVD grown films have shown microstructural degradation, that we attribute to direct plasma exposure during growth. Improvements in the system design and growth sequences are at the focus of on-going efforts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2014

Effect of deposition temperature on electron-beam evaporated polycrystalline silicon thin-film and crystallized by diode laser

The effects of the deposition temperature on the microstructure, crystallographic orientation, and electrical properties of a 10-μm thick evaporated Si thin-film deposited on glass and crystallized using a diode laser, are investigated. The crystallization of the Si thin-film is initiated at a deposition temperature between 450 and 550 °C, and the predominant (110) orientation in the normal direction is found. Pole figure maps confirm that all films have a fiber texture and that it becomes stronger with increasing deposition temperature. Diode laser crystallization is performed, resulting in the formation of lateral grains along the laser scan direction. The laser power required to form lateral grains is higher in case of films deposited below 450 °C for all scan speeds. Pole figure maps show 75% occupancies of the (110) orientation in the normal direction when the laser crystallized film is deposited above 550 °C. A higher density of grain boundaries is obtained when the laser crystallized film is deposited below 450 °C, which limits the solar cell performance by n = 2 recombination, and a performance degradation is expected due to severe shunting.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

NASA NTRS1984

Metallic glass as a temperature sensor during ion plating

The temperature of the interface and/or a superficial layer of a substrate during ion plating was investigated using a metallic glass of the composition Fe67Co18B14Si1 as the substrate and as the temperature sensor. Transmission electron microscopy and diffraction studies determined the microstructure of the ion-plated gold film and the substrate. Results indicate that crystallization occurs not only in the film, but also in the substrate. The grain size of crystals formed during ion plating was 6 to 60 nm in the gold film and 8 to 100 nm in the substrate at a depth of 10 to 15 micrometers from the ion-plated interface. The temperature rise of the substrate during ion plating was approximately 500 C. Discontinuous changes in metallurgical microstructure, and physical, chemical, and mechanical properties during the amorphous to crystalline transition in metallic glasses make metallic glasses extremely useful materials for temperature sensor applications in coating processes.

Miyoshi, K.↗

NASA NTRS1985

Metallic glass as a temperature sensor during ion plating

Miyoshi, K.↗

DOE OSTI2015

On the thermal stability of physical vapor deposited oxide-hardened nanocrystalline gold thin films

We describe a correlation between electrical resistivity and grain size for PVD synthesized polycrystalline oxide-hardened metal-matrix thin films in oxide-dilute (<5 vol. % oxide phase) compositions. The correlation is based on the Mayadas-Shatzkes (M-S) electron scattering model, predictive of grain size evolution as a function of composition in the oxide-dilute regime for 2 μm thick Au-ZnO films. We describe a technique to investigate grain boundary (GB) mobility and the thermal stability of GBs based on in situ electrical resistivity measurements during annealing experiments, interpreted using a combination of the M-S model and the Michels et al. model describing solute drag stabilized grain growth kinetics. Using this technique, activation energy and pre-exponential Arrhenius parameter values of E{sub a} = 21.6 kJ/mol and A{sub o} = 2.3 × 10{sup −17} m{sup 2}/s for Au-1 vol. % ZnO and E{sub a} = 12.7 kJ/mol and A{sub o} = 3.1 × 10{sup −18} m{sup 2}/s for Au-2 vol. % ZnO were determined. In the oxide-dilute regime, the grain size reduction of the Au matrix yielded a maximum hardness of 2.6 GPa for 5 vol. % ZnO. A combined model including percolation behavior and grain refinement is presented that accurately describes the composition dependent change in electrical resistivity throughout the entire composition range for Au-ZnO thin films. The proposed correlations are supported by microstructural characterization using transmission electron microscopy and electron diffraction mapping for grain size determination.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Shape-Controlled NaTaO 3 by Flux-Mediated Synthesis

NaTaO 3 is a stable and wide bandgap n-type semiconductor material with many different applications. Here, a flux-mediated synthesis method is presented for NaTaO 3 resulting in highly distinctive, substrate covering shapes via precursor chemistry variation at comparatively low temperatures. It is found that the microstructure of the resulting NaTaO 3 films can be varied from nanocubes to smooth thin films. These shapes and surface chemistries can be correlated by employing density functional theory calculations and surface sensitive X-ray photoemission spectroscopy. This study provides guidance on how to synthesize the material and tailor its shape and surface termination for different applications. Finally, as a proof of concept of one possible application, NaTaO 3 is applied to perovskite solar cells as the electron transport layer, resulting in conversion efficiencies of >19%. Further, this study provides a new strategy for designing ternary oxide thin films for renewable energy applications.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗