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At least 217 records · Page 12
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

A High-Ceramic-Loading LATP–PVDF–Al 2 O 3 Composite Film for Lithium-Ion Batteries With Favorable Porous Microstructure and Enhanced Thermal Stability

A separator plays a crucial role in a Li-ion battery to carry liquid electrolytes while preventing short-circuiting between electrodes. Nevertheless, conventional commercial separators often exhibit poor wettability and are prone to shrink at elevated temperatures due to their limited thermal stability. Herein, we report a heat-resistant LATP–PVDF–Al 2 O 3 composite film with outstanding wetting performance. The thin film was prepared using ball mill mixing and tape-casting processes. Two solvents, NMP and glycerol, were applied to prepare the slurry, and a favorable microstructure in the film was created after drying. Here, the ionic conductivity of the film was tested at 1.39 mS cm –1 when paired with liquid electrolyte, almost double that of the commercial counterpart. The high ceramic loading of 70% improved both the thermal shrinkage resistance and dendrite inhibition of the membrane. When assembled in an NMC half-cell, the cycling capacity retentions of 92.8% and 92.1% are achieved after 50 cycles at 0.5 C and 1 C, demonstrating its capability to be used in Li-ion batteries.

25 ENERGY STORAGE↗
DOE OSTI2019

Interfacial Strength Evaluation of Oxide Films on Carbon Steel by Using the Laser Shock Adhesion Test

We investigate the adhesion strength (interfacial strength) of the oxide film formed on a carbon steel substrate by using a laser shock adhesion test (LaSAT). A rolled carbon steel (SS400) plate is first heated at high temperature (700 °C) under the atmosphere (heat treatment) to cause the formation of oxide films about 20-50 μm thick on the steel surface. The film consisted of multiple layers, including wustite (FeO), magnetite (Fe{sub 3}O{sub 4}), and hematite (Fe{sub 2}O{sub 3}). Next, the x-ray diffraction method was used to measure the residual stress in the film. We find that compression stress develops in the film because of a mismatch of thermal strain in between the film and substrate after the heat treatment. With LaSAT, strong elastic wave generates by a pulsed laser ablation of the substrate backside, and results in interfacial fractures in the oxide films. To monitor the normal (out-of-plane) displacement of the top surface film, a laser ultrasonic interferometer is simultaneously utilized, such that we detect film delamination and determine the critical laser energy for interfacial fracture to obtain the critical stress (interfacial strength). Furthermore, additional pulsed laser irradiation is conducted against a pre-delaminated specimen in order to examine the growth of delamination area and evaluate the interfacial fracture toughness. Finally, elastic wave propagation in the sample is computed using the finite element method (FEM) in order to evaluate the interfacial stress field, accurately. For the FEM, multiple layers in the oxide film are modeled, and the residual stress due to thermal strain mismatch is introduced. The FEM computations reveal the stress distribution around the interface and evaluate the critical stress and critical stress intensity factor for delamination. We thus quantitatively evaluate the interfacial strength and interfacial fracture toughness of the oxide film formed on carbon steel. The mechanism of interfacial fracture is also discussed on the basis of microstructures in a film with multiple layers. This result may be useful for understanding the adhesion quality of oxide film during the hot-rolling process.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Strength, stiffness, and microstructure of Cu(In,Ga)Se{sub 2} thin films deposited via sputtering and co-evaporation

This work examines Cu(In,Ga)Se{sub 2} thin films fabricated by (1) selenization of pre-sputtered Cu-In-Ga and (2) co-evaporation of each constituent. The efficiency disparity between films deposited via these two methods is linked to differences in morphology and microstructure. Atomic force microscopy and scanning electron microscopy show that selenized films have rougher surfaces and poor adhesion to molybdenum back contact. Transmission electron microscopy and electron energy loss spectroscopy revealed multiple voids near the Mo layer in selenized films and a depletion of Na and Se around the voids. Residual stresses in co-evaporated films were found to be ∼1.23 GPa using wafer curvature measurements. Uniaxial compression experiments on 500 nm-diameter nanopillars carved out from co-evaporated films revealed the elastic modulus of 70.4 ± 6.5 GPa. Hertzian contact model applied to nanoindentation data on selenized films revealed the indentation modulus of 68.9 ± 12.4 GPa, which is in agreement with previous reports. This equivalence of the elastic moduli suggests that microstructural differences manifest themselves after the yield point. Typical plastic behavior with two distinct failure modes is observed in the extracted stress-strain results, with the yield strength of 640.9 ± 13.7 MPa for pillars that failed by shearing and 1100.8 ± 77.8 MPa for pillars that failed by shattering.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Effect of Different Zirconium Contents on the Corrosion Resistance of ZrO{sub 2}-TiO{sub 2} Film-Coated Stainless Steel

This work discusses the corrosion resistance of x%zirconia (ZrO{sub 2})–x%titania (TiO{sub 2}) nanocomposite films with different percentages of ZrO{sub 2} prepared on stainless steel by dipping the substrates in sol–gel solutions. The phase compositions and microstructures of the films were investigated by x-ray diffraction (XRD) and scanning electron microscopy (SEM). Tafel polarization curves and electrochemical impedance spectroscopy (EIS) were employed to investigate the corrosion resistance of the coated steel substrates during immersion in a 5% NaCl solution at room temperature. The results showed that when the percentage of ZrO{sub 2} in the sol–gel was relatively low, the film contained cracks, leading to a poor corrosion resistance. When the percentage of ZrO{sub 2} was higher, the corrosion resistance of the film was also affected by the sintering temperature; a sintering temperature of 650 °C gave the best protection of the metal surface, and the protection efficiency was 95%.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2014

Fabrication of CuAl{sub 1−x}M{sub x}O{sub 2} (M = Fe, Cr)/Ni film delafossite compounds using spin coating and their microstructure and dielectric constant

The discovery of delafossite compound has encouraged more rapid technological developments particularly in transparent electronic devices. Copper oxide-based transparent thin films delafossite semiconductor recently give much attention in the field of optoelectronic technology, after the discovery of p-type CuAlO{sub 2}. The potential applications of a p-type semiconductor transparent conductive oxides (TCO) have been applied in broad field of optoelectronics. To explore a broad physical properties interms of magnetic conducting subtitution is understudied. In this work we report the fabrication of delafossite film on Ni substrate and their characterization of CuAl{sub 1−x}M{sub x}O{sub 2} delafossite compounds doped with Cr{sup 3+} and Fe{sup 3+} from the raw material of Cu(NO{sub 3}){sub 2}@@‡3H{sub 2}O, Al(NO{sub 3}){sub 3}@@‡9H{sub 2}O, Fe(NO{sub 3}){sub 3}@@‡9H{sub 2}O and Cr(NO{sub 3}){sub 3}@@‡9H{sub 2}O. The films were prepared using spin coating through a sol-gel technique at various concentrations of x = 0, 0.03, 0.04, and 0.05 for chromium and x = 0, 0.02, 0.04, 0.06, and 0.08 for iron doped. Crystal and microstructure were characterized by means of Cu-Kα Bragg-Brentano X-RD followed by High Score Plus and SEM-EDAX. The dielectric constants of the films were characterized using LCR meter. It was found that the CuAl{sub 1−x}M{sub x}O{sub 2}/Ni delafossite films were successfully fabricated. The CuAl{sub 1−x}Fe{sub x}O{sub 2} compound crystallized with lattice parameters of a = b ranged from 2.8603 Å to 2.8675 Å and c ranged from 16.9576 to 17.0763 Å. The increase of the dopant give rise to the increase of the lattice parameters. Since iron has bigger ionic radius (69 pm) than original site of Al{sup 3+} with radius of 53 pm the crystal volume lattice also increase. Further analyses of increasing volume of the crystal, as expected, affected to the decreasing of its dielectric constant. The similar trends also shown by Cr{sup 3+} doped of CuAl{sub 1−x}Cr{sub x}O{sub 2} films with smaller effects.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Microstructure investigations of hcp phase CoPt thin films with high coercivity

CoPt films have been grown in the past with a high anisotropy in L1{sub 1} or L1{sub 0} phase, and a high coercivity is observed only in L1{sub 0} CoPt films. Recently, we have grown CoPt films which exhibited a high coercivity without exhibiting an ordered phase. In this study, high resolution transmission electron microscopy (HRTEM) investigations have been carried out to understand the strong thickness and deposition pressure dependent magnetic properties. HRTEM studies revealed the formation of an initial growth layer in a metastable hexagonal (hcp) CoPt with high anisotropy. This phase is believed to be aided by the heteroepitaxial growth on Ru as well as the formation of Ru-doped CoPt phase. As the films grew thicker, transformation from hcp phase to an energetically favourable face-centered cubic (fcc) phase was observed. Stacking faults were found predominantly at the hcp-fcc transformation region of the CoPt film. The higher coercivity of thinner CoPt film is attributed to relatively less fcc fraction, less stacking faults, and to the isolated grain structure of these films compared to the thicker films.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Investigation of cellular microstructure and enhanced coercivity in sputtered Sm{sub 2}(CoCuFeZr){sub 17} film

We have investigated the effect of annealing temperature on the microstructure and magnetic properties of Sm{sub 2}(CoCuFeZr){sub 17} films prepared using ion beam sputtering at room temperature. The as-deposited film shows randomly oriented polycrystalline grains and exhibits small coercivity (H{sub C}) of 0.04 T at room temperature. Post annealing of these films at 700 °C under Ar atmosphere shows significant changes in the microstructure transforming it to the development of cellular growth, concomitant with enhanced coercivity up to 1.3 T. The enhanced coercivity is explained using the domain wall pinning mechanism.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Dynamics of the gold–silicon eutectic reaction studied at limited length scales using in situ $\mathrm{TEM}$ and $\mathrm{STEM}$

We report the dynamics of the gold–silicon eutectic reaction in limited dimensions were studied using in situ transmission electron microscopy and scanning transmission electron microscopy heating experiments. The phase transformation, viewed in both plan-view and cross-section of the film, occurs through a complex combination of dislocation and grain boundary motion and diffusion of silicon along gold grain boundaries, which results in a dramatic change in the microstructure of the film. The conversion observed in cross-section shows that the eutectic mixture forms at the Au–Si interface and proceeds into the Au film at a discontinuous growth rate. This complex process can lead to a variety of microstructures depending on sample geometry, heating temperature, and the ratio of gold to silicon which was found to have the largest impact on the eutectic microstructure. The eutectic morphology varied from dendrites to hollow rectangular structures to Au–Si eutectic agglomerates with increasing silicon to gold ratio.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Annealing induced microstructure engineering of antimony tri-selenide thin films

Highlights: • Deposition of Sb{sub 2}Se{sub 3} thin films using thermal vapour deposition. • Films are deposited on substrates with concurrent heating and without heating. • Effect of post deposition annealing on the two types of films are investigated. • Influence of temperature and processing conditions on optical band gap are probed. • This Sb{sub 2}Se{sub 3} films can find application in solar cells and optoelectronic devices. - Abstract: The presented work demonstrates the effect of annealing on the structural, surface morphology and optical properties of Antimony Triselenide (Sb{sub 2}Se{sub 3}) thin films deposited by thermal evaporation. Two sets of thin films of Sb{sub 2}Se{sub 3} were grown on soda lime glass (SLG) substrates by thermal evaporation with and without substrate heating. Both sets of films were then annealed at three distinct temperatures (100 °C, 200 °C and 300 °C) to study the effects of annealing on the microstructure. Analysis using XRD (X-Ray Diffraction) characterization revealed that the as-deposited films without substrate heating exhibit an amorphous nature, whereas the films grown with concurrent substrate heating are polycrystalline with orthorhombic structure. The films annealed at high temperature with concurrent substrate heating possess smooth and continuous grain morphologies. The effect of annealing was also found to have significant impact on the band gap and optical properties of the Sb{sub 2}Se{sub 3} thin films.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS1984

Frictional and morphological properties of Au-MoS2 films sputtered from a compact target

AuMoS2 films 0.02 to 1.2 microns thick were sputtered from target compacted from 5 wt % Au + 95 wt % MoS2, to investigate the frictional and morphological film growth characteristics. The gold dispersion effects in MoS2 films are of interest to increase the densitification and strengthening of the film structure. Three microstructural growth stages were identified on the nano-micro-macrostructural level. During sliding both sputtered Au-MoS2 and MoS2 films have a tendency to break within the columner region. The remaining or effective film, about 0.2 microns thick, performs the lubrication. The Au-MoS2 films displayed a lower friction coefficient with a high degree of frictional stability and less wear debris generation as compared to pure MoS2 films. The more favorable frictional characteristics of the Au-MoS2 films are attributed to the effective film thickness and the high density packed columner zone which has a reduced effect on the fragmentation of the tapered crystallites during fracture.

Spalvins, T.↗
NASA NTRS1984

Frictional and morphological properties of Au-MoS2 films sputtered from a compact target

AuMoS2 films 0.02 to 1.2 microns thick were sputtered from target compacted from 5 wt percent Au + 95 wt percent MoS2, to investigate the frictional and morphological film growth characteristics. The gold dispersion effects in MoS2 films are of interest to increase the densification and strengthening of the film structure. Three microstructural growth stages were identified on the nano-micro-macrostructural level. During sliding both sputtered Au-MoS2 and MoS2 films have a tendency to break within the columner region. The remaining or effective film, about 0.2 microns thick, performs the lubrication. The Au-MoS2 films displayed a lower friction coefficient with a high degree of frictional stability and less wear debris generation as compared to pure MoS2 films. The more favorable frictional characteristics of the Au-MoS2 films are attributed to the effective film thickness and the high density packed columner zone which has a reduced effect on the fragmentation of the tapered crystallites during fracture.

Spalvins, T.↗
NASA NTRS1984

Frictional and morphological properties of Au-MoS2 films sputtered from a compact target

AuMoS2 films 0.02 to 1.2 microns thick were sputtered from target compacted from 5 wt pct. Au + 95 wt pct. MoS2, to investigate the frictional and morphological film growth characteristics. The gold dispersion effects in MoS2 films are of interest to increase the densitification and strengthening of the film structure. Three microstructural growth stages were identified on the nano-micro-macrostructural level. During sliding both sputtered Au-MoS2 and MoS2 films have a tendency to break within the columner region. The remaining or effective film, about 0.2 microns thick, performs the lubrication. The Au-MoS2 films displayed a lower friction coefficient with a high degree of frictional stability and less wear debris generation as compared to pure MoS2 films. The more favorable frictional characteristics of the Au-MoS2 films are attributed to the effective film thickness and the high density packed columner zone which has a reduced effect on the fragmentation of the tapered crystallites during fracture.

Spalvins, T.↗
DOE OSTI2018

The influence of Mo addition on the microstructure and its thermal stability for electrodeposited Ni films

Highlights: • The effect of Mo and saccharin additions on the stability of Ni layers was studied. • Both Mo and saccharin increased the defect density and reduced the grain size. • The higher Mo content resulted in a much better thermal stability. • At the same time, saccharin addition yielded a reduced stability of nanostructures. • The electrodeposited film had a better stability than the SPD-processed counterpart. - Abstract: An investigation was conducted to study the effect of molybdenum (Mo) alloying on the grain size and lattice defect structure in nanocrystalline nickel (Ni) films processed by electrodeposition. Moreover, the influence of saccharin addition to the electrolyte bath on the microstructure of Ni-Mo layers with low and high Mo contents was studied. It was found that the higher Mo content resulted in a larger dislocation density and twin fault probability as well as a smaller grain size. The addition of saccharin to the bath resulted in a further increase in the density of both dislocations and twin faults. It was also revealed that Mo alloying improved the thermal stability of the nanostructure in Ni films while saccharin addition yielded a reduction of stability. The reasons for these opposite behaviors were discussed in detail. In addition, the defect structure and its stability in Ni-Mo layers were compared with that for fine-grained bulk samples with the same composition but processed by severe plastic deformation.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Effect of microstructural evolution on mechanical and tribological properties of Ti-doped DLC films: How was an ultralow friction obtained?

This paper examined the evolution of microstructure and its effect on the mechanical and tribological properties of ultralow friction Ti-doped diamondlike carbon (DLC) films, by adjusting the CH{sub 4}/Ar ratio under constant radio frequency discharge power and bias. The Raman, high resolution transmission electron microscopy, atomic force microscope and nanoindentation measurements consistently reveal or indicate the formation of curved graphene sheets or fullerenelike nanostructures with increasing CH{sub 4}/Ar ratio. The superior frictional performance (0.008–0.01) of Ti-DLC films can be attributed to the special microstructure related to the development of embedded fullerenelike nanostructures as a result of incorporation of TiO{sub 2} clusters. The contributing factors include high hardness and cohesion, excellent toughness, high load-bearing capacity, as well as the ultralow shear resistance transform layer and the excellent antioxidation stability brought by the doped Ti.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Ti-Nb thin films deposited by magnetron sputtering on stainless steel

Thin films of Ti-Nb alloys were deposited on AISI 316L stainless steel substrate by magnetron sputtering, and the structure, composition, morphology, and microstructure of the films were analyzed by means of x-ray diffraction (XRD), (scanning) transmission electron microscopy (TEM) coupled with energy-dispersive x-ray spectroscopy, atomic force microscopy (AFM), and x-ray photoelectron spectroscopy (XPS). Thin films of four compositions were produced: Ti{sub 85}Nb{sub 15} (Ti-26 wt. % Nb), Ti{sub 80}Nb{sub 20} (Ti-33 wt. % Nb), Ti{sub 70}Nb{sub 30} (Ti-45 wt. % Nb), and Ti{sub 60}Nb{sub 40} (Ti-56 wt. % Nb). Structural characterization by XRD indicated that only the β phase was present in the thin films and that the increase in the Nb content modified the alloy film texture. These changes in the film texture, also detected by TEM analysis, were attributed to different growth modes related to the Nb content in the alloy films. The mean grain sizes measured by AFM increased with the Nb amount (from 197 to 222 nm). XPS analysis showed a predominance of oxidized Ti and Nb on the film surfaces and an enrichment of Ti.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Highly enhanced and temporally stable field emission from MWCNTs grown on aluminum coated silicon substrate

In this work, a detailed field emission study of multi-walled carbon nanotubes (MWCNTs) grown on Si and Al coated Si substrates is reported. Morphological and microstructural studies of the films show higher entanglement of CNTs in the case of CNT/Si film as compared to CNT/Al/Si film. Raman studies show that the defect mediated peak (D) is substantially suppressed as compared to graphitic peak (G) resulting in significant reduction in I{sub D}/I{sub G} value in CNT/Al/Si film. Field emission (FE) current density of CNT/Al/Si film (∼25 mA/cm{sup 2}) is significantly higher as compared to that of CNT/Si film (∼1.6 mA/cm{sup 2}). A substantial improvement in temporal stability is also observed in CNT/Al/Si film. This enhancement in field emission current is attributed to strong adhesion between substrate and CNTs, low work function, high local field enhancement factor at the CNT tips and less entanglement of CNTs grown on Al/Si. The temporally stable CNT/Al/Si cold cathode can be a potential candidate to replace conventional electron sources in prototype devices.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Effect of sputtering pressure on microstructure and bolometric properties of Nb:TiO{sub 2−x} films for infrared image sensor applications

This study aims to investigate the influence of the sputtering pressure (P{sub S}) on Nb:TiO{sub 2−x} films to enhance the bolometric properties. A decrease in the growth rate with the sputtering pressure was perceived in amorphous Nb:TiO{sub 2−x} films. The incorporation of oxygen with P{sub S} was confirmed in an X-ray photo electron spectroscopy analysis. The electrical resistivity was increased with an increase in P{sub S} due to a decrease in the number of oxygen vacancies. The linear I-V characteristics confirmed the ohmic contact behavior between the Nb:TiO{sub 2−x} layer and the electrode material. The present investigation finds that the sample with lower resistivity has good bolometric properties with low noise and high universal bolometric parameters. Finally, the Nb:TiO{sub 2−x} sample deposited at a sputtering pressure of 2 mTorr shows better bolometric properties than other materials for infrared image sensor applications.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2015

Effect of deposition pressure on the microstructure and thermoelectric properties of epitaxial ScN(001) thin films sputtered onto MgO(001) substrates

Four epitaxial ScN(001) thin films were successfully deposited on MgO(001) substrates by dc reactive magnetron sputtering at 2, 5, 10, and 20 mTorr in an Ar/N2 ambient atmosphere at 650 °C. The microstructure of the resultant films was analyzed by x-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Electrical resistivity, electron mobility and concentration were measured using the room temperature Hall technique, and temperature dependent in-plain measurements of the thermoelectric properties of the ScN thin films were performed. The surface morphology and film crystallinity significantly degrade with increasing deposition pressure. The ScN thin film deposited at 20 mTorr exhibits the presence of <221> oriented secondary grains resulting in decreased electric properties and a low thermoelectric power factor of 0.5 W/m-K² at 800 K. ScN thin films grown at 5 and 10 mTorr are single crystalline, yielding the power factor of approximately 2.5 W/m-K² at 800 K. The deposition performed at 2 mTorr produces the highest quality ScN thin film with the electron mobility of 98 cm² V⁻¹ s⁻¹ and the power factor of 3.3 W/m-K² at 800 K.

36 MATERIALS SCIENCE↗