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At least 847 records · Page 47
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Growth and microstructure of columnar Y-doped SrZrO{sub 3} films deposited on Pt-coated MgO by pulsed laser deposition

Direct integration of proton conductor films on Pt-coated substrates opens the way to film-based proton transport devices. Columnar SrZr{sub 0.95}Y{sub 0.05}O{sub 3−δ} (SZY) films with dense microstructure were deposited on Pt-coated MgO(100) substrates at 830 °C by pulsed laser deposition. The optimal window of ambient O{sub 2} pressure for good crystallinity of SZY films is from 400 to 600 mTorr. The ambient O{sub 2} compresses the plasma plume of SZY and increases the deposition rate. The 10 nm thick Ti adhesion layer on MgO(100) greatly affects the orientation of the sputtered Pt layers. Pt deposited directly on MgO shows a highly (111)-preferred orientation and leads to preferentially oriented SZY films while the addition of a Ti adhesion layer makes Pt show a less preferential orientation that leads to randomly oriented SZY films. The RMS surface roughness of preferentially oriented SZY films is larger than that of randomly oriented SZY films deposited under the same ambient O{sub 2} pressure. As the O{sub 2} pressure increased, the RMS surface roughness of preferentially oriented SZY films increased, reaching 45.7 nm (2.61% of film thickness) at 600 mTorr. This study revealed the ambient O{sub 2} pressure and orientation dependent surface roughness of SZY films grown on Pt-coated MgO substrates, which provides the potential to control the surface microstructure of SZY films for electrochemical applications in film-based hydrogen devices.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2014

Reactive sputtering of δ-ZrH{sub 2} thin films by high power impulse magnetron sputtering and direct current magnetron sputtering

Reactive sputtering by high power impulse magnetron sputtering (HiPIMS) and direct current magnetron sputtering (DCMS) of a Zr target in Ar/H{sub 2} plasmas was employed to deposit Zr-H films on Si(100) substrates, and with H content up to 61 at. % and O contents typically below 0.2 at. % as determined by elastic recoil detection analysis. X-ray photoelectron spectroscopy reveals a chemical shift of ∼0.7 eV to higher binding energies for the Zr-H films compared to pure Zr films, consistent with a charge transfer from Zr to H in a zirconium hydride. X-ray diffraction shows that the films are single-phase δ-ZrH{sub 2} (CaF{sub 2} type structure) at H content >∼55 at. % and pole figure measurements give a 111 preferred orientation for these films. Scanning electron microscopy cross-section images show a glasslike microstructure for the HiPIMS films, while the DCMS films are columnar. Nanoindentation yield hardness values of 5.5–7 GPa for the δ-ZrH{sub 2} films that is slightly harder than the ∼5 GPa determined for Zr films and with coefficients of friction in the range of 0.12–0.18 to compare with the range of 0.4–0.6 obtained for Zr films. Wear resistance testing show that phase-pure δ-ZrH{sub 2} films deposited by HiPIMS exhibit up to 50 times lower wear rate compared to those containing a secondary Zr phase. Four-point probe measurements give resistivity values in the range of ∼100–120 μΩ cm for the δ-ZrH{sub 2} films, which is slightly higher compared to Zr films with values in the range 70–80 μΩ cm.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Effect of AC target power on AlN film quality

The influence of alternating current (AC) target power on film stress, roughness, and x-ray diffraction rocking curve full width half maximum (FWHM) was examined for AlN films deposited using S-gun magnetron sputtering on insulative substrates consisting of Si wafers with 575 nm thermal oxide. As the AC target power was increased from 5 to 8 kW, the deposition rate increased from 9.3 to 15.9 A/s, film stress decreased from 81 to −170 MPa, and the rocking curve FWHM increased from 0.98 to 1.03°. AlN film behavior is observed to change with target life; films deposited at 200 kWh target life were approximately 40 MPa more compressive and had 0.02° degree higher rocking curve FWHM values than films deposited at 130 kWh. AlN films deposited in two depositions were compared with films deposited in a single deposition, in order to better characterize the growth behavior and properties of AlN films deposited on an existing AlN film, which is not well understood. Two deposition films, when compared with single deposition films, showed no variation in residual stress trends or grain size behavior, but the average film roughness increased from 0.7 to 1.4 nm and rocking curve FWHM values increased by more than 0.25°.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Production and characterization of thin film group IIIB, IVB and rare earth hydrides by reactive evaporation

A recent short history of reactive evaporation by D. M. Mattox [History Corner—A Short History of Reactive Evaporation, SVC Bulletin (Society of Vacuum Coaters, Spring 2014), p. 50–51] describes various methods for producing oxides, nitrides, carbides, and some compounds, but hydrides were not mentioned. A study was performed in the mid-1970s at the General Electric Company Neutron Devices Department in Largo, FL, by the author to study preparation of thin film hydrides using reactive evaporation and to determine their unique characteristics and properties. Films were produced of scandium (Sc), yttrium (Y), titanium (Ti), zirconium (Zr), and the rare earth praseodymium (Pr), neodymium (Nd), gadolinium (Gd), dysprosium (Dy), and erbium (Er) hydrides by hot crucible filament and electron beam evaporation in atmospheres of deuterium and tritium gases. All-metal vacuum systems were used and those used with tritium were dedicated for this processing. Thin film test samples 1000 nm thick were prepared on 1.27 cm diameter molybdenum disk substrates for each occluder (i.e., an element that can react with hydrogen to form a hydride) material. Loading characteristics as determined by gas-to-metal atomic ratios, oxidation characteristics as determined by argon–sputter Auger analysis, film structure as determined by scanning electron microscope analysis, and film stress properties as determined by a double resonator technique were used to define properties of interest. Results showed hydrogen-to-metal atomic ratios varied from 1.5 to 2.0 with near maximum loading for all but Pr and Nd occluders which correlated with the oxidation levels observed, with all occluder oxidation levels being variable due to vacuum system internal processing conditions and the materials used. Surface oxide levels varied from ∼80 Å to over 1000 Å. For most films studied, results showed that a maximum loading ratio of near 2.0 and a minimum surface oxide level of ∼80 Å could be obtained with a bulk film oxygen level of ∼0.54 oxygen as determined by microprobe analysis when an evaporation rate of ∼0.313 mg/cm{sup 2} min was used in an atmosphere of D{sub 2} or T{sub 2} gas at a system deposition pressure of 1 × 10{sup −3 }Torr (1.33 × 10{sup −1 }Pa) in an evaporation time of ∼2 min. Platelet type (i.e., a film microstructure showing an overlay of flat plates with large grain sizes) film structures were observed for most films with some film mechanical properties determined (i.e., grain size and Vickers μ-hardness), and reduced stress levels were seen with initial normalized differential (tensile) stress levels being (1.0–4.0) × 10{sup 8 }dyne/cm{sup 2} for tritium loaded samples and (1.5 ± 0.5) × 10{sup 9 }dyne/cm{sup 2} for deuterium loaded samples. Also, stress aging characteristics were determined for some hydride films prepared in a radioactive tritium gas atmosphere. Tritium loading, however, had the undesirable characteristic of having to dispose of the internal processing system fixtures, which can be minimized, but the reactive evaporation technique produced desirable thin films.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Effect of Ag in CdSe thin films prepared using thermal evaporation

It has been a general practice to dope thin films with suitable dopants to modify the properties of the films to make them more suitable for potential applications. When the dopant concentrations are low, they do not normally affect the structure and morphology of the films. However, it may lead to drastic changes in electronic properties of the films. This might result from the dopant getting incorporated into the lattice of the material of the films. Cadmium selenide is an important compound semiconductor material with an attractive energy band gap. The present work relates to an attempt made to dope CdSe thin films with silver. CdSe:Ag (1–5%) thin films were deposited on glass substrates at an optimized substrate temperature of 453 K using thermal evaporation technique. The grown films were analyzed using X-ray diffraction, scanning electron microscopy (SEM), energy dispersive analysis of X-ray (EDX) techniques. It is observed that undoped CdSe thin films and CdSe:Ag films have hexagonal structure. The grain size was found to increase marginally with an increase in the Ag concentration. The optical band gap of the films determined by optical transmission measurements agree with that of CdSe. Electrical conductivity is observed to increase from 10{sup –4} to 3.66 (Ω cm){sup –1} on addition of silver. The variation of resistance with temperature indicates that the prepared films consist of CdSe and Ag existing as two separate phases coexisting and contributing individually to the resistivity of the films.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Real-Time Monitoring of Strain Accumulation and Relief during Epitaxy of Ultrathin Co Ferrite Films with Varied Co Content

Ultrathin Co x Fe 3-x O 4 films of high structural quality and with different Co content (x = 0.6–1.2) were prepared by reactive molecular beam epitaxy on MgO(001) substrates. Epitaxy of these ferrite films is extensively monitored by means of time-resolved (operando) X-ray diffraction recorded in out-of-plane geometry to characterize the temporal evolution of the film structure. The Co ferrite films show high crystalline ordering and smooth film interfaces independent of their Co content. All Co x Fe 3-x O 4 films exhibit enhanced compressive out-of-plane strain during the early stages of growth, which partly releases with increasing film thickness. When the Co content of the ferrite films increases, the vertical-layer distances increase, accompanied by slightly increasing film roughnesses. The latter result is supported by surface-sensitive low-energy electron diffraction as well as X-ray reflectivity measurements on the final films. In contrast, the substrate–film interface roughness decreases with increasing Co content, which is confirmed with X-ray reflectivity measurements. In addition, the composition and electronic structure of the ferrite films is characterized by means of hard X-ray photoelectron spectroscopy performed after film growth. The experiments reveal the expected increasing Fe 3+ /Fe 2+ cation ratios for a higher Co content.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Technical Note: On GAFChromic EBT-XD film and the lateral response artifact

Purpose: The new radiochromic film, GAFChromic EBT-XD, contains the same active material, lithium-10,12-pentacosadiynoate, as GAFChromic EBT3, but the crystalline form is different. This work investigates the effect of this change on the well-known lateral response artifact when EBT-XD film is digitized on a flatbed scanner. Methods: The dose response of a single production lot of EBT-XD was characterized by scanning an unexposed film plus a set of films exposed to doses between 2.5 and 50 Gy using 6 MV photons. To characterize the lateral response artifact, the authors used the unexposed film plus a subset of samples exposed to doses between 20 and 50 Gy. Digital images of these films were acquired at seven discrete lateral locations perpendicular to the scan direction on three Epson 10000XL scanners. Using measurements at the discrete lateral positions, the scanner responses were determined as a function of the lateral position of the film. From the data for each scanner, a set of coefficients were derived whereby measured response values could be corrected to remove the effects of the lateral response artifact. The EBT-XD data were analyzed as in their previous work and compared to results reported for EBT3 in that paper. Results: For films scanned in the same orientation and having equal responses, the authors found that the lateral response artifact for EBT-XD and EBT3 films was remarkably similar. For both films, the artifact increases with increased net response. However, as EBT-XD is less sensitive than EBT3, a greater exposure dose is required to reach the same net response. On this basis, the lower sensitivity of EBT-XD relative to EBT3 results in less net response change for equal exposure and a reduction in the impact of the lateral response artifact. Conclusions: The shape of the crystalline active component in EBT-XD and EBT3 does not affect the fundamental existence of the lateral response artifact when the films are digitized on flatbed scanners. Owing its lower sensitivity, EBT-XD film requires higher dose to reach the same response as EBT3, resulting in lesser impact of the lateral response artifact. For doses >10 Gy, the slopes of the EBT-XD red and green channel dose response curves are greater than the corresponding ones for EBT3. For these two reasons, the authors prefer EBT-XD for doses exceeding about 10 Gy.

61 RADIATION PROTECTION AND DOSIMETRY↗
DOE OSTI2015

Nanomechanical properties of platinum thin films synthesized by atomic layer deposition

The nanomechanical properties of Pt thin films grown on Si (100) using atomic layer deposition (ALD) were investigated using nanoindentation. Recently, atomic layer deposition (ALD) has successfully demonstrated the capability to deposit ultra-thin films of platinum (Pt). Using (methylcyclopentadienyl) trimethylplatinum (MeCpPtMe3) as chemical platinum precursor and oxygen (O2) as the oxidizing agent, the ALD synthesis of Pt can be achieved with high conformity and excellent film uniformity. The ALD process window for Pt films was experimentally established in the temperature range between 270 °C and 320 °C, where the sheet conductance was constant over that temperature range, indicating stable ALD Pt film growth rate. ALD growth of Pt films exhibits very poor nucleation and adhesion characteristics on bare Si surfaces when the native oxide was removed by 2% HF etch. Pt adhesion improves for thermally oxidized Si wafers and for Si wafers covered with native oxide. Three ALD Pt films deposited at 800, 900, and 1000 ALD deposition cycles were tested for the structural and mechanical properties. Additionally, the sample with 900 ALD deposition cycles was further annealed in forming gas (95% N2 and 5% H2) at 450 °C for 30 min in order to passivate dangling bonds in the grain boundaries of the polycrystalline Pt film. Cross-sectional transmission electron microscopy (TEM), X-ray diffraction (XRD), atomic force microscopy (AFM), and scanning electron microscope (SEM) were employed to characterize the films' surface structure and morphology. Nanoindentation technique was used to evaluate the hardness and modulus of the ALD Pt films of various film thicknesses. The results indicate that the films depict comparable hardness and modulus results; however, the 800 and 1000 ALD deposition cycles films without forming gas annealing experienced significant amount of pileup, whereas the 900 ALD deposition cycles sample annealed in forming gas resulted in a smaller pileup.

Mamun, M.A.↗
NASA NTRS1992

Molecular films associated with LDEF

The molecular films deposited on the surface of the Long Duration Exposure Facility (LDEF) originated from the paints and room-temperature-vulcanized (RTV) silicone materials intentionally used on the satellite and not from residual contaminants. The high silicone content of most of the films and the uniformity of the films indicates a homogenization process in the molecular deposition and suggests a chemically most favored composition for the final film. The deposition on interior surfaces and vents indicated multiple bounce trajectories or repeated deposition-reemission cycles. Exterior surface deposits indicated a significant return flux. Ultraviolet light exposure was required to fix the deposited film as is indicated by the distribution of the films on interior surfaces and the thickness of films at the vent locations. Thermal conditions at the time of exposure to ultraviolet light seems to be an important factor in the thickness of the deposit. Sunrise facing (ram direction) surfaces always had the thicker film. These were the coldest surfaces at the time of their exposure to ultraviolet light. The films have a layered structure suggesting cyclic deposition. As many as 34 distinct layers were seen in the films. The cyclic nature of the deposition and the chemical uniformity of the film one layer to the next suggest an early deposition of the films though there is evidence for the deposition of molecular films throughout the nearly six year exposure of the satellite. A final 'spray' of an organic material associated with water soluble salts occurred very late in the mission. This may have been the result of one of the shuttle dump activities.

Crutcher, E. R.↗
NASA NTRS2003

Experiments on the Flow of a Thin Liquid Film Over a Horizontal Stationary and Rotating Disk Surface

Experiments on characterization of thin liquid films flowing over stationary and rotating disk surfaces are described. The thin liquid film was created by introducing deionized water from a flow collar at the center of an aluminum disk with a known initial film thickness and uniform radial velocity. Radial film thickness distribution was measured using a non-intrusive laser light interface reflection technique that enabled the measurement of the instantaneous film thickness over a finite segment of the disk. Experiments were performed for a range of flow rates between 3.01pm and 15.01pm, corresponding to Reynolds numbers based on the liquid inlet gap height and velocity between 238 and 1,188. The angular speed of the disk was varied from 0 rpm to 300 rpm. When the disk was stationary, a circular hydraulic jump was present in the liquid film. The liquid-film thickness in the subcritical region (down-stream of the hydraulic jump) was an order of magnitude greater than that in the supercritical region (upstream of the hydraulic jump) which was of the order of 0.3 mm. As the Reynolds number increased, the hydraulic jump migrated toward the edge of the disk. In the case of rotation, the liquid-film thickness exhibited a maximum on the disk surface. The liquid-film inertia and friction influenced the inner region where the film thickness progressively increased. The outer region where the film thickness decreased was primarily affected by the centrifugal forces. A flow visualization study of the thin film was also performed to determine the characteristics of the waves on the free surface. At high rotational speeds, spiral waves were observed on the liquid film. It was also determined that the angle of the waves which form on the liquid surface was a function of the ratio of local radial to tangential velocity.

Ozar, B.↗
NASA NTRS2003

Collaboration of the NASA Glenn Research Center and Rolls-Royce Developed Thin Film Multilayered Dielectrics for Harsh Environments

The use of thin films to electrically insulate thin film sensors on engine components minimizes the intrusiveness of the sensors and allows a more accurate measurement of the environment. A variety of insulating films were investigated for preventing electrical shorting caused by insulator failure between the sensor and the component. By alternating layers of sputtered high-temperature ceramics, a sequence of insulating layers was devised that (1) prevents pinholes from forming completely through the insulator and (2) maintains high electrical resistivity at high temperatures. The total thickness is only a fraction of that needed for conventional insulating techniques. The Sensors and Electronics Technology Branch of the NASA Glenn Research Center has an in-house effort to develop thin film sensors for surface measurement in propulsion system research. Thin film sensors do not require special machining of the components on which they are mounted, and they are considerably thinner (less than 10 mm thick) than wire or foil sensors. The thin film sensors are thus much less disturbing to the operating environment and have a minimal impact on the physical characteristics of the supporting component. To further this research, NASA Glenn and Rolls-Royce (Derby, UK), with assistance from the Ohio Aerospace Institute (OAI) and the Akima Corporation, pursued a joint investigation using multilayered thin film dielectrics as a reliable insulator in harsh environments. The use of a multilayered scheme is thought to be promising for the fabrication of electrically insulating thin films. A major cause of conduction in thin film dielectrics is the presence of defects, such as pinholes, that propagate through the film to the underlying substrate surface. By alternating the insulating material, each new growth pattern would deviate from the previous one, eliminating direct pathways for conduction to the substrate. The film depositions and testing were conducted in the Instrument Research Laboratory at Glenn. The multilayered insulator test samples were made from alumina and stainless steel shims that were first covered with a sputtered underlayer of either yttria-stabilized zirconia or chromium carbide, and then overcoated with a sputtered top layer of alumina. An example of a test sample is shown in the following photograph. Each multilayered insulator sample was 5 mm thick, at least an order of magnitude thinner than conventional insulators. The insulating properties of the samples were tested in a high-temperature air oven to determine their suitability. The multilayer insulators tested showed a stabilized film at temperatures in excess of 800 C (1472 F). The underlying materials in these multilayers allow thermal expansion stresses produced during the heating to be graded. The chromium carbide-alumina multilayer had the best adhesion at high temperatures, presumably from the induced chemical bonding between the substrate and the chromium carbide underlayer. However, the zirconia-alumina multilayer proved to have slightly better insulating properties when adhering. The application of the zirconia-alumina insulator has been demonstrated on a nickel-alloy fan blade, as shown. The insulators using thin film sensors still need to be tested in a relevant high-temperature combustion environment.

Wrbanek, John D.↗
DOE OSTI2018

Study of Electrical Transport and Magnetic Properties of Nd{sub 0.7}Sr{sub 0.3}MnO{sub 3}/Nd{sub 0.8}Na{sub 0.2}MnO{sub 3} Bilayer Thin Films

Bilayer films of Nd{sub 0.7}Sr{sub 0.3}MnO{sub 3}/Nd{sub 0.8}Na{sub 0.2} MnO{sub 3} were grown on 001-orientated LaAlO{sub 3} substrate by using RF magnetron sputtering. The thickness of the Nd{sub 0.8}Na{sub 0.2}MnO{sub 3} (NNMO) film was kept fixed at 120 nm while that of the Nd{sub 0.7}Sr{sub 0.3}MnO{sub 3} (NSMO) film was varied from 12 to 100 nm. X-ray diffraction patterns confirm the growth of films along the (001) direction, and the out-of-plane lattice constant of the NSMO film decreases with an increase in film thickness. The bilayer films are found to undergo out-of-plane tensile strain, and the lattice strain is found to decrease with an increase in film thickness. The ferromagnetic transition temperature is found to increase with an increase in the NSMO film thickness. M–H loops recorded at 50 K show a systematic increase in saturation magnetisation with an increase in film thickness. Metal–insulator transition has been observed for the film thickness of 30 nm and above, and the transition temperature is found to increase with an increase in film thickness. The electrical resistivity data in the metallic region were explained based on electron–electron and electron–magnon scattering mechanism by including a weak localisation effect at low temperature. The electrical resistivity data in the insulating region follow the Mott-variable range hopping model.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Tuning of Magnetic and Optical Properties of Co{sub 0.8}Zn{sub 0.2}Fe{sub 2}O{sub 4} Spinel Ferrite Thin Films Based on Post Annealing Temperature

This paper is dedicated to deposit zinc substituted cobalt ferrite (Co{sub 0.8}Zn{sub 0.2}Fe{sub 2}O{sub 4}) thin films on glass substrate using electron beam deposition technique. The effect of post annealing temperature on structural, magnetic, and optical properties of thin films has been investigated. Thin films have been characterized using x-ray diffraction (XRD), Raman spectroscopy, atomic force microscopy (AFM), vibrating sample magnetometer (VSM), UV-VIS spectroscopy, and spectroscopic ellipsometry (SE) analysis. The as-deposited thin films are amorphous in nature. After deposition, these thin films post annealed at different temperature ranges from 200 to 500 {sup ∘}C to enhance the crystallinity of films. The film post annealed at 200 {sup ∘}C is also amorphous in nature. As the post annealing temperature increases, the thin films become more crystalline. X-ray diffractometer and Raman analysis confirm the formation of cubical inverse spinel structure of thin films. The saturation magnetization of the thin films decreases with the annealing temperature due to the sites occupancy of cations between tetrahedral and octahedral. The reduction in coercivity is correlated with the anisotropy constant, but the anisotropy value is still high which is suitable to form stable magnetic storage memories. The band gap energy are decreased which is mainly attributed due to increase in grain size of the film. It is noted that the band gap energy of these thin films are higher than that of bulk material, so these may be suggested for use in wide band gap applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Effect of RF Power on Structural, Magnetic, and Optical Properties of CoFe{sub 2}O{sub 4} Thin Films

The thin films of CoFe{sub 2}O{sub 4} were deposited on glass substrates by radio-frequency (RF) sputtering. The effect of RF power variation from 60–120 W on the structure, magnetic, and optical properties of the as-deposited films and films annealed at 500 °C was studied. The magnetic parameters of the film, i.e., in-plane coercivity (H{sub c}), saturation magnetization (M{sub s}), and remanence (M{sub r}) increase as RF power is increased from 60 to 80 W followed by a decreasing trend with further increase in RF power to 120 W. Annealing of the film significantly improves the magnetic properties. The largest grain size and the best crystallinity of the film are obtained for the film deposited at 80 W of RF power. The thin films exhibited 70–80% optical transmittance. Optical band gap (E{sub g}) depends on the RF power and grain size, and it varies between 2.08 and 2.16 eV for the as-deposited films and between 2.16 and 2.30 eV for the annealed films. The study shows that RF power used for depositing the film has strong effect on the microstructure and properties of the film.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Microstructural dependence of defect formation in iron-oxide thin films

In this report passivating iron-oxide films are grown atop iron films simulating the corrosion process in a nuclear reactor environment. Two oxide films grown via physical vapor deposition at 600 °C and room temperature exhibited dense-epitactic and columnar-polycrystalline, microstructures respectively. A third oxide film grown in open air at 600 °C exhibited an eqiuaxed, porous morphology. Cubic maghemite and magnetite phases in each oxide film were identified via grazing incidence X-ray diffraction. Positron annihilation spectroscopy was used to characterize point defects and measure their depth and size distributions in each oxide layer and showed a range of average positron lifetimes from 0.23 ns in the high temperature, vapor deposited film, 0.35 ns in the room temperature-grown film, and 0.31 ns in the thermally grown oxide. These data indicate that the film morphology, which varies greatly in these films, leads to very different defect content. Finally, four-dimensional scanning transmission electron microscopy was used to measure the internal stress of each film and was correlated to the strain state presented in the X-ray diffraction spectra. The defect formation in each film is reasoned through using a thin film growth model.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Magnetron sputtered nanostructured cadmium oxide films for ammonia sensing

Nanostructured cadmium oxide (CdO) films were deposited on to glass substrates by reactive dc magnetron sputtering technique. The depositions were carried out for different deposition times in order to obtain films with varying thicknesses. The CdO films were polycrystalline in nature with cubic structure showing preferred orientation in (1 1 1) direction as observed by X-ray diffraction (XRD). Field-emission scanning electron microscope (FE-SEM) micrographs showed uniform distribution of grains of 30–35 nm size and change in morphology from spherical to elliptical structures upon increasing the film thickness. The optical band gap value of the CdO films decreased from 2.67 to 2.36 eV with increase in the thickness. CdO films were deposited on to interdigitated electrodes to be employed as ammonia (NH{sub 3}) gas sensor. The fabricated CdO sensor with thickness of 294 nm has a capacity to detect NH{sub 3} as low as 50 ppm at a relatively low operating temperature of 150 °C with quick response and recovery time. - Highlights: • Nanostructured CdO films were deposited on to glass substrates using magnetron sputtering. • Deposition time was varied in order to obtain films with different thicknesses. • The CdO films were polycrystalline in nature with preferred orientation along (1 1 1) direction. • The optical bandgap values of the films decreased on increasing the thickness of the films. • CdO films with different thickness such as 122, 204, 294 nm was capable to detect NH{sub 3} down to 50 ppm at operating temperature of 150 °C.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Large-scale fabrication of linear low density polyethylene/layered double hydroxides composite films with enhanced heat retention, thermal, mechanical, optical and water vapor barrier properties

Novel LDH intercalated with organic aliphatic long-chain anion was large-scale synthesized innovatively by high-energy ball milling in one pot. The linear low density polyethylene (LLDPE)/layered double hydroxides (LDH) composite films with enhanced heat retention, thermal, mechanical, optical and water vapor barrier properties were fabricated by melt blending and blowing process. FT IR, XRD, SEM results show that LDH particles were dispersed uniformly in the LLDPE composite films. Particularly, LLDPE composite film with 1% LDH exhibited the optimal performance among all the composite films with a 60.36% enhancement in the water vapor barrier property and a 45.73 °C increase in the temperature of maximum mass loss rate compared with pure LLDPE film. Furthermore, the improved infrared absorbance (1180–914 cm{sup −1}) of LLDPE/LDH films revealed the significant enhancement of heat retention. Therefore, this study prompts the application of LLDPE/LDH films as agricultural films with superior heat retention. - Graphical abstract: The fabrication process of LLDPE/LDH composite films. - Highlights: • LDH with basal spacing of 4.07 nm was synthesized by high-energy ball milling. • LLDPE composite films with homogeneous LDH dispersion were fabricated. • The properties of LLDPE/LDH composite films were improved. • LLDPE/LDH composite films show superior heat retention property.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Preparation and characterization of RF magnetron sputtered CuO/CaTi{sub 4}O{sub 9} thin films with enhanced third-order nonlinear optical properties

The titanate, is a material of interest for various energy applications, including photovoltaics, catalysts, and high-rate energy storage devices. Herein, its related materials, CuO/CaTi{sub 4}O{sub 9} [CCTO] thin films, were successfully fabricated on SrTiO{sub 3} (100) substrates by RF magnetron sputtering assisted with subsequent oxygen annealing. This obtained CCTO thin films were then systemically studied by X-ray powder diffraction (XRD), atomic force microscopy (AFM), scan electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and high-resolution transmission electron microscopy (HRTEM). It was found that CuO and CaTi{sub 4}O{sub 9} (001) particles were closely accumulated together on the surface of the substrate in the annealing process after comparing with that of the as-prepared thin film, which was verified by SEM and AFM results. Furthermore, we investigated the third-order nonlinear optical (NLO) properties of the as-prepared and annealed CCTO thin film by means of the Z-scan technique using 650 nm femtosecond laser pulse. Post-deposition oxygen annealing was found to modify the morphological characteristics of the films, resulting in enhancing their NLO properties. The observation of NLO performance of annealed CCTO thin film indicates that RF magnetron sputtering is a feasible method for the fabrication of optical thin films, which can be expanded to fabricate other NLO materials from the corresponding dispersions. Naturally, we concluded that the CCTO thin film occupy a better NLO property, and thus enlarge its application in nonlinear optics. - Highlights: • The CCTO thin film was prepared using the RF magnetron sputtering and oxygen annealing. • The film was prepared on the SrTiO{sub 3}(100) substrates with a Ca{sub 2}CuO{sub 3} target. • The oxygen annealing was found can effectively enhance the film quality and NLO property. • The film was characterized using XPS, SEM, AFM, TEM, XRD and Z-scan techniques.

36 MATERIALS SCIENCE↗