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At least 1,171 records · Page 65
All sourcesNASA NTRSDOE OSTI
NASA NTRS1990

Study of diamond film growth and properties

The objective was to study diamond film growth and its properties in order to enhance the laser damage threshold of substrate materials. Calculations were performed to evaluate laser induced thermal stress parameter, R(sub T) of diamond. It is found that diamond has several orders of magnitude higher in value for R(sub T) compared to other materials. Thus, the laser induced damage threshold (LIDT) of diamond is much higher. Diamond films were grown using a microwave plasma enhanced chemical vapor deposition (MPECVD) system at various conditions of gas composition, pressure, temperature, and substrate materials. A 0.5 percent CH4 in H2 at 20 torr were ideal conditions for growing of high quality diamond films on substrates maintained at 900 C. The diamond films were polycrystalline which were characterized by scanning electron microscopy (SEM) and Raman scattering spectroscopy. The top surface of the growing film is always rough due to the facets of polycrystalline film while the back surface of the film replicates the substrate surface. An analytical model based on two dimensional periodic heat flow was developed to calculate the effective in-plane (face parallel) diffusivity of a two layer system. The effective diffusivity of diamond/silicon samples was measured using a laser pulse technique. The thermal conductivity of the films was measured to be 13.5 W/cm K, which is better than that of a type Ia natural diamond. Laser induced damage experiments were performed on bare Si substrates, diamond film coated Si, and diamond film windows. Significant improvements in the LIDT were obtained for diamond film coated Si compared to the bare Si.

Albin, Sacharial↗
NASA NTRS1991

Synthesis and superconducting properties of Tl-Ba-Ca-Cu-O films

Tl-Ba-Ca-Cu-O superconducting films were synthesized by sputtering either from a single target or from two oxide targets in a symmetric configuration. Films with zero resistance Tc of up to 122 K were obtained after various postannealing treatments at 870-950 C under an oxygen atmosphere. The composition of the films is not very homogeneous on the submicrometer scale. The critical current of these films at 77 K is in the 1000 A/sq cm to 10,000 A/sq cm range, which is much smaller than that of films prepared on SrTiO3 and LaAlO3 substrates. The low critical current density in these films is probably due to the granularity in the films. The morphology, structure, and magnetic and superconducting properties of the films were studied. Films prepared by two different sputtering techniques have similar results which depend mostly on the film compositions and their annealing conditions. It is found that the induced magnetic flux in the film decreases rapidly with increasing temperature, indicating weak flux pinning.

Liou, S. H.↗
NASA NTRS1996

The Effect of Wake Passing on Turbine Blade Film Cooling

The effect of upstream blade row wake passing on the showerhead film cooling performance of a downstream turbine blade has been investigated through a combination of experimental and computational studies. The experiments were performed in a steady-flow annular turbine cascade facility equipped with an upstream rotating row of cylindrical rods to produce a periodic wake field similar to that found in an actual turbine. Spanwise, chordwise, and temporal resolution of the blade surface temperature were achieved through the use of an array of nickel thin-film surface gauges covering one unit cell of showerhead film hole pattern. Film effectiveness and Nusselt number values were determined for a test matrix of various injectants, injectant blowing ratios, and wake Strouhal numbers. Results indicated a demonstratable reduction in film effectiveness with increasing Strouhal number, as well as the expected increase in film effectiveness with blowing ratio. An equation was developed to correlate the span-average film effectiveness data. The primary effect of wake unsteadiness was found to be correlated well by a chordwise-constant decrement of 0.094-St. Measurable spanwise film effectiveness variations were found near the showerhead region, but meaningful unsteady variations and downstream spanwise variations were not found. Nusselt numbers were less sensitive to wake and injection changes. Computations were performed using a three-dimensional turbulent Navier-Stokes code which was modified to model wake passing and film cooling. Unsteady computations were found to agree well with steady computations provided the proper time-average blowing ratio and pressure/suction surface flow split are matched. The remaining differences were isolated to be due to the enhanced mixing in the unsteady solution caused by the wake sweeping normally on the pressure surface. Steady computations were found to be in excellent agreement with experimental Nusselt numbers, but to overpredict experimental film effectiveness values. This is likely due to the inability to match actual hole exit velocity profiles and the absence of a credible turbulence model for film cooling.

Heidmann, James David↗
NASA NTRS1996

Friction and Wear Properties of As-Deposited and Carbon Ion-Implanted Diamond Films

Recent work on the friction and wear properties of as-deposited and carbon ion-implanted diamond films was reviewed. Diamond films were produced by the microwave plasma chemical vapor deposition (CVD) technique. Diamond films with various grain sizes and surface roughnesses were implanted with carbon ions at 60 keV ion energy, resulting in a dose of 1.2 x 10(exp 17) carbon ions per cm(exp 2). Various analytical techniques, including Raman spectroscopy, proton recoil analysis, Rutherford backscattering, transmission and scanning electron microscopy, X-ray photoelectron spectroscopy, and X-ray diffraction, were utilized to characterize the diamond films. Sliding friction experiments were conducted with a polished natural diamond pin in contact with diamond films in the three environments: humid air (40% relative humidity), dry nitrogen (less than 1 percent relative humidity), and ultrahigh vacuum (10(exp -7) Pa). The CVD diamond films indeed have friction and wear properties similar to those of natural diamond in the three environments. The as-deposited, fine-grain diamond films can be effectively used as self-lubricating, wear-resistant coatings that have low coefficients of friction (0.02 to 0.04) and low wear rates (10(exp -7) to lO(exp -8) mm(exp 3) N(exp -1) m(exp -1)) in both humid air and dry nitrogen. However, they have high coefficients of friction (1.5 to 1.7) and a high wear rate (10(exp -4) mm(exp 7) N(exp -1) m(exp -1)) in ultrahigh vacuum. The carbon ion implantation produced a thin surficial layer (less than 0.1 micron thick) of amorphous, non-diamond carbon on the diamond films. In humid air and dry nitrogen, the ion-implanted, fine and coarse-grain diamond films have a low coefficient of friction (around 0.1) and a low wear rate (10(exp -7) mm(exp 3) N(exp -1) m(exp-1)). Even in ultrahigh vacuum, the presence of the non-diamond carbon layer reduced the coefficient of friction of fine-grain diamond films to 0.1 or lower and the wear rate to 10(exp -6) mm(exp 3) N(exp -1) m(exp -1). Thus, the carbon ion-implanted, fine-grain diamond films can be effectively used as wear-resistant, self-lubricating coatings not only in air and dry nitrogen, but also in ultrahigh vacuum.

Miyoshi, Kazuhisa↗
NASA NTRS2004

CuInS2 Films Deposited by Aerosol-Assisted Chemical Vapor Deposition Using Ternary Single-Source Precursors

Polycrystalline CuInS2 films were deposited by aerosol-assisted chemical vapor deposition using both solid and liquid ternary single-source precursors (SSPs) prepared in-house. Films with either (112) or (204/220) preferred orientation were obtained, and compositional analysis showed that (112)-oriented films contained more copper than (204/220)-oriented films. Using X-ray diffraction, the signature of chalcopyrite structure was often confirmed for (112)-oriented films. The preferred orientation of the film is likely related to the decomposition and reaction kinetics associated with the molecular structure of the precursors at the substrate. Interestingly, the (204/220)-oriented films were always accompanied by a secondary phase, which was identified as an unknown In-rich compound from the results of post-growth annealing, etching experiments, and Raman spectroscopic data. By increasing Cu to In ratio in the film, (112)-oriented films were obtained with a maximum grain size of about 0.5 micrometers, and their X-ray diffractions did not show any observable signature of the In secondary phase. Electrical and optical properties of all the films grown were characterized. They all showed p-type conduction with an electrical resistivity between 0.1 omega cm and 30 omega cm, and an optical band gap of 1.46eV +/- 0.02, as deposited. The material properties of deposited films revealed this methodology of using SSPs for fabricating chalcopyrite-based solar cells to be highly promising.

Jin, Michael H.-C.↗
NASA NTRS2005

Film Delivery Module For Fiber Placement Fabrication of Hybridized Composite Structures

A new fabrication technology has been developed at the NASA Marshall Space Flight Center that will allow for the fabrication of hybridized composite structures using fiber placement processing. This technology was originally developed in response to a need to address the issue of hydrogen permeation and microcracking in cryogenic propellant tanks. Numerous thin polymeric and metallized films were investigated under low temperatures conditions for use as barrier films in a composite tank. Manufacturing studies conducted at that time did not address the processing issues related to fabrication of a hybridized tank wall. A film processing head was developed that will allow for the processing of thin polymeric and metallized films, metallic foils, and adhesives using fiber placement processing machinery. The film head is designed to enable the simultaneous processing of film materials and composite tape/tow during the composite part layup process and is also capable of processing the film during an independent operation. Several initial demonstrations were conducted to assess the performance of the film module device. Such assessments included film strip lay-up accuracy, capability to fabricate panels having internal film liners, and fabrication of laminates with embedded film layers.

Hulcher, Anthony Bruce↗
DOE OSTI2011

Neutron Reflectometry and QCM-D Study of the Interaction of Cellulase Enzymes with Films of Amorphous Cellulose

Improving the efficiency of enzymatic hydrolysis of cellulose is one of the key technological hurdles to reduce the cost of producing ethanol and other transportation fuels from lignocellulosic material. A better understanding of how soluble enzymes interact with insoluble cellulose will aid in the design of more efficient enzyme systems. We report a study involving neutron reflectometry (NR) and quartz crystal microbalance with dissipation (QCM-D) of the interaction of a commercial fungal enzyme extract (T. viride), two purified endoglucanses from thermophilic bacteria (Cel9A from A. acidocaldarius and Cel5A from T. maritima), and a mesophilic fungal endoglucanase (Cel45A from H. insolens) with amorphous cellulose films. The use of amorphous cellulose is motivated by the promise of ionic liquid pretreatment as a second generation technology that disrupts the native crystalline structure of cellulose. NR reveals the profile of water through the film at nm resolution, while QCM-D provides changes in mass and film stiffness. At 20 oC and 0.3 mg/ml, the T. viride cocktail rapidly digested the entire film, beginning from the surface followed by activity throughout the bulk of the film. For similar conditions, Cel9A and Cel5A were active for only a short period of time and only at the surface of the film, with Cel9A releasing 40 from the ~ 700 film and Cel5A resulting in only a slight roughening/swelling effect at the surface. Subsequent elevation of the temperature to the Topt in each case resulted in a very limited increase in activity, corresponding to the loss of an additional 60 from the film for Cel9A and 20 from the film for Cel5A, and very weak penetration into and digestion within the bulk of the film, before the activity again ceased. The results for Cel9A and Cel5A contrast sharply with results for Cel45A where very rapid and extensive penetration and digestion within the bulk of the film was observed at 20 C. We speculate that the large differences are due to the use of the thermophilic enzymes far below their optimal temperatures and also the presence of a cellulose binding module (CBM) on Cel45A while the thermophilic enzymes lack a CBM.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2012

Prototyping and Development of Commercial Nanocrystalline and Thin Film Silicon for Photovoltaic Manufacturing

The College of Nanoscale Science and Engineering (CNSE) at the University at Albany received funding from the Department of Energy for its proposal Prototyping and Development of Commercial Nanocrystalline and Thin Film Si for Photovoltaic Manufacturing. This project was created to identify growth rate, texture uniformity, process window, economics, composition and thickness uniformity solutions related to fabricating large area, high efficiency thin film silicon based solar cells. This document serves as a final report for the closure of this program and details the deliverables from CNSE against its original scope of work. Thin-film silicon solar cells are a promising candidate for electricity generation applications because of a combination of advantages. Nanocrystalline and poly-Si based thin films, reduces the use of expensive semiconductor material content, can be deposited onto a foreign substrate (e.g. glass or flexible stainless steel) and enables use of the cells in wide variety of applications. In addition, nano and poly-Si films have higher carrier mobility as well as reduce recombination effects, relative to traditional amorphous-silicon films. They can be mass-produced at low cost, and expected to have a strong position in the international photovoltaic industry, which is experiencing a compounded annual growth of 25%. The objectives included: Demonstration of high rate VHF (Very High Frequency) growth of nc-Si over large areas with uniform thickness. Demonstration of single chamber device growth that allows mass production processing. Demonstration of uniform segmented electrodes. Development of computer models to accelerate efforts. Demonstration of large grain thin film polycrystalline silicon films fabrication. Utilizing the AIC (Aluminum Induced Crystallization) process for large grain silicon film fabrication. Demonstration of 12% efficient nanocrystalline and polycrystalline thin film devices. The end result expected was the production of high-efficiency, low-cost thin film Si devices with reduced cost per watt, allowing dramatically increased market penetration. While further research is required to meet these ultimate goals, this project proved its feasibility.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2010

Preparation of ZnO:CeO{sub 2-x} thin films by AP-MOCVD: Structural and optical properties

The growth of columnar CeO{sub 2}, ZnO and ZnO:CeO{sub 2-x} films on quartz and AA6066 aluminum alloy substrates by economic atmospheric pressure metal-organic chemical vapor deposition (AP-MOCVD) is reported. A novel and efficient combination of metal acetylacetonate precursors as well as mild operating conditions were used in the deposition process. The correlation among crystallinity, surface morphology and optical properties of the as-prepared films was analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), transmission electron microscopy (TEM) and UV-vis spectroscopy. The synthesized films showed different crystallographic orientations depending on the ZnO and CeO{sub 2} lattice mismatch, cerium content and growth rate. The CeO{sub 2} films synthesized in this work showed plate-like compact structures as a result of the growth process typical of CVD. Both pure and ZnO:CeO{sub 2-x} films were obtained with a hexagonal structure and highly preferred orientation with the c-axis perpendicular to both substrates under the optimal deposition conditions. The microstructure was modified from dense, short round columns to round structures with cavities ('rose-flower-like' structures) and the typical ZnO morphology by controlling the cerium doping the film and substrate nature. High optical transmittance (>87%) was observed in the pure ZnO films. As for the ZnO:CeO{sub 2-x} films, the optical transmission was decreased and the UV absorption increased, which subsequently was affected by an increase in cerium content. This paper assesses the feasibility of using ZnO:CeO{sub 2-x} thin films as UV-absorbers in industrial applications. - Graphical abstract: TEM micrographs and their corresponding SAED pattern obtained for the as-deposited ZnO-CeO{sub 2-x} thin films for a Zn/Ce metallic ratio 16:9.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2012

Effect of processor temperature on film dosimetry

Optical density (OD) of a radiographic film plays an important role in radiation dosimetry, which depends on various parameters, including beam energy, depth, field size, film batch, dose, dose rate, air film interface, postexposure processing time, and temperature of the processor. Most of these parameters have been studied for Kodak XV and extended dose range (EDR) films used in radiation oncology. There is very limited information on processor temperature, which is investigated in this study. Multiple XV and EDR films were exposed in the reference condition (d{sub max.}, 10 Multiplication-Sign 10 cm{sup 2}, 100 cm) to a given dose. An automatic film processor (X-Omat 5000) was used for processing films. The temperature of the processor was adjusted manually with increasing temperature. At each temperature, a set of films was processed to evaluate OD at a given dose. For both films, OD is a linear function of processor temperature in the range of 29.4-40.6 Degree-Sign C (85-105 Degree-Sign F) for various dose ranges. The changes in processor temperature are directly related to the dose by a quadratic function. A simple linear equation is provided for the changes in OD vs. processor temperature, which could be used for correcting dose in radiation dosimetry when film is used.

61 RADIATION PROTECTION AND DOSIMETRY↗
DOE OSTI2021

Correlation of the Structure with Performance in MEH-PPV/dPS Thin Films Illuminated during Processing

Thin films containing conjugated polymers have been used in a wide array of optoelectronic devices, and much research has focused on the conformation of the conjugated polymer as a key aspect to tuning the performance of the resulting devices. White light exposure has been studied as a post-processing method to alter the film’s morphology and photoluminescence (PL) in systems composed of poly[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylenevinylene] (MEH-PPV) and polystyrene (PS). To date, there have been few studies that correlate the changes in the depth profile with the PL performance of MEH-PPV/PS films. This study is designed to address this gap in knowledge. Thin films of MEH-PPV/dPS annealed above the glass transition temperatures (T g ) in an illuminated environment led to lower PL than that found in annealed samples that are not illuminated. However, at higher MEH-PPV loading in the blend film, the extent of variation of PL with illumination diminished. Additionally, time-of-flight secondary ion mass spectrometry and small-angle neutron scattering document the three-dimensional morphology of the films under illumination conditions, which are correlated with the changes in PL. Illumination during annealing compressed MEH-PPV-rich layers in the thin film blends at low loadings of MEH-PPV (below 10 wt %) but resulted in significant in-plane phase separation at higher loadings (above 15 wt %). Both changes increase interchain interactions and lower the PL of the illuminated samples. The changes in the depth profile significantly alter the PL of the films, while the in-plane phase separation affected the optoelectronic properties to a lesser degree. This work, therefore, provides insights into how illumination and film composition can be utilized to predictably alter the structure and optoelectronic performance of conjugated polymer blend films.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Correlation between surface chemistry, density and band gap in nanocrystalline WO3 thin films

Nanocrystalline WO3 thin films were produced by sputter-deposition by varying the ratio of argon to oxygen in the reactive gas mixture during deposition. The surface chemistry, physical characteristics, and optical properties of nanocrystalline WO3 films were evaluated using X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray reflectivity (XRR), and spectrophotometric measurements. The effect of ultra-microstructure was significant on the optical properties of WO3 films. The XPS analyses indicate the formation of stoichiometric WO3 with tungsten existing in fully oxidized valence state (W6+). However, WO3 films grown at high oxygen concentration (>60%) in the sputtering gas mixture were over stoichiometric with excess oxygen. XRR simulations, which are based on isotropic WO3 film - SiO2 interface - Si substrate model, indicate that the density of WO3 films is sensitive to the oxygen content in the sputtering gas. The spectral transmission of the films increased with the increasing oxygen. The band gap of these films increases from 2.78 eV to 3.25 eV with increasing oxygen. A direct correlation between the film-density and band gap in nanocrystalline WO3 films is established based on the observed results.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Empirical assessment of a prismatic daylight-redirecting window film in a full-scale office testbed

Daylight redirecting systems with vertical windows have the potential to offset lighting energy use in deep perimeter zones. Microstructured prismatic window films can be manufactured using low-cost, roll-to-roll fabrication methods and adhered to the inside surface of existing windows as a retrofit measure or installed as a replacement insulating glass unit in the clerestory portion of the window wall. A clear film patterned with linear, 50-250 micrometer high, four-sided asymmetrical prisms was fabricated and installed in the south-facing, clerestory low-e, clear glazed windows of a full-scale testbed facility. Views through the film were distorted. The film was evaluated in a sunny climate over a two-year period to gauge daylighting and visual comfort performance. The daylighting aperture was small (window-towall ratio of 0.18) and the lower windows were blocked off to isolate the evaluation to the window film. Workplane illuminance measurements were made in the 4.6 m (15 ft) deep room furnished as a private office. Analysis of discomfort glare was conducted using high dynamic range imaging coupled with the evalglare software tool, which computes the daylight glare probability and other metrics used to evaluate visual discomfort. The window film was found to result in perceptible levels of discomfort glare on clear sunny days from the most conservative view point in the rear of the room looking toward the window. Daylight illuminance levels at the rear of the room were significantly increased above the reference window condition, which was defined as the same glazed clerestory window but with an interior Venetian blind (slat angle set to the cut-off angle), for the equinox to winter solstice period on clear sunny days. For partly cloudy and overcast sky conditions, daylight levels were improved slightly. To reduce glare, the daylighting film was coupled with a diffusing film in an insulating glazing unit. The diffusing film retained the directionality of the redirected light spreading it within a small range of outgoing angles. This solution was found to reduce glare to imperceptible levels while retaining for the most part the illuminance levels achieved solely by the daylighting film.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗
DOE OSTI2011

CdS thin films on LiNbO{sub 3} (1 0 4) and silicon (1 1 1) substrates prepared through an atom substitution method

CdS thin films on LiNbO{sub 3} (1 0 4) and silicon (1 1 1) substrates were prepared through an atom substitution technique using cadmium nitrate as a reactant in an H{sub 2}S atmosphere at 230 {sup o}C. X-ray diffraction, scanning electron microscopy and transmission microscopy results indicate that the CdS film grows on LiNbO{sub 3} oriented along the [0 0 1] axis in form of crystallized nanoplates, while that deposited on silicon forms randomly oriented nanoparticles. Investigation of the precursor thin film suggests that CdS forms from the O in the CdO precursor thin film being substituted by S from H{sub 2}S in the surrounding environment, which is designated as an atom substitution process. This novel method involving an atom substitution reaction between the CdO precursor thin film and its environment can provide a new low cost approach to the preparation of chalcogenide or other compound thin films. A schematic illustration and corresponding mechanism describing the details of this method are proposed. -- Graphical abstract: Elemental O in CdO is substituted by elemental S from the atmosphere in the apparatus, which is designated as an atom substitution process. This novel method involving an atom substitution reaction between the CdO precursor thin film and its environment can provide a new low cost approach to the preparation of chalcogenide or other compound thin films. Display Omitted Research highlights: {yields} An atom substitution method for thin film preparation was demonstrated. {yields} Combination of the atom substitution and spin coating method was achieved. {yields} Well oriented CdS thin film was prepared on LiNbO{sub 3} substrate. {yields} The atom substitution method could be used for many compound systems.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Self-Assembly of Cellulose Nanocrystals into Semi-Spherical Photonic Cholesteric Films

Spherical-shape cholesteric (Ch) photonic films offer promising applications such as omnidirectional lasing and broadband reflection. Here, a strategy is reported for the fabrication of photonic Ch films by the self-assembly of cellulose nanocrystals (CNCs) in semi-spherical cavities. It is shown that film structure and photonic properties are controlled by the film curvature, the composition of the precursor CNC suspension, and its liquid crystalline or isotropic state. The effect of curvature of the drying Ch-CNC films coupled with the restricted mobility of CNCs during film preparation results in the variation in pitch and helical axis inclination, thus leading to broadband reflectance properties of the films. The role of curvature of the Ch-CNC films is underlined by comparing their distinct properties with those of planar films with the same composition. We report these findings provide a novel insight into the design and development of biomimetic photonic Ch films.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Stoichiometric Control and Optical Properties of BaTiO 3 Thin Films Grown by Hybrid MBE

BaTiO 3 is a technologically relevant material in the perovskite oxide class with above-room-temperature ferroelectricity and a very large electro-optical coefficient, making it highly suitable for emerging electronic and photonic devices. An easy, robust, straightforward, and scalable growth method is required to synthesize epitaxial BaTiO 3 thin films with sufficient control over the film's stoichiometry to achieve reproducible thin film properties. Here the growth of BaTiO 3 thin films by hybrid molecular beam epitaxy is reported. A self-regulated growth window is identified using complementary information obtained from reflection high energy electron diffraction, the intrinsic film lattice parameter, film surface morphology, and scanning transmission electron microscopy. Subsequent optical characterization of the BaTiO 3 films by spectroscopic ellipsometry revealed refractive index and extinction coefficient values closely resembling those of stoichiometric bulk BaTiO 3 crystals for films grown inside the growth window. Even in the absence of a lattice parameter change of BaTiO 3 thin films, degradation of optical properties is observed, accompanied by the appearance of a wide optical absorption peak in the IR spectrum, attributed to optical transitions involving defect states present. Therefore, the optical properties of BaTiO 3 can be utilized as a much finer and more straightforward probe to determine the stoichiometry level present in BaTiO 3 films.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Tuning hydrophobicity of a fluorinated terpolymer in differently assembled thin films

In the current work, casting from good solvent (acetone) and casting from mixed solvent and nonsolvent were employed for preparing thin films of terpolymer of Tetrafluoroethylene (TFE), Hexafluoropropylene (HFP), and Vinylidene fluoride (VDF) (THV), on silicon wafers. These films revealed various morphologies and wetting behaviors depending on the solution concentration, temperature, and thin film preparation method. The THV thin films prepared by casting from good solvent showed smooth morphology with holes. The thin film prepared from a 3 wt % THV/acetone solution by casting from good solvent at 15 °C demonstrated spheres in addition to the smooth morphology, while the thin film prepared from a 5 wt % THV/acetone solution at 15 °C by casting from good solvent had a mesh-like structure with some linked spheres. Casting the thin films from mixed solvent and nonsolvent resulted in various morphologies such as different sphere sizes embedded in a dense film layer, and hexagonal close packed structures. The thin films prepared by casting from good solvent showed a slightly hydrophobic character, with a measured water contact angle of approximately 99°, while the nonsolvent cast films had a water contact angle as high as 145°.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Understanding Reproducibility of Sputter‐Deposited Metastable Ferroelectric Wurtzite Al 0.6 Sc 0.4 N Films Using In Situ Optical Emission Spectrometry

High‐Sc Al 1– x Sc x N thin films are of tremendous interest because of their attractive piezoelectric and ferroelectric properties, but overall film quality and reproducibility are widely reported to suffer as x increases. In this study, structural and electrical properties of metastable Al 0.6 Sc 0.4 N films are connected with plasma changes during film growth, identified via glow discharge optical emission spectroscopy (GD‐OES), and linked to the target mode changes. This in situ GD‐OES technique uses changes in the N 2 (I) intensity, correlated with DC bias hysteresis behavior of a Al 0.6 Sc 0.4 target in metallic and poisoned modes, to identify films that subsequently exhibit unacceptable structural and electrical performance. Two representative samples deposited under identical conditions but possessing distinct properties related to phases present in the films are focused on. Films sputtered under a poisoned target mode produce pure wurtzite ferroelectric Al 0.6 Sc 0.4 N with a reversible 80 μC cm −1 polarization and 3.1 MV cm −1 coercive field. When identical chamber settings are used but the process starts in metallic mode, a mixed wurtzite/rocksalt film is deposited which exhibits nanometer‐scale changes to the film microstructure and a nonferroelectric response. These results illustrate the utility of optical emission spectroscopy for tracking target mode fluctuations when fabricating metastable materials such as high‐Sc Al 1– x Sc x N films.

36 MATERIALS SCIENCE↗