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NASA NTRS1995

3D thin film microstructures for space microrobots

Micromechanisms of locomotion and a manipulator with an external skeleton like the structure of an insect are proposed. Several micro-sized models were built on silicon wafers by using polysilicon for rigid plates and polyimide for elastic joints. Due to scale effects, friction in micromechanical components is dominant as compared to the inertial forces because friction is proportional to L(exp 2) while mass is proportional to L(exp 3). Therefore, to ensure efficient motion, rotational joint that exhibits rubbing should be avoided. In this paper, paper models of a robot leg and a micro-manipulator are presented to show structures with external skeletons and elastic joints. Then the large scale implementation using plastic plates, springs, and solenoids is demonstrated. Since the assembly technique is based on paper folding, it is compatible with thin film micro-fabrication and integrated circuit (IC) planar processes. Finally, several micromechanisms were fabricated on silicon wafers to demonstrate the feasibility of building a 3D microstructure from a single planar structure that can be used for space microrobots.

Shimoyama, Isao↗

DOE OSTI2024

Chain rigidity controlled aggregation ability and solid-state microstructures for efficient stretchable conjugated polymer films

Stretchable conjugated polymer films with good electrical performance under mechanical deformation are highly desirable for soft electronics. However, the mechanical and electrical properties of these films, particularly in conjugated polymer:elastomer blends, are not fully understood at molecular level. Here, this study explores the relationships among molecular structure, aggregation ability, film microstructure, and the electrical/mechanical properties of three diketopyrrolopyrrole-based conjugated polymers (P1, P2, P3) with decreasing backbone rigidity and their corresponding polymer:elastomer blends. The most flexible polymer P3 shows strong aggregation, which forms highly crystalline fibers to produce fragile neat film and produces large isolated crystallites restricting charge transport in blend film. As chain rigidity increases, the P1 and P2 polymers show weaker aggregation, and produce smaller crystallites in neat films with enhanced ductility. P1 and P2 based blend films display nanocrystallites polymer networks with dispersed elastomer domains. As a result, we achieved near-constant charge mobility before and after stretching under 50 % strain for P2-based blend films with well-controlled pathways for both charge transport and energy dissipation. This study demonstrates the critical role of backbone rigidity in regulating the properties of stretchable conjugated polymer films, paving the way for more reliable and deformable materials in soft electronics.

36 MATERIALS SCIENCE↗

NASA NTRS1991

Thin film diamond microstructure applications

Selective deposition and abrasion, as well as etching in atomic oxygen or reduced-pressure air, have been used to prepare patterned polycrystalline diamond films which, on further processing by anisotropic Si etching, yield the microstructures of such devices as flow sensors and accelerometers. Both types of sensor have been experimentally tested in the respective functions of hot-wire anemometer and both single- and double-hinged accelerometer.

Roppel, T.↗

NASA NTRS1989

Effects of microstructure and nonstoichiometry on electrical properties of vanadium dioxide films

Voided growth structures of sputter-deposited films affect strongly their optical and electrical properties. Vanadium dioxide is an interesting material to study effects of film microstructure and nonstoichiometry on electrical properties because its phase transition makes it possible to investigate electrical behavior both in a semiconducting phase and in a metallic phase. Vanadium oxide films were deposited with different vanadium oxygen ratios for substrate temperatures between 250 and 550 C by dc reactive magnetron sputtering. The resistivity ratios between a semiconducting phase and a metallic phase are limited to 1000 order by voided boundaries and oxygen vacancies. The voided boundaries are defined by columnar structure and agglomerated grain growth. The results emphasize the necessity of a combination of deposition to obtain the film with a favorable structure and postdeposition annealing to control the film stoichiometry.

Kusano, Eiji↗

DOE OSTI2025

High-rate magnetron sputter deposition of low-stress boron carbide films on tilted substrates

Boron carbide is attractive for several applications, including nuclear fuel capsules for inertial confinement fusion (ICF). The fabrication of ICF capsules involves the deposition of ultrathick coatings with density and thickness uniformity on submicron length scales on non-planar (spherical) substrates. Such a deposition requires control of the deposition rate, residual stress, and film microstructure. Here, we systematically study the direct-current magnetron sputter deposition of B 4 C coatings with a full-face-erosion magnetron source as a function of substrate tilt and Ar working gas pressure. Film properties are correlated with results of plasma diagnostics and predictions of Monte Carlo simulations of ballistic sputtering and gas-phase transport. The fabrication of low-stress amorphous B 4 C films with deposition rates of 7μm/h is demonstrated.

Kawasaki, K. [Lawrence Livermore National Laborato↗

DOE OSTI2025

Dendritic microstructures observed in electron-beam deposited hafnia films

Dendritic microstructures inside hafnia dielectric coatings fabricated via electron-beam deposition are investigated. These structures are observable with different optical characterization tools, including atomic force microscopy, fluorescence microscopy, Raman microscopy, and differential interference contrast microscopy. Long-term monitoring of individual samples over a seven-year time span revealed that the dendrite-like structures evolve over time, while the hafnia material in the dendrite structure—as compared to the rest of the coating—shows a decrease in crystallinity and an increase in defect density.

Hoffman, B. N. [Univ. of Rochester, NY (United Sta↗

NASA NTRS1998

Tunable Dielectric Materials and Devices for Broadband Wireless Communications

Wireless and satellite communications are a rapidly growing industries which are slated for explosive growth into emerging countries as well as countries with advanced economies. The dominant trend in wireless communication systems is towards broadband applications such as multimedia file transfer, video transmission and Internet access. These applications require much higher data transmission rates than those currently used for voice transmission applications. To achieve these higher data rates, substantially larger bandwidths and higher carrier frequencies are required. A key roadblock to implementing these systems at K-band (18-26.5 GHz) and Ka-band (26.5-40 GHz) is the need to develop hardware which meets the requirements for high data rate transmission in a cost effective manner. In this chapter, we report on the status of tunable dielectric thin films for devices, such as resonators, filters, phased array antennas, and tunable oscillators, which utilize nonlinear tuning in the control elements. Paraelectric materials such as Barium Strontium Titanate ((Ba, Sr)TiO3) have dielectric constants which can be tuned by varying the magnitude of the electric field across the material. Therefore, these materials can be used to control the frequency and/or phase response of various devices such as electronically steerable phased array antennas, oscillators, and filters. Currently, tunable dielectric devices are being developed for applications which require high tunability, low loss, and good RF power-handling capabilities at microwave and millimeter-wave frequencies. These properties are strongly impacted by film microstructure and device design, and considerable developmental work is still required. However, in the last several years enormous progress has occurred in this field, validating the potential of tunable dielectric technology for broadband wireless communication applications. In this chapter we summarize how film processing techniques, microwave test configurations, and prototype devices have combined to drive the field to its current stage of development.

Mueller, Carl H.↗

DOE OSTI2026

Scalable Layer-by-Layer Electrospray-Assisted Interfacial Polymerization: Enabling Large-Area Polyamide Membrane Fabrication

Layer-by-layer electrospray-assisted interfacial polymerization (LBL-EAIP) has recently been proposed as an alternative approach for fabricating polyamide membranes with precisely controlled thickness and polymerization degree, showing great potential for reverse osmosis (RO) membrane synthesis. In this article, we report a scale-up strategy for LBL-EAIP to enable its practical application in RO membrane manufacturing. A multi-jet electrospray apparatus was developed, and the device configuration and process parameters were carefully adjusted to produce polyamide-on-polyethersulfone thin film composite (TFC) membranes with consistently high salt rejection and water permeance across the membrane area. Specifically, an average 97.1% NaCl rejection from a 2000 ppm NaCl feed was achieved with an area-to-area deviation of 1%, along with a deionized water permeance of 0.90 ± 0.11 LMH/bar at 15 bar feed pressure. In addition, a Fourier-transform infrared spectroscopy (FTIR)-based analytical method was developed for semi-quantitative assessment of membrane thickness and compositional uniformity, enabling rapid mapping of film microstructure and chemical variations. This work provides a pathway to scale up LBL-EAIP technology, bridging the gap between laboratory-scale innovation and industrial-scale manufacturing.

Feng, Yue (ORCID:0000000221343980)↗

DOE OSTI2026

Synthesis of epitaxial TaO$_2$ thin films on Al$_2$O$_3$ by suboxide molecular-beam epitaxy and thermal laser epitaxy

Tantalum dioxide (TaO2) is a metastable tantalum compound. Here, we report the epitaxial stabilization of TaO2 on Al2O3 (1-102) (r-plane sapphire) substrates using suboxide molecular-beam epitaxy (MBE) and thermal laser epitaxy (TLE), demonstrating single-oriented, monodomain growth of anisotropically strained thin films. Microstructural investigation is performed using synchrotron X-ray diffraction and scanning transmission electron microscopy. The tetravalent oxidation state of tantalum is confirmed using X-ray absorption and photoemission spectroscopy as well as electron energy-loss spectroscopy. Optical properties are investigated via spectroscopic ellipsometry and reveal a 0.3 eV Mott gap of the tantalum 5d electrons. Density-functional theory and group theoretical arguments are used to evaluate the limited stability of the rutile phase and reveal the potential to unlock a hidden metal-insulator transition concomitant with a structural phase transition to a distorted rutile phase, akin to NbO2. Our work expands the understanding of tantalum oxides and paves the way for their integration into next-generation electronic and photonic devices.

FOS: Physical sciences↗

NASA NTRS1994

High Tc superconducting bolometric and nonbolometric infrared (IR) detectors

The original workplan for the first year of the project includes the following: establishment of a pilot superconductivity application laboratory at UDC to support the research component of the project; research on the source of electrical noise in High Tc superconducting films in order to optimize the film microstructure and lower the NEP; and lay the foundation of an academic support for exposing UDC students to the theory and application of High Tc superconductivity. Attached to this status report are abstracts and the course description for Introduction to Applications of Superconductivity.

Lakeou, Samuel↗

NASA NTRS1991

Oxygen plasma ashing effects on aluminum and titanium space protective coatings

Using variable angle spectroscopic ellipsometry and atomic force microscopy (AFM), the surface roughness and oxidation of aluminum and titanium thin films have been studied as a function of substrate deposition temperature and oxygen plasma exposure. Increasing substrate deposition temperatures affect film microstructure by greatly increasing grain size. Short exposures to an oxygen plasma environment produce sharp spikes rising rapidly above the surface as seen by AFM. Ellipsometric measurements were made over a wide range of plasma exposure times, and results at longer exposure times suggest that the surface is greater than 30% void. This is qualitatively verified by the AFM images.

Synowicki, R.↗

NASA NTRS2007

Absorber Materials for Transition-Edge Sensor X-ray Microcalorimeters

Arrays of superconducting transition-edge sensors (TES) can provide high spatial and energy resolution necessary for x-ray astronomy. High quantum efficiency and uniformity of response can be achieved with a suitable absorber material, in which absorber x-ray stopping power, heat capacity, and thermal conductivity are relevant parameters. Here we compare these parameters for bismuth and gold. We have fabricated electroplated gold, electroplated gold/electroplated bismuth, and evaporated gold/evaporated bismuth 8x8 absorber arrays and find that a correlation exists between the residual resistance ratio (RRR) and thin film microstructure. This finding indicates that we can tailor absorber material conductivity via microstructure alteration, so as to permit absorber thermalization on timescales suitable for high energy resolution x-ray microcalorimetry. We show that by incorporating absorbers possessing large grain size, including electroplated gold and electroplated gold/electroplated bismuth, into our current Mo/Au TES, devices with tunable heat capacity and energy resolution of 2.3 eV (gold) and 2.1 eV (gold/bismuth) FWHM at 6 keV have been fabricated.

Brown, Ari-David↗

NASA NTRS2003

Interplay Between Thin Film Ferroelectric Composition, Microstructure and Microwave Phase Shifter Performance

One of the keys to successfully incorporating ferroelectric films into Ku-band (12 to 18 GHz) phase shifters is to establish the composition, microstructure, and thickness required to meet the tuning needs, and tailor the film properties to meet these needs. Optimal performance is obtained when the film composition and device design are such that the device performance is limited by odd mode dielectric losses, and these losses are minimized as much as possible while still maintaining adequate tunability. The parameters required to maintain device performance will vary slightly depending on composition, but we can conclude that the best tuning-to-loss figures of merit (K-factor) are obtained when there is minimal variation between the in-plane and out-of-plane lattice parameters, and the full-width half maximum values of the BSTO (002) peaks are less than approximately 0.04 deg. We have observed that for phase shifters in which the ferroelectric crystalline quality and thickness are almost identical, higher losses are observed in films with higher BaISr ratios. The best performance was observed in phase shifters with Ba:Sr = 30:70. The superiority of this composition was attributed to several interacting factors: the B a: Sr ratio was such that the Curie temperature (180 K) was far removed from room temperature, the crystalline quality of the film was excellent, and there was virtually no difference between the inplane and out-of-plane lattice parameters of the film.

Mueller, Carl H.↗

NASA NTRS1984

Characteristic morphological and frictional changes in sputtered MoS/sub 2 films

Three microstructural growth stages of sputtered MoS2 films were identified with respect to film thickness: (1) ridge formation during nucleation, (2) an equiaxed transition zone, and (3) a columnar-fiber-like structure. Each of these growth stages are characterized in terms of microcrystallite size, shape, and orientation. The effective lubricating film thickness is established in terms of the microstructural growth stages during sliding experiments. The film has a tendency to break up within the columnar zone. Actual lubrication is performed by the remaining film which is 0.18 to 0.22 microns thick. Also a visual screening is proposed to evaluate the integrity of the as-sputtered MoS2 film. The lubricating properties are identified with respect to optical changes before and after wiping. The orientation of the microcrystallites are responsible for the optical reflective changes observed.

Spalvins, T.↗

NASA NTRS2004

Raman Microscopic Characterization of Proton-Irradiated Polycrystalline Diamond Films

The microstructural effects of irradiating polycrystalline diamond films with proton dosages ranging from 10(exp 15) to 10(exp 17) H(+) per square centimeter was examined. Scanning Electron Microscopy and Raman microscopy were used to examine the changes in the diamond crystalline lattice as a function of depth. Results indicate that the diamond lattice is retained, even at maximum irradiation levels.

Newton, R. L.↗

NASA NTRS1991

Investigation of microstructural changes in polyetherether-ketone films at cryogenic temperatures by positron lifetime spectroscopy

Microstructural changes in Polyetherether-ketone (PEEK) films were investigated in the temperature ranges of 23 to -196 C, using Positron Lifetime Spectroscopy (PLS) technique. It was determined that the total free volume decreases by about 46 percent in amorphous PEEK samples and about 36 percent in semicrystalline PEEK samples when they are cooled down from room temperature to liquid nitrogen (LN2) temperature. If this trend in reduction in free volume with decreasing temperature continues, as expected, it is surmised that PEEK will be able to withstand cooling down to liquid hydrogen (LH2) temperature without any detrimental effect on its diffusivity for liquid hydrogen.

Singh, Jag J.↗

NASA NTRS1991

Applications of diamond films and related materials; Proceedings of the 1st International Conference, Auburn, AL, Aug. 17-22, 1991

The present conference discusses the nucleation and growth of diamond from hydrocarbons, the cutting tool performance of CVD thick-film diamond, the characterization of CVD diamond grinding powder, industrial applications of crystalline diamond-coated tools, standardized SEM tribometry of diamond-coated substrates, residual stress in CVD diamond films, the optical properties of CVD diamond films, polycrystalline diamond films for optical applications, and diamond growth on ferrous metals. Also discussed are ion beam-irradiation smoothing of diamond films, electronic circuits on diamond substrates, diamond-laminated surfaces for evaporative spray cooling, electron devices based on the unique properties of diamond, diamond cold cathodes, thin-film diamond microstructure applications, Schottky diodes from flame-grown diamond, diamond films for thermionic applications, methods of diamond nucleation and selective deposition, high-rate/large-area diamond film production, halogen-assisted diamond growth, the economics of diamond technology, and the optical and mechanical properties of diamondlike films.

Tzeng, Yonhua↗

DOE OSTI2025

High-throughput multimodal exploration of a nanocrystalline Cu-Ag library

Sputter-deposited, nanocrystalline Cu-Ag thin films produced across a broad compositional and deposition-parameter space were evaluated to unravel the process-structure-property relationships important for creating hard, conductive electrical contacts and coatings. Combinatorial deposition involving pulsed direct current magnetron sputtering of elemental targets enabled swift examination of nearly the full range of alloy compositions and a relevant portion of deposition atomistics. Several high-throughput characterization modalities were employed to evaluate the chemistry, structure, and properties of the films. The resultant hardness, modulus, film density, crystal texture, and resistivity were analyzed in terms of key deposition characteristics (incident atom kinetic energy and incidence angle) predicted by binary-collision, kinematic Monte Carlo simulations. The study revealed improved hardness, parabolic resistivity dependence on composition, and compositional and process dependencies of film tarnishing. The results are discussed in the context of variations in microstructure and film density. Transmission electron microscopy and X-ray diffraction demonstrate several forms of compositional variation including solute segregation to grain boundaries as well as periodic, intragranular compositional modulations. Annealing of a Cu-rich alloy film exhibiting grain boundary segregation showed that this as-deposited, compositional variation is not stable above 100 °C. Finally, the Cu-Ag system is shown to have potential for hard, conductive, tarnish-resistant and room temperature-stable nanocrystalline thin films across the composition space.

36 MATERIALS SCIENCE↗