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DOE OSTI2023

Epitaxial Electrodeposition of Wide Bandgap Semiconductors for Energy Conversion and Storage

The focus of this project was to electrodeposit epitaxial films and nanostructures of inorganic materials. Although electrodeposition is normally associated with the electroplating of metals, the emphasis in this work was the deposition of compound materials such as metal oxides, semiconductors, catalysts, and magnetic materials. An electrochemical/chemical approach was used, in which an electrochemical redox reaction was followed by a chemical reaction to produce the product. The materials were deposited as epitaxial thin films or nanostructures onto a single-crystal substrate that determined their in-plane and out-of-plane orientation. Epitaxial films can have enhanced properties due to the lack of grain boundaries. They can also produce catalytic materials which have enhanced reactivity due to the exposure of the most catalytically active surface. A method was developed to produce inexpensive single-crystal-like metal foils that could be used as the substrate to deposit materials for applications such as flexible electronics. It was also demonstrated that epitaxial films of inorganic materials could be produced by a simple spin-coating technique.

36 MATERIALS SCIENCE↗

DOE OSTI2025

FCET Solid Oxide Fuel Cell Testing and Development (CRADA 526) (Final Report)

Pacific Northwest National Laboratory (PNNL) tested electrolyte coatings from Fuel Cell Enabling Technologies, Inc. (FCET) for use in solid oxide fuel cells (SOFCs). The key technology held by FCET is a process to deposit thin layers of oxide materials, less than 1 μm in thickness. The range of possible materials that can be deposited with their method is broad, but this project focused on the gadolinium-doped ceria (GDC) and yttria-stabilized zirconia (YSZ) electrolytes for SOFCs. Thin, gas tight electrolyte membranes have been a long-sought target in SOFC research. The thinner the electrolyte, the lower the cell resistance, and the higher performance of the cell (or the lower the operating temperature). A YSZ thickness of 1 μm would be a step change from the state-of-the-art, tape-cast electrolytes (~10 μm). An in-house prototype SOFC stack from FCET was first tested. The sealing geometry of the prototype stack was determined to be problematic, and testing shifted to button cells. Anode-supported solid oxide electrolysis cell (SOEC) button cells without an electrolyte layer were produced at PNNL and sent to FCET for coating with electrolyte. Three cells were tested with a gadolinium-doped ceria (GDC) electrolyte applied via spin coating. GDC was chosen for its conductivity at lower temperatures than YSZ. All three cells failed during initial reduction under hydrogen at 600°C. Testing then shifted to YSZ, which is the standard SOFC electrolyte. Several button cells were coated with YSZ and examined with scanning electron microscopy (SEM). A promising coating of ~1 mm thickness was observed under SEM. A similarly coated button cell was tested and failed similarly to previous tests during reduction at 600°C. The YSZ coating appeared dense and uniform in SEM analysis. The roughness of the underlying Ni/YSZ anode is on the order of 1 μm, and that may have compromised the gas-tightness of the coating. Further development is warranted to understand and refine the coating process. Thin YSZ applied via this spin-coating technique could be used as a low-cost, drop-in replacement in large-scale SOFC manufacturing processes, improving cell performance and lowering the cost per watt of SOFCs.

30 DIRECT ENERGY CONVERSION↗

DOE OSTI2023

Developing Enzyme Immobilization with Fibrous Membranes: Longevity and Characterization Considerations

Fibrous membranes offer broad opportunities to deploy immobilized enzymes in new reactor and application designs, including multiphase continuous flow-through reactions. Enzyme immobilization is a technology strategy that simplifies the separation of otherwise soluble catalytic proteins from liquid reaction media and imparts stabilization and performance enhancement. Flexible immobilization matrices made from fibers have versatile physical attributes, such as high surface area, light weight, and controllable porosity, which give them membrane-like characteristics, while simultaneously providing good mechanical properties for creating functional filters, sensors, scaffolds, and other interface-active biocatalytic materials. This review examines immobilization strategies for enzymes on fibrous membrane-like polymeric supports involving all three fundamental mechanisms of post-immobilization, incorporation, and coating. Post-immobilization offers an infinite selection of matrix materials, but may encounter loading and durability issues, while incorporation offers longevity but has more limited material options and may present mass transfer obstacles. Coating techniques on fibrous materials at different geometric scales are a growing trend in making membranes that integrate biocatalytic functionality with versatile physical supports. Biocatalytic performance parameters and characterization techniques for immobilized enzymes are described, including several emerging techniques of special relevance for fibrous immobilized enzymes. Diverse application examples from the literature, focusing on fibrous matrices, are summarized, and biocatalyst longevity is emphasized as a critical performance parameter that needs increased attention to advance concepts from lab scale to broader utilization. This consolidation of fabrication, performance measurement, and characterization techniques, with guiding examples highlighted, is intended to inspire future innovations in enzyme immobilization with fibrous membranes and expand their uses in novel reactors and processes.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2024

Advances in Electrospun Poly(ε-caprolactone)-Based Nanofibrous Scaffolds for Tissue Engineering

Tissue engineering has great potential for the restoration of damaged tissue due to injury or disease. During tissue development, scaffolds provide structural support for cell growth. To grow healthy tissue, the principal components of such scaffolds must be biocompatible and nontoxic. Poly(ε-caprolactone) (PCL) is a biopolymer that has been used as a key component of composite scaffolds for tissue engineering applications due to its mechanical strength and biodegradability. However, PCL alone can have low cell adherence and wettability. Blends of biomaterials can be incorporated to achieve synergistic scaffold properties for tissue engineering. Electrospun PCL-based scaffolds consist of single or blended-composition nanofibers and nanofibers with multi-layered internal architectures (i.e., core-shell nanofibers or multi-layered nanofibers). Nanofiber diameter, composition, and mechanical properties, biocompatibility, and drug-loading capacity are among the tunable properties of electrospun PCL-based scaffolds. Scaffold properties including wettability, mechanical strength, and biocompatibility have been further enhanced with scaffold layering, surface modification, and coating techniques. In this article, we review nanofibrous electrospun PCL-based scaffold fabrication and the applications of PCL-based scaffolds in tissue engineering as reported in the recent literature.

Polymer Science↗

NASA NTRS1971

Thin wing corrections for phase-change heat-transfer data.

Since no methods are available for determining the magnitude of the errors incurred when the semiinfinite slab assumption is violated, a computer program was developed to calculate the heat-transfer coefficients to both sides of a finite, one-dimensional slab subject to the boundary conditions ascribed to the phase-change coating technique. The results have been correlated in the form of correction factors to the semiinfinite slab solutions in terms of parameters normally used with the technique.

Hunt, J. L.↗

NASA NTRS1972

Hypersonic aerothermal characteristics of a manned low finenes ratio shuttle booster

An investigation of a winged booster model having canards and an ascent configuration comprised of the booster mounted in tandem with an orbiter model has been conducted at Mach 10.2 in the continuous flow hypersonic tunnel. Longitudinal and lateral directional force characteristics were obtained over angle of attack ranges of -12 deg to 60 deg for the booster and -11 deg to 11 deg for the ascent configuration. Interference heating effects on the booster using the phase-change coating technique were determined at 0 deg angle of attack. Some oil flow photographs of the isolated booster and orbiter and ascent configuration are also presented.

Bernot, P. T.↗

NASA NTRS1972

Effect of wing sweep, angle of attack, Reynolds number, and wing root fillet on the interference heating to the wing windward surface of an entry vehicle configuration

The phase-change-coating technique was used to study the interference heating to the windward surface of 14 deg, 25 deg, and 50 deg swept wings of an entry vehicle configuration. One wing root of each model was faired to the fuselage with a fillet. Tests were made at Mach 8 at angles of attack of 0 deg, 20 deg, 40 deg, and 60 deg and at free-stream Reynolds numbers based on model length of 0.47 and 1.7 million. Bow shock impingement heating was found to increase in magnitude and affected area with increasing angle of attack until at a higher angle of attack it decreases; this angle of attack is lower for a 50 deg swept wing. Wing root interference heating was found to increase with angle of attack up to 40 deg and then to remain approximately constant. Consequently, wing root interference heating becomes the major type of interference heating at large angles of attack, and this occurs at a lower angle of attack for the highest sweep angle. A wing leading-edge root fillet reduces the peak in wing root interference heating near the leading edge, and increasing Reynolds number increases the level of interference heating.

Clark, L. E.↗

NASA NTRS1971

Heat transfer tests of the NASA-MSC space shuttle configuration at the Langley Research Center Mach 8 Variable Density Facility

The experimental investigations performed on the NASA-Manned Spacecraft Center Space Shuttle orbiter and booster configurations at a Mach 8 variable density facility are presented. The test program was a series of aerothermodynamic wind tunnel tests that were run over a range of angles of attack, yaw angles, and Reynolds numbers. Objectives of the test program were to obtain heat transfer data over the NASA-Manned Spacecraft Center Space Shuttle orbiter, booster, and launch configurations for a range of angles of attack from - 20 to + 30 deg, yaw angles of 0 and + or - 6 deg, and Reynolds numbers of 0.6, 2.0, and 3.7 x one million. The phase-change coating technique was used to obtain heat transfer data. Information received from these tests will be instrumental in performing thermal protection systems studies and vehicle aerodynamic design.

Connor, L. E.↗

NASA NTRS1974

Experimental investigation at Mach 8 of the effects of projections and cavities on heat transfer to a model of the Viking aeroshell

An experimental investigation into the aerodynamic heating on a Mars entry vehicle shape with several types of local surface distortion is presented. The configurations tested were 0.033-scale models of a spherically blunted 70 deg half-angle cone with two protuberances of different length, representing the tube leading to the gas chromograph mass spectrometer, and two aeroshell-bioshield attachment points of different size. These models were tested at free-stream Reynolds numbers per meter of 3.7 million and 17 million over an angle-of-attack range from 0 to 18 deg in the Langley Mach 8 variable density hypersonic tunnel. The phase change-coating technique was used to measure heat transfer coefficient. The long protuberance caused more severe interference heating than the short protuberance for the same conditions. When the short projection was located close to the edge of the aeroshell, the interference heating was greater than that on the same projection when located near the vertex. A significant increase in heat transfer coefficient was measured only on the larger aeroshell-bioshield attachment point.

Creel, T. R., Jr.↗

NASA NTRS1976

Abrasion-resistant coatings for plastic surfaces

Optically clear composition of organosilicon compounds insulates plastic surfaces and protects them from abrasion. Plasma polymerization process produces superior uniformity and clarity than previous coating techniques.

Wydeven, T.↗

NASA NTRS1976

Cyclic debonding of unidirectional composite bonded to aluminum sheet for constant-amplitude loading

Cyclic debonding rates were measured during constant-amplitude loading of specimens made of graphite/epoxy bonded to aluminum and S-glass/epoxy bonded to aluminum. Both room-temperature and elevated-temperature curing adhesives were used. Debonding was monitored with a photoelastic coating technique. The debonding rates were compared with three expressions for strain-energy release rate calculated in terms of the maximum stress, stress range, or a combination of the two. The debonding rates were influenced by both adherent thickness and the cyclic stress ratio. For a given value of maximum stress, lower stress ratios and thicker specimens produced faster debonding. Microscopic examination of the debonded surfaces showed different failure mechanisms both for identical adherends bonded with different adhesive and, indeed, even for different adherends bonded with identical adhesives. The expressions for strain-energy release rate correlated the data for different specimen thicknesses and stress ratios quite well for each material system, but the form of the best correlating expression varied among material systems. Empirical correlating expressions applicable to one material system may not be appropriate for another system.

Roderick, G. L.↗

NASA NTRS1977

Correlation of turbulent shear layer attachment peak heating near Mach 6

A correlation of new turbulent two-dimensional data and peak heating data for attaching free shear layers is presented for a 2.54-cm and 5.08-cm diam cylindrical leading-edge slab 25.4 cm long, and 7.62 and 10.16 cm wide. A 30.48 x 25.4 cm sharp leading-edge flat plate set at 15 and 20 deg is used to generate plane impinging shocks. The freestream Mach number is 6 and the freestream Reynolds number varies from 3,300,000 to 25,600,000/m. Peak heating is measured on silica-based epoxy models with a phase change coating technique. A comparison of the free shear layer data with the transition data of Birch and Keyes (1972) reveals that the shear layer data are turbulent at attachment. The trend of the data shows that peak heating is strongly affected by the state of development at attachment. As the free shear layers become more fully developed, the data approach the two-dimensional correlation. Persistence of transitional flow structures for supersonic free shear flows is pointed out.

Keyes, J. W.↗

NASA NTRS1978

The Array Automated Assembly Task for the Low Cost Solar Array Project, Phase 2

During the program a process sequence was proposed and tested for the fabrication of dendritic welb silicon into solar modules. This sequence was analyzed as to yield and cost and these data suggest that the price goals of 1986 are attainable. Specifically, it was shown that a low cost POCL3 is a suitable replacement for the semiconductor grade, and that a suitable CVD oxide can be deposited from a silane/air mixture using a Silox reactor. A dip coating method was developed for depositing an antireflection coating from a metalorganic precursor. Application of photoresist to define contact grids was made cost effective through use of a dip coating technique. Electroplating of both Ag and Cu was shown feasible and cost effective for producing the conductive metal grids on the solar cells. Laser scribing was used to separate the cells from the dendrites without degradation. Ultrasonic welding methods were shown to be feasible for interconnecting the cells. A study of suitable low cost materials for encapsulation suggest that soda lime glass and phenolic filled board are preferred.

Campbell, R. B.↗

NASA NTRS1981

Evaluation of non-specular reflecting silvered Teflon and filled adhesives

A non-specular silver-Teflon tape thermal control coating was tested to provide the data necessary to qualify it for use on the Space Shuttle Orbiter radiators. Effects of cure cycle temperature and pressure on optical and mechanical properties on the silver-Teflon tape were evaluated. The baseline Permacel P-223 adhesive, used with the specular silver-Teflon tape initially qualified for the Orbiter radiators, and four alternate metal-filled and unfilled adhesives were evaluated. Tests showed the cure process has no effect on the silver-Teflon optical properties, and that the baseline adhesive cure cycle gives best results. In addition the P-223 adhesive bond is more reproducible than the alternates, and the non-specular tape meets both the mechanical and the optical requirements of the Orbiter radiator coating specification. Existing Orbiter coating techniques were demonstrated to be effective in aplying the non-specular tape to a curved panel simulating the radiators. Author

Bourland, G.↗

NASA NTRS1981

A Module Experimental Process System Development Unit (MEPSDU)

The development of a cost effective process sequence that has the potential for the production of flat plate photovoltaic modules which meet the price goal in 1986 of 70 cents or less per Watt peak is described. The major accomplishments include (1) an improved AR coating technique; (2) the use of sand blast back clean-up to reduce clean up costs and to allow much of the Al paste to serve as a back conductor; and (3) the development of wave soldering for use with solar cells. Cells were processed to evaluate different process steps, a cell and minimodule test plan was prepared and data were collected for preliminary Samics cost analysis.

Source record↗

NASA NTRS1983

Rewaterproofing Silica Tiles

Waterproofing agent, vaporized in bubbler transported by gas flowing in system and deposits in pores of tiles. Vapor carried through hole of approximately 1/16 inch (1.6.mm) diameter made in tile coating. Technique used to waterproof buildups (concrete and brick) and possibly fabrics.

Lleger, L. J.↗

NASA NTRS1984

Aerodynamic heating rate distributions induced by trailing edge controls on hypersonic aircraft configurations at Mach 8

Aerodynamic surface heating rate distributions in three dimensional shock wave boundary layer interaction flow regions are presented for a generic set of model configurations representative of the aft portion of hypersonic aircraft. Heat transfer data were obtained using the phase change coating technique (paint) and, at particular spanwise and streamwise stations for sample cases, by the thin wall transient temperature technique (thermocouples). Surface oil flow patterns are also shown. The good accuracy of the detailed heat transfer data, as attested in part by their repeatability, is attributable partially to the comparatively high temperature potential of the NASA-Langley Mach 8 Variable Density Tunnel. The data are well suited to help guide heating analyses of Mach 8 aircraft, and should be considered in formulating improvements to empiric analytic methods for calculating heat transfer rate coefficient distributions.

Kaufman, L. G., II↗

NASA NTRS1984

Evaporative coating of a sphere from a point source

To optimize the procedure for evaporating a metal film onto a sphere, calculations of the film thickness distribution for various motions of the sphere have been carried out. These calculations, including shadowing effects of sphere support rods, are presented in this paper. Also, an apparatus and procedure for the evaporative coating of a sphere are described. A comparison of measured thickness with the calculated values is made for one example of sphere motion. The implications of the calculated results for coating techniques are discussed.

Strayer, D. M.↗