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At least 775 records · Page 43

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DOE OSTI2023

Asymmetric Electrode Work Function Customization via Top Electrode Replacement in Ferroelectric and Field–Induced Ferroelectric Hafnium Zirconium Oxide Thin Films

Non-volatile memory device structures such as ferroelectric random-access memory and ferroelectric tunnel junctions employ switchable spontaneous polarization to hold binary states. These devices can potentially benefit from the imposition of spontaneous internal biases and their resulting effect on the polarization properties of the ferroelectric (or field-induced ferroelectric/ antiferroelectric) layer. While HfO 2 -based thin films are ideal candidates for implementation into these devices due to their scalability and silicon compatibility, the phase purity of these oxides is sensitive to the selection of electrode material, preventing incorporation of asymmetric electrode layers into such structures. Within this work, electrode replacement following post-metallization anneal processing is introduced as a route to achieve ferroelectric and field-induced ferroelectric Hf x Zr 1–x O 2 (HZO) thin films with electrode-independent phase constitutions. The effects of this process and the corresponding internal biases imposed across the HZO layers due to asymmetric work functions are investigated. It is shown that internal biases vary in magnitude in accordance with prediction based on the work functions of the replaced electrode layers and affect remanent polarization magnitudes. Accordingly, electrode replacement presents a processing route that can readily produce HZO films with spontaneous internal biases and electrode- independent phase constitutions, facilitating implementation of these ferroelectrics into the next generation device structures.

36 MATERIALS SCIENCE↗

NASA NTRS1979

Feasibility study of silicon nitride regenerators

The feasibility of silicon nitride as a regenerator matrix material for applications requiring inlet temperatures above 1000 C is examined. The present generation oxide ceramics are used as a reference to examine silicon nitride from a material characteristics, manufacturing, thermal stress and aerothermodynamic viewpoint.

Fucinari, C. A.↗

NASA NTRS1989

Making MgO/SiO2 Glasses By The Sol-Gel Process

Silicon dioxide glasses containing 15 mole percent magnesium oxide prepared by sol-gel process. Not made by conventional melting because ingredients immiscible liquids. Synthesis of MgO/SiO2 glass starts with mixing of magnesium nitrate hexahydrate with silicon tetraethoxide, both in alcohol. Water added, and transparent gel forms. Subsequent processing converts gel into glass. Besides producing glasses of new composition at lower processing temperatures, sol-gel method leads to improved homogeneity and higher purity.

Bansal, Narottam P.↗

NASA NTRS2008

Oxidation Behavior of Carbon Fiber-Reinforced Composites

OXIMAP is a numerical (FEA-based) solution tool capable of calculating the carbon fiber and fiber coating oxidation patterns within any arbitrarily shaped carbon silicon carbide composite structure as a function of time, temperature, and the environmental oxygen partial pressure. The mathematical formulation is derived from the mechanics of the flow of ideal gases through a chemically reacting, porous solid. The result of the formulation is a set of two coupled, non-linear differential equations written in terms of the oxidant and oxide partial pressures. The differential equations are solved simultaneously to obtain the partial vapor pressures of the oxidant and oxides as a function of the spatial location and time. The local rate of carbon oxidation is determined at each time step using the map of the local oxidant partial vapor pressure along with the Arrhenius rate equation. The non-linear differential equations are cast into matrix equations by applying the Bubnov-Galerkin weighted residual finite element method, allowing for the solution of the differential equations numerically.

Sullivan, Roy M.↗

NASA NTRS2014

Novel Materials, Processing and Device Technologies for Space Exploration with Potential Dual-Use Applications

We highlight results of a broad spectrum of efforts on lower-temperature processing of nanomaterials, novel approaches to energy conversion, and environmentally rugged devices. Solution-processed quantum dots of copper indium chalcogenide semiconductors and multiwalled carbon nanotubes from lower-temperature spray pyrolysis are enabled by novel (precursor) chemistry. Metal-doped zinc oxide (ZnO) nanostructured components of photovoltaic cells have been grown in solution at low temperature on a conductive indium tin oxide substrate. Arrays of ZnO nanorods can be templated and decorated with various semiconductor and metallic nanoparticles. Utilizing ZnO in a more broadly defined energy conversion sense as photocatalysts, unwanted organic waste materials can potentially be repurposed. Current efforts on charge carrier dynamics in nanoscale electrode architectures used in photoelectrochemical cells for generating solar electricity and fuels are described. The objective is to develop oxide nanowire-based electrode architectures that exhibit improved charge separation, charge collection and allow for efficient light absorption. Investigation of the charge carrier transport and recombination properties of the electrodes will aid in the understanding of how nanowire architectures improve performance of electrodes for dye-sensitized solar cells. Nanomaterials can be incorporated in a number of advanced higher-performance (i.e. mass specific power) photovoltaic arrays. Advanced technologies for the deposition of 4H-silicon carbide are described. The use of novel precursors, advanced processing, and process studies, including modeling are discussed from the perspective of enhancing the performance of this promising material for enabling technologies such as solar electric propulsion. Potential impact(s) of these technologies for a variety of aerospace applications are highlighted throughout. Finally, examples are given of technologies with potential spin-offs for dual-use or terrestrial applications.

solid state devices↗

NASA NTRS1974

Gravitational effects of process-induced dislocations in silicon

Matters pertaining to semiconductor device fabrication were studied in terms of the influence of gravity on the production of dislocations in silicon wafers during thermal cycling in a controlled ambient where no impurities are present and oxidation is minimal. Both n-type and p-type silicon wafers having a diameter of 1.25 in to 1.5 in, with fixed orientation and resistivity values, were used. The surface dislocation densities were measured quantitatively by the Sirtl etch technique. The results show two significant features of the plastic flow phenomenon as it is related to gravitational stress: (1) the density of dislocations generated during a given thermal cycle is directly related to the duration of the cycle; and (2) the duration of the thermal cycle required to produce a given dislocation density is inversely related to the equilibrium temperature. Analysis of the results indicates that gravitational stress is instrumental in process-induced defect generation.

Porter, W. A.↗

NASA NTRS1980

Silicon solar cells with high open-circuit voltage

Open-circuit voltages as high as 0.645 V (AM0-25 C) have been obtained by a new process developed for low-resistivity silicon. The method utilizes high-dose phosphorus implantation, followed by furnace annealing and simultaneous oxide growth to form high-efficiency, shallow junctions. The effect of the thermally grown oxide is a reduction of surface recombination velocity; the oxide also acts as a moderately efficient AR coating. Boron doped silicon with resistivities from 0.1 to 0.3 ohm-cm has been processed according to this sequence; results show highest open-circuit voltage is attained with 0.1-ohm-cm starting material. The effects of bandgap narrowing, caused by high doping concentrations in the junction, were also investigated by implanting phosphorus over a wide range of dose levels.

Minnucci, J. A.↗

NASA NTRS2000

Corrosion Issues for Ceramics in Gas Turbines

The requirements for hot-gas-path materials in gas turbine engines are demanding. These materials must maintain high strength and creep resistance in a particularly aggressive environment. A typical gas turbine environment involves high temperatures, rapid gas flow rates, high pressures, and a complex mixture of aggressive gases. Figure 26.1 illustrates the requirements for components of an aircraft engine and critical issues [1]. Currently, heat engines are constructed of metal alloys, which meet these requirements within strict temperature limits. In order to extend these temperature limits, ceramic materials have been considered as potential engine materials, due to their high melting points and stability at high temperatures. These materials include oxides, carbides, borides, and nitrides. Interest in using these materials in engines appears to have begun in the 1940s with BeO-based porcelains [2]. During the 1950s, the efforts shifted to cermets. These were carbide-based materials intended to exploit the best properties of metals and ceramics. During the 1960s and 1970s, the silicon-based ceramics silicon carbide (SiC) and silicon nitride (Si3N4) were extensively developed. Although the desirable high-temperature properties of SiC and Si3N4 had long been known, consolidation of powders into component-sized bodies required the development of a series of specialized processing routes [3]. For SiC, the major consolidation routes are reaction bonding, hot-pressing, and sintering. The use of boron and carbon as additives which enable sintering was a particularly noteworthy advance [4]. For Si3N4 the major consolidation routes are reaction bonding and hot pressing [5]. Reaction-bonding involves nitridation of silicon powder. Hot pressing involves addition of various refractory oxides, such as magnesia (MgO), alumina (Al2O3), and yttria (y2O3). Variations on these processes include a number of routes including Hot Isostatic Pressing (HIP), gas-pressure sintering, sinter-HIPing, and Encapsulation-HIPing. It is important to note that each process involves the addition of secondary elements, which later were shown to dramatically influence oxidation and corrosion behavior. As dense bodies of silicon-based ceramics became more readily available, their desirable high temperature properties were confirmed. These materials retained strength to very high temperatures (i.e. 1300-1400 C). Further, they were lightweight and made from abundant materials. SiC and Si3N4 therefore emerged as leading ceramic candidates for components in heat engines, designed to operate at higher temperatures for better performance and fuel efficiency. The first US programs for ceramics in heat engines have been reviewed [6]. Selected programs on ceramic engine parts are summarized here in regard to their contributions to understanding the corrosion behavior of a heat engine environment.

Jacobson, Nathan S.↗

NASA NTRS1995

Thermomechanical Fatigue Behavior of Three Cfcc's

The thermomechanical fatigue (TMF) behavior of three continuous-fiber ceramic composites (CFCC's) was examined. The three matrices consisted of two different glass-ceramics and silicon carbide, respectively. The matrices of some of the specimens with the silicon carbide matrix were enhanced to improve oxidation resistance. All three were reinforced with Nicalon fibers with various fiber architectures. The thermoelastic properties of the matrix relative to the fibers, the elastic moduli and coefficients of thermal expansion (CTE), were different in each composite, providing a comparison of the effects of these critical properties. The specimens were tested under in-phase (IP) and out-of-phase (OP) cyclic loadings with respect to thermal cycling between 600 C and 1100 C. One of the glass-ceramic composites had greatly increased TMF lives compared to the other glass-ceramic matrix composites. This was probably caused by the reversal of the CTE mismatch between the fibers and the matrices and caused by the different oxidation resistances of the composites. For the same TMF lives a cross-ply reinforced composite had a maximum cyclic stress half as great, as that of unidirectionally reinforced composite. This indicated that the (0 deg) ply fibers had a strong influence of TMF life. Both the glass ceramic matrix composites had shallow-slope stress-life plots that indicated sensitivity to damage and therefore low damage tolerance. The composites with an unenhanced silicon carbide matrix experienced the shortest TMF lives of all the CFCC's tested. However, the enhanced composite had the longest. Also, the enhanced composite demonstrated the best damage tolerance as evidenced by a stress-life curve that curves sharply upward to the left. In all the composites, out-of-phase cyclic loading was worse than in-phase cyclic loadings despite the CTE mismatch between fiber and matrix. A damage investigation and a preliminary analysis of the stresses in the fibers and matrices taking into account their respective thermoelastic properties provided insight into the relative behavior of the glass-ceramic matrix composites under IP and OP TMF.

Worthem, Dennis W.↗

NASA NTRS1994

The effect of Low Earth Orbit exposure on some experimental fluorine and silicon-containing polymers

Several experimental fluorine and silicon-containing polymers in film form were exposed to low Earth orbit (LEO) on a Space Shuttle flight experiment (STS-46, Evaluation of Oxygen Interaction with Materials, EOIM-3). The environmental parameters of primary concern were atomic oxygen (AO) and ultraviolet (UV) radiation. The materials were exposed to 2.3 plus or minus 0.1 x 10(exp 20) oxygen atoms/sq cm and 30.6 UV sun hours during the flight. In some cases, the samples were exposed at ambient, 120 C and 200 C. The effects of exposure on these materials were assessed utilizing a variety of characterization techniques including optical, scanning electron (SEM) and scanning tunneling (STM) microscopy, UV-visible (UV-VIS) transmission, diffuse reflectance infrared (DR-FTIR), x-ray photoelectron (XPS) spectroscopy, and in a few cases, gel permeation chromatography (GPC). In addition, weight losses of the films, presumably due to AO erosion, were measured. The fluorine-containing polymers exhibited significant AO erosion and exposed films were diffuse or 'frosted' in appearance and consequently displayed dramatic reductions in optical transmission. The silicon-containing films exhibited minimum AO erosion and the optical transmission of exposed films was essentially unchanged. The silicon near the exposed surface in the films was converted to silicate/silicon oxide upon AO exposure which subsequently provided protection for the underlying material. The silicon-containing epoxies are potentially useful as AO resistant coatings and matrix resins as they are readily processed into carbon fiber reinforced composites and cured via electron radiation.

Connell, John W.↗

NASA NTRS1991

Space Shuttle Orbiter carbon-carbon oxidation performance

Reusable, oxidation protected reinforced carbon carbon (RCC) has been successfully flown on forty Shuttle Orbiter flights. Thermal testing of the silicon carbide coated, reinforced carbon-carbon to determine its oxidation characteristics has been performed in both radiant and convective (plasma arc jet) heating test facilities. Subsurface oxidation of the RCC substrate as a result of oxygen penetrating micro cracks (fizzures) in the coating was characterized as a function of temperature and pressure for both convective and radiant environments. High temperature testing was performed to establish coating recession for over-temperature flight conditions experienced on abort trajectories. Suggested methods for using these test data to establish multi-mission reuse (i.e., mission life) and single mission limits are presented.

Curry, D. M.↗

NASA NTRS1996

Porous silicon carbide (SIC) semiconductor device

Porous silicon carbide is fabricated according to techniques which result in a significant portion of nanocrystallites within the material in a sub 10 nanometer regime. There is described techniques for passivating porous silicon carbide which result in the fabrication of optoelectronic devices which exhibit brighter blue luminescence and exhibit improved qualities. Based on certain of the techniques described porous silicon carbide is used as a sacrificial layer for the patterning of silicon carbide. Porous silicon carbide is then removed from the bulk substrate by oxidation and other methods. The techniques described employ a two-step process which is used to pattern bulk silicon carbide where selected areas of the wafer are then made porous and then the porous layer is subsequently removed. The process to form porous silicon carbide exhibits dopant selectivity and a two-step etching procedure is implemented for silicon carbide multilayers.

Shor, Joseph S.↗

NASA NTRS1995

Method of fabricating porous silicon carbide (SiC)

Shor, Joseph S.↗

DOE OSTI2020

Enhanced Interfacial Stability of Si Anodes for Li-Ion Batteries via Surface SiO2 Coating

Silicon is a promising alloying anode for lithium-ion batteries owing to its high capacity and low cost. However, its use has been hampered by mechanical failure arising from the large volume change upon cycling and by an insufficiently stable solid-electrolyte interphase (SEI). SEI formation depends on the Si surface, which is often an oxide (SiO x ). In this study we compare three different Si surfaces using Si wafers: 1.3 nm native SiO x , 1.4 nm thermally grown SiO2, and a SiOx-free surface. The oxide-free surface showed the worst electrochemical performance, never exceeding 94% Coulombic efficiency (CE). Furthermore, it also exhibited the thickest SEI and the highest overpotential for lithiation, which correlated with uninhibited electrolyte reduction and the incorporation of P-F species into the SEI. The oxide-coated surfaces performed significantly better, demonstrating a CE above 99% beyond the second cycle, low overpotential for lithiation, and a thinner and more stable SEI. The oxides lower the onset potential for electrolyte reduction, and yield an SEI with fewer P-F species. However, it was found that the CE with the native oxide surface decays from the fifth cycle onwards and correlates with a resurgence of electrolyte reduction. A 1-2 nm thermal SiO 2 coating is optimum for achieving a stable SEI that minimizes side reactions and sustains efficient cycling.

25 ENERGY STORAGE↗

NASA NTRS1995

Thermo-Oxidative Degradation Of SiC/Si3N4 Composites

Experimental study conducted on thermo-oxidative degradation of composite-material specimens made of silicon carbide fibers in matrices of reaction-bonded silicon nitride. In SiC/Si3N4 composites of study, interphase is 3-micrometers-thick carbon-rich coat on surface of each SiC fiber. Thermo-oxidative degradation of these composites involves diffusion of oxygen through pores of composites to interphases damaged by oxidation. Nondestructive tests reveal critical exposure times.

Baaklini, George Y.↗

NASA NTRS1979

A New Method of Metallization for Silicon Solar Cells

A low cost ohmic contact on silicon solar cells based on molybdenum-tin metal systems was developed. The approach is based on the formulation of a screenable ink composed from molybdenum oxide and tin mixture. The reduction of Mo03 into Mo and the establishment of Mo 03:Sn ratio is studied. Both tasks were done in an experimental station constructed for this purpose. The results show that molybdenum was formed from its oxide at 800 C. and improved in bonding to silicon at 900 C. A 20% Mo03-80%Sn mixture was converted into metallic coating within this temperature range.

Macha, M.↗

NASA NTRS1982

Ellipsometric studies of sputtered silicon nitride on n-GaAs

Ellipsometry, which is the study of optical systems through their effect on polarized light, is a nondestructive technique offering extremely high sensitivity and in situ operation. One of the intriguing possibilities is to make use of the high sensitivity of ellipsometry for studying the very thin interface between an insulating film and a semiconductor substrate. Researchers have been especially interested in native or anodic oxides. In a recent study, Aspnes and Theeten used ellipsometry to study the interface between silicon and its thermally grown oxide, SiO2. These authors were able to conclude that the interface consisted of a 7 +/- 2 A graded region of atomically mixed silicon and oxygen. In this paper we report both analysis and experimental results for the system: sputtered silicon nitride on (100) n-type gallium arsenide.

Peng, Y. K.↗

DOE OSTI2026

Ammonia Synthesis by a Supported Iron-Lithium Hydride Precatalyst: Silicon Nitride Support Enabled Synthesis and Nitrogen Reservoir Dynamics

Amorphous silicon nitride (Si 3 N 4 ) is an unconventional support for the chemisorption of organometallic complexes and offers potential improvements in active site stability and reactivity through enhanced metal-nitrogen covalency and orbital overlap in bonding interactions with the nitride framework. Here, we show that silicon nitride-supported iron mesityl complexes display divergent reactivity compared to their silica-supported homologues, resisting metallic particle formation under reducing pretreatment conditions (exposure to excess organolithium reagents) and maintaining active iron/lithium speciation under ammonia synthesis conditions that is absent on the oxide support. When the organometallic iron complex on silicon nitride is exposed to excess n-butyllithium, iron remains isolated, catalyzing the conversion of butyllithium to lithium hydride, resulting in a divalent iron site in a polyhydride environment. In contrast, the silica-supported complex is converted to reduced iron clusters without forming persistent isolated hydrides. These structural differences lead to markedly different catalytic behaviors under ammonia synthesis conditions. The Li/Fe/Si 3 N 4 catalyst is highly active (7.5 mol NH 3 /mol Fe/h at 300 °C, 10 bar, or 46 mol NH 3 /mol Fe/h at 400 °C, 10 bar), while both the silica-supported analog and the nonlithiated Si 3 N 4 -supported species are inactive. Notably, this activity is enhanced relative to previously reported iron-lithium hydride composite catalysts (0.43–4.1 mol NH 3 /mol Fe/h at 300 °C, 10 bar) and relative to the industrial benchmark promoted iron catalyst KM1 (3.0 mol NH 3 /mol Fe/h at 400 °C, 10 bar). The catalyst activation and LiH/LiNH x nitrogen reservoir dynamics for Li/Fe/Si 3 N 4 are studied by X-ray Absorption, Mössbauer, and in situ DRIFT spectroscopies and isotopic exchange kinetics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗