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NASA NTRS1977

Low cost silicon solar array project silicon materials task: Establishment of the feasibility of a process capable of low-cost, high volume production of silane (step 1) and the pyrolysis of silane to semiconductor-grade silicon (step 2)

A quartz fluid bed reactor capable of operating at temperatures of up to 1000 C was designed, constructed, and successfully operated. During a 30 minute experiment, silane was decomposed within the reactor with no pyrolysis occurring on the reactor wall or on the gas injection system. A hammer mill/roller-crusher system appeared to be the most practical method for producing seed material from bulk silicon. No measurable impurities were detected in the silicon powder produced by the free space reactor, using the cathode layer emission spectroscopic technique. Impurity concentration followed by emission spectroscopic examination of the residue indicated a total impurity level of 2 micrograms/gram. A pellet cast from this powder had an electrical resistivity of 35 to 45 ohm-cm and P-type conductivity.

Breneman, W. C.↗

NASA NTRS1977

The reduction of SiO2 with carbon in a plasma

The feasibility of a process for the reduction of low impurity silica (SiO2) with carbon in a plasma heat source was investigated. An RF induction plasma reactor was fabricated and used to optimize process variables. Maximum silicon content of the product was 33% by weight. Emission spectrographic analysis of this product showed a reduction in some impurity levels of one to two orders of magnitude. While the plasma approach proved technically feasible, poor heat transfer from the plasma to the reactant and low yield make the process economically unattractive for large-scale use.

Coldwell, D. M.↗

NASA NTRS1978

Laser-zone growth in a Ribbon-To-Ribbon (RTR) process. Silicon sheet growth development for the large area sheet task of the low-cost solar array project

A new calculation of the effects of thermal stresses during growth on silicon ribbon quality is reported. Thermal stress distributions are computed for ribbon growth under a variety of temperature profiles. A growth rate of 55 cu cm/min with a single ribbon was achieved. The growth of RTR ribbon with a fairly uniform parallel dendritic structure was demonstrated. Results with two approaches were obtained for reducing the Mo impurity level in polycrystalline feedstock. Coating the Mo substrate with Si3N4 does not effect thermal shear separation of the polyribbon; this process shows promise of improving cell efficiency and also increasing the useful life of the molybdenum substrate. A number of solar cells were fabricated on RTR silicon grown from CVD feedstock.

Baghdadi, A.↗

NASA NTRS1979

Development and evaluation of die and container materials

X = 0.75 Beta prime Sialon (a silicon aluminum oxynitride) and Sibeon (silicon beryllium oxynitride) are promising die materials. In sessile drop tests in contact with molten silicon, beryllium contamination was less than ppm and aluminum contamination 50 ppm. A shaping die of the Sialon material was successfully fabricated. Dry milling studies for the preparation of Si3N4-Al2O3-ALN mixtures were performed with butanol, acetic anhydride, oleic acid, and triethanolamine milling aids. Optimum mixing was achieved with 0.15 percent triethanolamine using a milling time of 8 hours. Preliminary evaluation of Sibeon materials indicates that they are more resistent to molten silicon attack than Sialon. Silicon contamination from the beryllium was less than aluminum contamination even though the aluminum impurity level in the Sibeon was only 450 to 1300 ppm. Work designed to produce an aluminum-free Sibeon is described.

Wills, R. R.↗

NASA NTRS1981

Bulk lifetime indicates surface contamination

Indirect measurement of wafer surface impurities has sensitivity of 300 monolayers. Photoconductivity-decay apparatus determines bulk recombination lifetime in semiconductor materials. Bulk impurity levels before and after annealing relate to level of surface contamination. Method evaluates wafer cleaning techniques, qualifying purity of chemical and deionized water used, or monitors production process.

Blais, P. D.↗

NASA NTRS1980

Evaluation of present-day thermal barrier coatings for industrial/utility applications

Atmospheric burner rig tests have been conducted to evaluate the corrosion resistance of present-day thermal barrier coatings. The coatings are primarily plasma-sprayed and zirconia-based. Both duplex and graded coating systems were tested at a gas temperature of 2100 F and metal temperatures that range from 1475 F to 1650 F. The fuels ranged from clean GT No. 2 to that doped with impurity levels which simulate water-washed residual fuels. Results to date suggest that liquid sulfate condensates play an important role in the coating degradation mechanisms, whereas the role of vanadium and its salts is less clear.

Bratton, R. J.↗

NASA NTRS1981

Combustion system processes leading to corrosive deposits

Degradation of turbine engine hot gas path components by high temperature corrosion can usually be associated with deposits even though other factors may also play a significant role. The origins of the corrosive deposits are traceable to chemical reactions which take place during the combustion process. In the case of hot corrosion/sulfidation, sodium sulfate was established as the deposited corrosive agent even when none of this salt enters the engine directly. The sodium sulfate is formed during the combustion and deposition processes from compounds of sulfur contained in the fuel as low level impurities and sodium compounds, such as sodium chloride, ingested with intake air. In other turbine and power generation situations, corrosive and/or fouling deposits can result from such metals as potassium, iron, calcium, vanadium, magnesium, and silicon.

Stearns, C. A.↗

NASA NTRS1981

Processing of silicon solar cells by ion implantation and laser annealing

Methods to improve the radiation tolerance of silicon cells for spacecraft use are described. The major emphasis of the program was to reduce the process-induced carbon and oxygen impurities in the junction and base regions of the solar cell, and to measure the effect of reduced impurity levels on the radiation tolerance of cells. Substrates of 0.1, 1.0 and 10.0 ohm-cm float-zone material were used as starting material in the process sequence. High-dose, low-energy ion implantation was used to form the junction in n+p structures. Implant annealing was performed by conventional furnace techniques and by pulsed laser and pulsed electron beam annealing. Cells were tested for radiation tolerance at Spire and NASA-LeRC. After irradiation by 1 MeV electrons to a fluence of 10 to the 16th power per sq cm, the cells tested at Spire showed no significant process induced variations in radiation tolerance. However, for cells tested at Lewis to a fluence of 10 to the 15th power per sq cm, ion-implanted cells annealed in vacuum by pulsed electron beam consistently showed the best radiation tolerance for all cell resistivities.

Minnucci, J. A.↗

NASA NTRS1982

Study of photoconductive indium antimonide

Indium antimonide (InSb) material was assessed for use as photoconductive infrared detectors under low background conditions. Such detectors must be more rugged, and have lower capacitance, than the common photovoltaic InSb detector. Electronic grade n-type InSb was etched to 50 micrometers thickness, and tin and gold contacts were applied by evaporation. The test devices showed a relatively low ultimate impedance: 7 Mohms at 4.2 K. This was attributed to the presence of impurity levels of very shallow energies, and this material was judged unsuitable for low background detection.

Low, F. J.↗

NASA NTRS1983

Combustion system processes leading to corrosive deposits

Stearns, C. A.↗

NASA NTRS1984

Oxygen diffusion in alpha-Al2O3

Oxygen self diffusion coefficients were determined in single crystal alpha-Al2O3 using the gas exchange technique. The samples were semi-infinite slabs cut from five different boules with varying background impurities. The diffusion direction was parallel to the c-axis. The tracer profiles were determined by two techniques, single spectrum proton activation and secondary ion mass spectrometry. The SIMS proved to be a more useful tool. The determined diffusion coefficients, which were insensitive to impurity levels and oxygen partial pressure, could be described by D = .00151 exp (-572kJ/RT) sq m/s. The insensitivities are discussed in terms of point defect clustering. Two independent models are consistent with the findings, the first considers the clusters as immobile point defect traps which buffer changes in the defect chemistry. The second considers clusters to be mobile and oxygen diffusion to be intrinsic behavior, the mechanism for oxygen transport involving neutral clusters of Schottky quintuplets.

Cawley, J. D.↗

NASA NTRS1985

Enhancement of intensity-dependent absorption in InP and GaAs at 1.9 microns by doping

It is pointed out that the study of intensity-dependent absorption (IDA) in general, and two-photon absorption (TPA), in particular, has suffered from experimental difficulties and inadequate theoretical models. Bass et al. (1979) could improve the experimental situation by making use of laser calorimetry to obtain directly the TPA coefficient of a medium with a high degree of sensitivity. In the present investigation, the employed technique has been used to study the effect of deep level dopants on IDA in InP and GaAs. It is found that the coefficient for IDA is strongly dependent on the presence of Fe in InP and Cr in GaAs. The conducted investigation had the objective to examine the effect of deep level impurities on IDA processes in InP and GaAs. Fe-doped InP and Cr-doped GaAs were compared with undoped crystals.

Li, N.-L.↗

NASA NTRS1985

Corrosion of metals by hydrazine

The mechanism of corrosion of metals by hydrazine has been studied by means of coupons in sealed ampoules and by electrochemical techniques. The variables considered were temperature, CO2 impurity level, alloy composition and microcrystalline structure. The coupon studies, to date, verify that increasng temperature and the presence of CO2 does increase the corrosion rate as expected. The presence of molybdenum in stainless steels to the 3 percent level is not necessarily deleterious, contrary to published reports. The influence of microcrystalline structure and surface characteristics are more dominant effects. However, with Ti-6Al-4V, two different microcrystalline structures showed no significant differences. Corrosion rates of CRES 304 L in hydrazine have also been measured by several electrochemical techniques such as Tafel plots, polarization resistance and A. C. Impedance. This is the first documented work to show that A. C. Impedance can be used with non-aqueous solvents. Preliminary data correlated satisfactorily with the results of the coupon studies.

Lawton, E. A.↗

NASA NTRS1985

The effects of surface pretreatment and nitrogen tetroxide purification on the corrosion rate of Type 304L stainless steel

Corrosion rates of 304L stainless steel coupons in MON-1 oxidizer have been measured as a function of cleaning procedures employed, surface layer positions, propellant impurity levels, and short-term exposure durations (14 to 90 days). Of special interest was propellant contamination by buildup of soluble iron, which may cause flow decay. Surface treatments employed were combinations of cleaning, pickling, and passivation procedures. Propellants used were MIL-SPEC MON-1 and several types of purified NTO (i.e., low water, low chloride) which may, at a later time, be specified as spacecraft grade. Pretest coupon surface analysis by X-ray photoelectron spectroscopy (XPS-ESCA) has revealed important differences, for the different cleaning procedures, in the make-up of the surface layer, both in composition and state of chemical combination of the elements involved. Comparisons will be made of XPS/ESCA data, for different cleaning procedures, for specimens before and after propellant exposure.

Blue, G. D.↗

NASA NTRS1986

Solar silicon from directional solidification of MG silicon produced via the silicon carbide route

A process of metallurgical grade (MG) silicon production is presented which appears particularly suitable for photovoltaic (PV) applications. The MG silicon is prepared in a 240 KVA, three electrode submerged arc furnace, starting from high grade quartz and high purity silicon carbide. The silicon smelted from the arc furnace was shown to be sufficiently pure to be directionally solidified to 10 to 15 kg. After grinding and acid leaching, had a material yield larger than 90%. With a MG silicon feedstock containing 3 ppmw B, 290 ppmw Fe, 190 ppmw Ti, and 170 ppmw Al, blended with 50% of off grade electronic grade (EG) silicon to reconduct the boron content to a concentration acceptable for solar cell fabrication, the 99% of deep level impurities were concentrated in the last 5% of the ingot. Quite remarkably this material has OCV values higher tham 540 mV and no appreciable shorts due to SiC particles.

Rustioni, M.↗

NASA NTRS1986

Characterization of solar-grade silicon produced by the SiF4-Na process

A process was developed for producing low cost solar grade silicon by the reaction between SiF4 gas and sodium metal. The results of the characterization of the silicon are presented. These results include impurity levels, electronic properties of the silicon after crystal growth, and the performance of solar photovoltaic cells fabricated from wafers of the single crystals. The efficiency of the solar cells fabricated from semiconductor silicon and SiF4-Na silicon was the same.

Sanjurjo, A.↗

NASA NTRS1988

Amorphous silicon carbide coatings for extreme ultraviolet optics

Amorphous silicon carbide films formed by sputtering techniques are shown to have high reflectance in the extreme ultraviolet spectral region. X-ray scattering verifies that the atomic arrangements in these films are amorphous, while Auger electron spectroscopy and Rutherford backscattering spectroscopy show that the films have composition close to stoichiometric SiC, although slightly C-rich, with low impurity levels. Reflectance vs incidence angle measurements from 24 to 1216 A were used to derive optical constants of this material, which are presented here. Additionally, the measured extreme ultraviolet efficiency of a diffraction grating overcoated with sputtered amorphous silicon carbide is presented, demonstrating the feasibility of using these films as coatings for EUV optics.

Kortright, J. B.↗

NASA NTRS1988

Infrared absorption study of neutron-transmutation-doped germanium

Using high-resolution far-infrared Fourier transform absorption spectroscopy and Hall effect measurements, the evolution of the shallow acceptor and donor impurity levels in germanium during and after the neutron transmutation doping process was studied. The results show unambiguously that the gallium acceptor level concentration equals the concentration of transmutated Ge-70 atoms during the whole process indicating that neither recoil during transmutation nor gallium-defect complex formation play significant roles. The arsenic donor levels appear at full concentration only after annealing for 1 h at 450 C. It is shown that this is due to donor-radiation-defect complex formation. Again, recoil does not play a significant role.

Park, I. S.↗