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The various steps involved in obtaining quantitative information of structural defects in crystalline silicon samples are described. Procedures discussed include: (1) chemical polishing; (2) chemical etching; and (3) automated image analysis of samples on the QTM 720 System.
The JPL Continuous Czochralski Growth Facility is now essentially complete and is functional. In this reporting period, a silicon lump recharging device was designed, and a prototype was built which performed well in simulated recharge tests. The large chamber (designed to accommodate a 14-inch hot zone) was put into operation initially with the standard hot zone in order to compare performance with previous experience. Some modifications were made to the hot zones in the larger chamber due to considerably larger radiative heat losses. Several short (one-ingot) runs were performed and four continuous runs were attempted. The largest continuous run lasted 64 hours and produced 57 kilograms of ingot.
The various steps involved in the chemical polishing and etching of silicon samples are described and the data on twins, grain boundaries and dislocation pits from fifty-three (53) samples are discussed.
One hundred and seventy four silicon sheet samples were analyzed for twin boundary density, dislocation pit density, and grain boundary length. Procedures were developed for the quantitative analysis of the twin boundary and dislocation pit densities using a QTM-720 Quantitative Image Analyzing system. The QTM-720 system was upgraded with the addition of a PDP 11/03 mini-computer with dual floppy disc drive, a digital equipment writer high speed printer, and a field-image feature interface module. Three versions of a computer program that controls the data acquisition and analysis on the QTM-720 were written. Procedures for the chemical polishing and etching were also developed.
The exposure of silicones to atomic oxygen in low Earth orbit causes oxidation of the surface, resulting in conversion of silicone to silica. This chemical conversion increases the elastic modulus of the surface and initiates the development of a tensile strain. Ultimately, with sufficient exposure, tensile strain leads to cracking of the surface enabling the underlying unexposed silicone to be converted to silica resulting in additional depth and extent of cracking. The use of silicone coatings for the protection of materials from atomic oxygen attack is limited because of the eventual exposure of underlying unprotected polymeric material due to deep tensile stress cracking of the oxidized silicone. The use of moderate to high volatility silicones in low Earth orbit has resulted in a silicone contamination arrival at surfaces which are simultaneously being bombarded with atomic oxygen, thus leading to conversion of the silicone contaminant to silica. As a result of these processes, a gradual accumulation of contamination occurs leading to deposits which at times have been up to several microns thick (as in the case of a Mir solar array after 10 years in space). The contamination species typically consist of silicon, oxygen and carbon. which in the synergistic environment of atomic oxygen and UV radiation leads to increased solar absorptance and reduced solar transmittance. A comparison of the results of atomic oxygen interaction with silicones and silicone contamination will be presented based on the LDEF, EOIM-111, Offeq-3 spacecraft and Mir solar array in-space results. The design of a contamination pin-hole camera space experiment which uses atomic oxygen to produce an image of the sources of silicone contamination will also be presented.
A novel gate insulator consisting of silicon dioxide (SiO2) with a thin silicon (Si) interfacial layer has been investigated for high-power microwave indium phosphide (InP) metal-insulator-semiconductor field effect transistors (MISFETs). The role of the silicon interfacial layer on the chemical nature of the SiO2/Si/InP interface was studied by high-resolution X-ray photoelectron spectroscopy. The results indicated that the silicon interfacial layer reacted with the native oxide at the InP surface, thus producing silicon dioxide, while reducing the native oxide which has been shown to be responsible for the instabilities in InP MISFETs. While a 1.2-V hysteresis was present in the capacitance-voltage (C-V) curve of the MIS capacitors with silicon dioxide, less than 0.1 V hysteresis was observed in the C-V curve of the capacitors with the silicon interfacial layer incorporated in the insulator. InP MISFETs fabricated with the silicon dioxide in combination with the silicon interfacial layer exhibited excellent stability with drain current drift of less than 3 percent in 10,000 sec, as compared to 15-18 percent drift in 10,000 sec for devices without the silicon interfacial layer. High-power microwave InP MISFETs with Si/SiO2 gate insulators resulted in an output power density of 1.75 W/mm gate width at 9.7 GHz, with an associated power gain of 2.5 dB and 24 percent power added efficiency.
For reaction-formed silicon carbide (RFSC) ceramics produced by silicon melt infiltration of porous carbon preforms, equations are developed to relate the amount of residual silicon to the initial carbon density. Also, for a slurry derived preform containing both carbon and silicon powder, equations are derived which relate the amount of residual silicon in the RFSC to the relative density of the carbon in the preform and to the amount of silicon powder added to the slurry. For a porous carbon preform that does not have enough porosity to prevent choking-off of the silicon infiltration, these results show that complete silicon infiltration can occur by adding silicon powder to the slurry mixture used to produce these preforms.
The volumetric changes of silicon electrodes, along with the strong adhesive properties of certain binders, can lead to plastic deformation of the current collector and create damage in the electrode coating. Here, in this study, we report a detailed study of silicon coatings on a high-tensile alloy (HTA) foil of copper with strength over twice that of conventional copper foils. The HTA current collectors with high mechanical strength can mitigate plastic deformation upon continuous cycling. At moderate areal capacities (2.5–3 mAh cm −2 ), conventional copper foils show significant wrinkling after only a few electrochemical cycles, whereas the HTA foils remain intact. We demonstrate viability of the HTA foils in large format xx6395 pouch cells, in which the HTA current collectors remain intact even at an areal capacity of 4.5 mAh cm −2 ; in contrast, wrinkles form in conventional copper current collectors increasing the likelihood of lithium plating. Computational studies show that stresses generated during cycling of silicon electrodes are very high in the current collector and at the current collector-coating interface, explaining the wrinkling of conventional Cu foils. Our studies highlight importance of current collector to solve the electrochemical and chemo-mechanical performance challenges associated with high-loading silicon electrodes.
The evaporation coefficient and equilibrium vapor pressure of silicon monoxide over a mixture of silicon and vitreous silica have been studied over the temperature range (1433 to 1608) K. The evaporation coefficient for this temperature range was (0.007 plus or minus 0.002) and is approximately an order of magnitude lower than the evaporation coefficient over amorphous silicon monoxide powder and in general agreement with previous measurements of this quantity. The enthalpy of reaction at 298.15 K for this reaction was calculated via second and third law analyses as (355 plus or minus 25) kJ per mol and (363.6 plus or minus 4.1) kJ per mol respectively. In comparison with previous work with the evaporation of amorphous silicon monoxide powder as well as other experimental measurements of the vapor pressure of silicon monoxide gas over mixtures of silicon and silica, these systems all tend to give similar equilibrium vapor pressures when the evaporation coefficient is correctly taken into account. This provides further evidence that amorphous silicon monoxide is an intimate mixture of small domains of silicon and silica and not strictly a true compound.
A saturated solution of silicon and an element such as carbon having a segregation coefficient less than unity is formed by placing a solid piece of carbon in a body of molten silicon having a temperature differential decreasing toward the surface. A silicon carbide seed crystal is disposed on a holder beneath the surface of the molten silicon. As a rod or ribbon of silicon is slowly pulled from the melt, a supersaturated solution of carbon in silicon is formed in the vicinity of the seed crystal. Excess carbon is emitted from the solution in the form of silicon carbide which crystallizes on the seed crystal held in the cool region of the melt.
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Experience has shown that different methods of analysis of SiC products give different results. Methods identified as AFNOR, FEPA, and manufacturer P, currently used to detect SiC, free C, free Si, free Fe, and SiO2 are reviewed. The AFNOR method gives lower SiC content, attributed to destruction of SiC by grinding. Two products sent to independent labs for analysis by the AFNOR and FEPA methods showed somewhat different results, especially for SiC, SiO2, and Al2O3 content, whereas an X-ray analysis showed a SiC content approximately 10 points lower than by chemical methods.
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The primary objective of this contract is to develop equipment and methods for the economic production of single crystal ingot material by the continuous Czochralski (CZ) process. Continuous CZ is defined for the purpose of this work as the growth of at least 100 kilograms of ingot from only one melt container. During the reporting period (October, 1977 - September, 1978), a modified grower was made fully functional and several recharge runs were performed. The largest run lasted 44 hours and over 42 kg of ingot was produced. Little, if any, degradation in efficiency was observed as a result of pulling multiple crystals from one crucible. Solar efficiencies observed were between 9.3 and 10.4% AMO (13.0 and 14.6% AMI) compared to 10.5% (14.7% AMI) for optimum CZ material control samples. Using the SAMICS/IPEG format, economic analysis of continuous CZ suggests that 1986 DoE cost goals can only be met by the growth of large diameter, large mass crystals.
Significant progress is reported in fabricating a 4 sq cm cell having a 10.1 percent conversion efficiency and a 10 sq cm cell having a 9.2 percent conversion efficiency. The continuous (SCIM) coater succeeded in producing a 16 sq cm coating exhibiting unidirectional solidification and large grain size. A layer was grown at 0.2 cm/sec in the experimental coater which was partially dendritic but also contained a large smooth area approximately 100 micron m thick. The dark characteristic measurements of a typical SCC solar cell yield shunt resistance values of 10K ohms and series resistance values and 0.4 ohm. The production dip-coater is operating at over 50 percent yield in terms of good cell quality material. The most recent run yielded 13 good substrates out of 15.
During the reporting period, a successful 100 kilogram run was performed. Six ingots of 13 cm diameter were grown, ranging in size from 15.5 kg to 17.7 kg. Melt replenishment methods included both poly rod and lump feed material. Samples from each ingot were prepared for solar cell fabrication and analyses, impurity analysis, and structural studies. The furnace was converted to the 14-inch hot zone and preliminary heat runs were performed. Two sucessful runs were demonstrated, by growing 25 kg ingots from 30 kg melts. Also, a 100 kg run was attempted, utilizing the 14 inch crucible hot zone, but was prematurely terminated due to excessive monoxide which accumulated on the viewports and a seed failure.
Statistically significant quantitative structural imperfection measurements were made on samples from ubiquitous crystalline process (UCP) Ingot 5848 - 13C. Important correlation was obtained between defect densities, cell efficiency, and diffusion length. Grain boundary substructure displayed a strong influence on the conversion efficiency of solar cells from Semix material. Quantitative microscopy measurements gave statistically significant information compared to other microanalytical techniques. A surface preparation technique to obtain proper contrast of structural defects suitable for quantimet quantitative image analyzer (QTM) analysis was perfected and is used routinely. The relationships between hole mobility and grain boundary density was determined. Mobility was measured using the van der Pauw technique, and grain boundary density was measured using quantitative microscopy technique. Mobility was found to decrease with increasing grain boundary density.