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Germanium and GaAs crystals were investigated for studies on photovoltaic effects, chemical etching and epitaxial growth according to the overall objective to assess the defect structure of single crystalline materials. A brief survey of basic theory and topographical techniques is provided; examples of topographs are presented.
Experiments on containerless crystal growth from the melt were conducted during Skylab missions SL3 and SL4 (Skylab Experiment M-560). Six samples of InSb were processed, one of them heavily doped with selenium. The concept of the experiment is discussed and related to general crystal growth methods and their merits as techniques for containerless processing in space. The morphology of the crystals obtained is explained in terms of volume changes associated with solidification and wetting conditions during solidification. All samples exhibit extremely well developed growth facets. Analysis by X-ray topographical methods and chemical etching shows that the crystals are of high structural perfection. Average dislocation density as revealed by etching is of the order of 100 per sq cm; no dislocation clusters could be observed in the space-grown samples. A sequence of striations that is observed in the first half of the selenium-doped sample is explained as being caused by periodic surface breakdown.
Thick-sputtered S-Monel, silver, and 304 stainless steel coatings were deposited on mica and metal substrates with various surface finishes to investigate the nodular growth in the coating by scanning electron microscopy. The geometry and the surface structure of the nodules are characterized. Compositional changes within the coating were analyzed by energy dispersive X-ray analysis. Defects in the surface finish (i.e., scratches, inclusions, etc.), act as preferential nucleation sites and form isolated and complex nodules and various surface overgrowths in the coating. The nodule boundaries are very vulnerable to chemical etching and these nodules do not disappear after full annealing. Further, they have undesirable effects on mechanical properties; cracks are initiated at the nodules when the coating is stressed by mechanical forces. These effects are illustrated by micrographs. Nodular growth within a coating can be minimized or eliminated by increasing the surface smoothness.
Three vapor transport experiments on multicomponent systems were performed during the Apollo Soyuz mission to determine the effects of microgravity forces on crystal morphology and mass transport rates. The mixed systems used germanium selenide, tellurium, germanium tetraiodide (transport agent), germanium monosulfide, germanium tetrachloride (transport agent), and argon (inert atmosphere). The materials were enclosed in evacuated sealed ampoules of fused silica and were transported in a temperature gradient of the multipurpose electric furnace onboard the Apollo Soyuz spacecraft. Preliminary evaluation of 2 systems shows improved quality of space grown crystals in terms of growth morphology and bulk perfection. This conclusion is based on a direct comparison of space grown and ground based crystals by means of X-ray diffraction, microscopic, and chemical etching techniques. The observation of greater mass transport rates than predicted for a microgravity environment by existing vapor transport models indicates the existence of nongravity caused transport effects in a reactive solid/gas phase system.
An ultrasonic cavitation method for restoring obliterated serial numbers has been further explored by application to articles involved in police cases. The method was applied successfully to gun parts. In one case portions of numbers were restored after prior failure by other laboratories using chemical etching techniques. The ultrasonic method was not successful on a heavily obliterated and restamped automobile engine block, but it was partially successful on a motorcycle gear-case housing. Additional studies were made on the effect of a larger diameter ultrasonic probe, and on the method's ability to restore numbers obliterated by peening.
Sputtered S-Monel, silver, and 304 stainless steel coatings and molybdenum disulfide coatings were deposited on mica and metal substrates with various surface finishes to investigate the structural growth of the coating by scanning electron microscopy. The geometry and the surface morphology of the nodules are characterized. Compositional changes within the coating were analyzed by energy dispersive X-ray analysis. Defects in the surface finish act as preferential nucleation sites and form isolated overlapping and complex nodules and various unusual surface overgrowths on the coating. The nodule boundaries are very vulnerable to chemical etching and these nodules do not disappear after full annealing. Further, they have undesirable effects on mechanical properties; cracks are initiated at the nodules when the coating is stressed by mechanical forces.
Recent advances in solar cell technology have led to the development of laboratory cells with efficiencies above 15% and production cells with efficiencies in the area of 13%. The increased output is largely the result of increases in the short-circuit current. The most significant gain in the amount of light entering the cell has been obtained through surface texturing by chemical etching techniques. Sheet resistances resulting from phosphorus diffusion in the 800 C temperature range yield junction depths on the order of 0.1 micrometer, leading to significant increases in the blue region of the cell spectral response. The inclusion of a back surface field in 10 ohm-cm cells has produced an increase in open-circuit voltage of about 50 mV and an increase in the minority carrier lifetime. It appears that a low emitter efficiency of the diffused region is the cause of poor voltages. Future research will be primarily directed toward correcting this deficiency and toward the development of low cost production methods.
Boron-on-tungsten fibers with tensile strength and strain-to-failure values increased by fifty percent over commercial grades are produced by controlled chemical-etching process. Improved fibers have potential applications as lightweight composites in ground vehicles, spacecraft, and rotors for energy storage.
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.
During the months of February and March, work towards the goals of the contract were started as scheduled. The first shipment of thin substrates were received and wafer processing was initiated. The objective of the contract is to investigate, develop and characterize the methods for establishing a production-ready manufacturing process which utilizes thin silicon substrates for solar cells. The thin substrates to be manufactured are three inches diameter, p-type Czochralski wafers of approximately 1 Omega cm resistivity. The wafers are prepared by sawing directly to thickness of 8 mils and 5 mils. To ensure removal of residual saw damage, most substrates are chemically etched to final thicknesses of 7 mils and 4 mils. The thin substrates are used to fabricate solar cells by standard processing techniques.
A miniature gas analysis system has been built based on the principles of gas chromatography (GC). The major components are fabricated in silicon using photolithography and chemical etching techniques, which allows size reductions of nearly three orders of magnitude compared to conventional laboratory instruments. The chromatography system consists of a sample injection valve and a 1.5-m-long separating capillary column, which are fabricated on a substrate silicon wafer. The output thermal conductivity detector is separately batch fabricated and integrably mounted on the substrate wafer. The theory of gas chromatography has been used to optimize the performance of the sensor so that separations of gaseous hydrocarbon mixtures are performed in less than 10 s. The system is expected to find application in the areas of portable ambient air quality monitors, implanted biological experiments, and planetary probes.
The results of a preliminary study of two dendritic web samples are presented. The structure and electrical activity of the defects in the silicon webs were studied. Optical microscopy of chemically etched specimens was used to determine dislocation densities. Samples were mechanically polished, then Secco etched for approximately 5 minutes. High voltage transmission electron microscopy was used to characterize the crystallographic nature of the defects.
Plated silicon wafers with surface roughness ranging from 0.4 to 130 microinches were subjected to tensile pull strength tests. Electroless Ni/electroless Cu/electroplated Cu and electroless Ni/electroplated Cu were the two types of plate contacts tested. It was found that smoother surfaces had higher pull strength than rougher, chemically etched surfaces. The presence of the electroless Cu layer was found to be important to adhesion. The mode of fracture of the contact as it left the silicon was studied, and it was found that in almost all cases separation was due to fracture of the bulk silicon phase. The correlation between surface roughness and mode of contact failure is presented and interpreted.
Processing experiments using wire-saw techniques to slice thin silicon wafers are described. Substrates were sliced directly to 17 mil, 8 mil, and 5 mil thicknesses. Some of the 8 mil substrates and all of the 5 mil substrates were chemically etched to 7 and 4 mils, respectively, to guarantee removal of any saw damage. The wafers wire sawed to 17 mil thicknesses were processed as reference cells. A baseline process which results in an n(+)-p cell structure, and two advanced processes which provide n(+)-p-p(+) structures were utilized. By using a p(+) enhancement layer on the solar cell back surface, the performance of the 7 mil wafers was increased to exceed that of the 17 mil solar cells with simple n(+)-p structures. Cells fabricated by an ion implantation sequence utilizing elemental boron and phosphorus implants were shown to be capable of equalling or exceeding the performance of cells fabricated by an equivalent all-diffusion process.
In connection with the relatively poor insulating characteristics of the native oxides of most III-V compound semiconductors, there has been interest in the development of deposited dielectric layers for surface passivation and MOS device fabrication on III-V compound semiconductor substrates. The chemical system of SiO2 deposited on single-crystal InSb substrates has been proposed for the fabrication of IR CCD. The considered investigation is concerned with a detailed examination of the chemical nature of the interactions between deposited and native oxides using X-ray photoelectron spectroscopy (XPS) in conjunction with a chemical-etching technique for depth profiling. The compositional structure of the interfaces obtained in the SiO2/native oxide/InSb system is derived on the basis of an intensity analysis of XPS spectra. Thermal oxidation of the InSb substrate is found to result in an In-rich native oxide and excess elemental Sb at the native oxide/substrate interface.
A study of the arc discharge patterns and resultant damage patterns on thin Mylar films exposed to a 20 keV electron beam is described. In particular, it is established that there is a broad directional correlation among the directions associated with visible linear arcs, damage tracks, the 'slow' optical direction and the longitudinal marks left on the films surface as a result of chemical etching. Transverse etch marks also appear to be associated with secondary groups of damage track directions. The 'fast' optical direction is associated with the absence of visible arcs or arc damage.
Dust from several comets can be returned to earth with minimum propulsion effort after a high-speed encounter. The collection concept involves the capture of individual dust particles by condensation in a cell after vaporization by a thin diaphragm. This collection concept has been validated in laboratory tests. To compensate for the slower laboratory velocities in a two-stage light-gas gun, higher-density metals (Zn and Cd) have been used for particles and diaphragms to simulate hypervelocity vaporization. Teflon has proved to be a suitable material for the collection cell; more than 50 percent of the vaporized projectile material has been recovered by chemical etching from such cells. Hypervelocity-impact parameters (such as diaphragm-to-projectile ratio, hole size, and plume angles) determined by tests permit the modification of existing analytical models. These new findings are necessary for flyby cometary experiments.
Deformed chondrules in the Leoville carbonaceous chondrite define a preferred orientation, also recognized previously in other CV3 chondrites. Identifying the strain mechanism is necessary for understanding the conditions which caused this compressional shortening. Luckly, the major mineralogical constituent of CV3 meteorites is olivine, for which experimental data on strain mechanisms exist. The conditions that caused strain in the olivine were obviously applicable to the whole meteorite. Possible mechanisms of olivine deformation are cataclasis, low temperature plasticity, power low creep, and diffusional flow, each of which occurs under different combinations of temperature and deviatoric stress. Cataclasis can be ruled out on the basis of its high deviatoric stress requirements; some fractures occur in chondrule olivines, but these may have formed during excavation or impact. Low temperature plasticity and power low creep occur by means of various types of lattice dislocations. However, methods of thermal decoration and chemical etching of dislocations failed to indicate evidence for either mechanism. Thus, the inference is that diffusional flow, characteristic of low to moderately high temperatures and low deviatoric stress, was the major deformation mechanism.