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A Process Development Unit (PDU), which consisted of the four major units of the process, was designed, installed, and experimentally operated. The PDU was sized to 50MT/Yr. The deposition took place in a fluidized bed reactor. As a consequences of the experiments, improvements in the design an operation of these units were undertaken and their experimental limitations were partially established. A parallel program of experimental work demonstrated that Zinc can be vaporized for introduction into the fluidized bed reactor, by direct induction-coupled r.f. energy. Residual zinc in the product can be removed by heat treatment below the melting point of silicon. Current efficiencies of 94 percent and above, and power efficiencies around 40 percent are achievable in the laboratory-scale electrolysis of ZnCl2.

The construction and operation of an experimental process system development unit (EPSDU) for the production of granular semiconductor grade silicon by the zinc vapor reduction of silicon tetrachloride in a fluidized bed of seed particles is presented. The construction of the process development unit (PDU) is reported. The PDU consists of four critical units of the EPSDU: the fluidized bed reactor, the reactor by product condenser, the zinc vaporizer, and the electrolytic cell. An experimental wetted wall condenser and its operation are described. Procedures are established for safe handling of SiCl4 leaks and spills from the EPSDU and PDU.

The initial effort on feasibility of the closed cycle process was begun with the design of the two major items of untested equipment, the silicon tetrachloride by product converter and the rotary drum reactor for deposition of silicon from trichlorosilane. The design criteria of the initial laboratory equipment included consideration of the reaction chemistry, thermodynamics, and other technical factors. Design and construction of the laboratory equipment was completed. Preliminary silicon tetrachloride conversion experiments confirmed the expected high yield of trichlorosilane, up to 98 percent of theoretical conversion. A preliminary solar-grade polysilicon cost estimate, including capital costs considered extremely conservative, of $6.91/kg supports the potential of this approach to achieve the cost goal. The closed cycle process appears to have a very likely potential to achieve LSA goals.

Refinements of the design of the 50 MT/year Experimental Process System Development Unit were made and competitive bids were received from mechanical, electrical, and structural contractors. Bids on most of the equipment were received and cataloged. Emergency procedures were defined to counter a variety of contingencies disclosed in operations and safety reviews. Experimental work with an electrolytic cell for zinc chloride disclosed no significant increase in power efficiency by steps taken to increase electrolyte circulation. On the basis of materials compatibility and permeability tests, 310 stainless steel was chosen for the shell of the fluidized-bed reactor and SiC-coated graphite for the liner.

A miniplant, consisting of a 5 cm-diameter fluidized-bed reactor and associated equipment was used to study the deposition parameters, temperature, reactant composition, seed particle size, bed depth, reactant throughput, and methods of reactant introduction. It was confirmed that the permissible range of fluidized-bed temperature was limited at the lower end by zinc condensation (918 C) and at higher temperatures by rapidly decreasing conversion efficiency. Use of a graded bed temperature was shown to increase the conversion efficiency over that obtained in an isothermal bed. Other aspects of the process such as the condensation and fused-salt electrolysis of the ZnCl2 by-product for recycle of zinc and chlorine were studied to provide information required for design of a 50 MT/year experimental facility. In view of the favorable technical and economic indications obtained, it was recommended that construction and operation of the 50 MT/year experimental facility be implemented.

Progress from October 1, 1977, through December 31, 1977, is reported in the design of the 50 MT/year experimental facility for the preparation of high purity silicon by the zinc vapor reduction of silicon tetrachloride in a fluidized bed of seed particles to form a free flowing granular product.

Potential designs for an integrated fluidized-bed reactor/zinc vaporizer/SiCl4 preheater unit are being considered and heat-transfer calculations have been initiated on versions of the zinc vaporizer section. Estimates of the cost of the silicon prepared in the experimental facility have been made for projected capacities of 25, 50, 75, and 100 metric ton of silicon. A 35 percent saving is obtained in going from 25 metric ton/year to the 50 metric ton/year level. This analysis, coupled with the recognition that use of two reactors in the 50 metric ton/year version allows for continued operation (at reduced capacity) with one reactor shut down, has resulted in a recommendation for adoption of an experimental facility capacity of 50 metric ton/year or greater. At this stage, the change to a larger size facility would not increase the design costs appreciably. In the experimental support program, the effects of seed bed particle size and depth were studied, and operation of the miniplant with a new zinc vaporizer was initiated, revealing the need for modification of the latter.

Low temperature ductility and high temperature strength of pure chromium and chromium-thoria alloy prepared from vapor deposited powders