Abstract Silicon of high purity is made by decomposing silane in a fluidized bed reactor. To obtain good process economics, two modes of operation are used. In a first mode, the reactor is operated under high productivity conditions which also result in co-production of silicon dust or fines. The dust on the particles can cause problems in handling. For example, in bagging the particles, or removing the particles from a bag, the dust can become airborne from the larger particle surfaces and form an objectionable cloud of silicon dust. The invention provides a method for uniting dust to the larger silicon particles. In a second process mode, a thin (0.1-5.0 micron) layer of high purity silicon is deposited on the dust laden particles. This second mode is most preferably carried out by (a) treating the dust-laden particles with a deposition gas comprising 1 to 5 mole % silicon admixed with an inert carrier gas such as hydrogen, (b) in a fluidized bed reactor, and (c) at a process temperature of 620°-650° C. The product polysilicon is composed of free flowing, approximately spherical particles having a size distribution of 150-1500 microns, an average size of 650- 750 microns and has a particle bulk density of 2.3 grams per cubic centimeter, a bulk density of about 1360 kg/m 3 and a silicon surface dust content of less than 0.08 wt. %.
A process comprising the step of intimately contacting: (a) a bed of particles of silicon maintained: (i) in a vertically disposed reaction zone, and (ii) at a reaction temperature higher than the thermal decomposition temperature of silane with; (b) silane contained in a first and second decomposition gas, each of said deposition gases being introduced into said bed of particles at a flow rate sufficient to maintain said bed in a fluidized state within said reaction zone, said first deposition gas being introduced for a first deposition period and being a mixture of about 10 to about 15 mole percent silane in hydrogen, said second deposition gas being introduced for a second deposition period beginning substantially immediately after the termination of said first deposition period, and being a mixture of about 1 to 5 mole percent silane in hydrogen, said process being further characterized in that said first deposition period is from about 2 to about 5 times as long in time duration as said second deposition period, such that polysilicon in the form of approximately spherical particles is produced, said particles having (i) a size distribution of from 400 to 100 microns; (ii) an average size of 650 to 750 microns; (iii) a boron content of no more than 0.25 ppba; (iv) a phosphorus content of no more than 0.19 ppba; (v) a carbon content of no more than 0.33 ppm; and (vi) a surface dust content less than about 0.08 weight percent bonded to said particles by a silicon layer in the range of 0.1 to about 5 microns in thickness.
Claim 2
Dependent Claim
263 words
A process comprising the step of intimately contacting: (a) a bed of particles of silicon maintained: (i) in a vertically disposed reaction zone, and (ii) at a reaction temperature higher than the thermal decomposition temperature of silane with; (b) silane contained in a first and second decomposition gas, each of said deposition gases being introduced into said bed of particles at a flow rate sufficient to maintain said bed in a fluidized state within said reaction zone, said first deposition gas being introduced for a first deposition period and being a mixture of about 10 to about 15 mole percent silane in hydrogen, said second deposition gas being introduced for a second deposition period beginning substantially immediately after the termination of said first deposition period, and being a mixture of about 1 to 5 mole percent silane in hydrogen, said process being further characterized in that said first deposition period is from about 2 to about 5 times as long in time duration as said second deposition period, such that polysilicon in the form of approximately spherical particles is produced, said particles having (i) a size distribution of from 400 to 100 microns; (ii) an average size of 650 to 750 microns; (iii) a boron content of no more than 0.25 ppba; (iv) a phosphorus content of no more than 0.19 ppba; (v) a carbon content of no more than 0.33 ppm; and (vi) a surface dust content less than about 0.08 weight percent bonded to said particles by a silicon layer in the range of 0.1 to about 5 microns in thickness.
Claim 3
Dependent Claim
25 words
A process of claim 1 further characterized by producing said approximately spherical particles such that said silicon layer is 0.1 to 1.0 micron in thickness.