Processing of fine silicon powder to produce bulk silicon
View Patent ↗A method for using substantial quantities of silicon powders as charge and processing it to produce a high quality silicon ingots suitable for photovoltaic use is disclosed. In a fused silica crucible, silicon feedstock containing more than about 5% by weight silicon powder is charged. The crucible with the charged silicon feedstock is placed into a furnace chamber and a vacuum is drawn to remove air. The vacuum is applied slowly. Then, the furnace chamber is backfilled with argon gas and heated to form molten silicon. Afterward, the molten silicon is solidified and annealed to form a multicrystalline silicon ingot.
1. A method for making multicrystalline silicon ingots suitable for photovoltaic use comprises:
providing a fused silica crucible,
charging the crucible with silicon feedstock comprising more than about 5% by weight silicon powder of less than about 20 microns in size,
placing the crucible with the charged silicon feedstock into a furnace chamber,
drawing a vacuum on the furnace chamber to remove air, the vacuum being applied by reducing the pressure in the range of about 8-15 mBar/min,
heating the furnace chamber, crucible and silicon feedstock to melt the silicon,
solidifying the molten silicon to form multicrystalline silicon, and
cooling the multicrystalline silicon.
2. The method of claim 1 , further comprising, before heating, placing the crucible in a box having a graphite bottom plate and graphite side plates, the box further comprising a graphite top plate having a central opening, wherein the side plates also have openings.
3. The method of claim 2 , further comprising providing argon through the top plate central opening to exit through the side plate openings.
4. The method of claim 3 , further comprising providing graphite tubes in the furnace chamber to direct the argon from an injection point to the central opening of the top plate.
5. The method of claim 1 , further comprising after reaching a furnace temperature of about 1000° C., the heating rate is maintained at a rate about 4-6° C./minute.
6. The method of claim 1 , further comprising after the heating step, backfilling with argon, and after a partial solidification during the solidifying step, applying another vacuum to evacuate the furnace chamber and crucible.
7. The method of claim 1 , further comprising two heating steps, wherein after the first heating step, backfilling with argon, applying another vacuum to evacuate the furnace chamber and crucible again, then, backfilling a second time with argon and providing a second heating step.
8. A method for making multicrystalline silicon ingots suitable for photovoltaic use comprises:
providing a fused silica crucible having a silicon nitride coating,
charging the crucible with silicon feedstock comprising bulk silicon pieces and more than about 5% by weight silicon powder of less than about 20 microns in size,
placing the crucible with the charged silicon feedstock into a furnace chamber,
drawing a vacuum on the furnace chamber to remove air, the vacuum being applied by reducing the pressure in the range of about 8-15 mBar/min,
heating the furnace chamber, crucible and silicon feedstock to melt the silicon,
backfilling the furnace chamber with argon gas,
continued heating the furnace chamber, crucible and silicon feedstock to completely melt the silicon,
solidifying the molten silicon to form multicrystalline silicon, and
annealing the multicrystalline silicon.
9. The method of claim 8 , wherein the furnace is a component of a directional solidification system, and further comprising applying a further vacuum after solidification of the silicon is at least about 80% complete.
10. The method of claim 8 , further comprising, before heating, placing the crucible in a box having a graphite bottom plate and graphite side plates, the box further comprising a graphite top plate having a central opening, wherein the side plates also have openings so that argon entering through the top plate central opening can exit through the side plate openings, and wherein the argon entering the furnace chamber is directed to the central opening of the top plate.
11. The method of claim 8 , further comprising, before heating, placing the crucible in a box having a graphite bottom plate and graphite side plates, the box further comprising a graphite top plate having a central opening, wherein the side plates also have openings.
12. The method of claim 11 , further comprising providing argon through the top plate central opening to exit through the side plate openings.
13. The method of claim 12 , further comprising providing graphite tubes in the furnace chamber to direct the argon from an injection point to the central opening of the top plate.
14. The method of claim 8 , further comprising after backfilling with argon, applying another vacuum to evacuate the furnace chamber and crucible again and, then, backfilling a second time with argon.