Silicon nitride powder for mold release agent of casting mold for casting polycrystalline silicon ingot and method for manufacturing said silicon nitride powder, slurry containing said silicon nitride powder, casting mold for casting polycrystalline silicon ingot and method for manufacturing same, and method for manufacturing polycrystalline silicon ingot using said casting mold

Patent metadata

Field	Value
Publication number	US-2016159648-A1
Application number	US-201414903679-A
Country	US
Kind code	A1
Filing date	Jul 9, 2014
Priority date	Jul 11, 2013
Publication date	Jun 9, 2016
Grant date	—

Abstract

A silicon nitride powder for a release agent of a polycrystalline silicon ingot casting mold, having a specific surface area of 5 to 40 m 2 /g, wherein, assuming that a content ratio of oxygen present in a particle surface layer is FSO (mass %), a content ratio of oxygen present inside a particle is FIO (mass %), and the specific surface area is FS (m 2 /g), FS/FSO is 8 to 30 and FS/FIO is 22 or more, and a ratio D10/D90 between a 10 vol % diameter D10 and a 90 vol % diameter D90 in a measurement of a particle size distribution on a volume basis by a laser diffraction particle size distribution meter of 0.05 to 0.20.

First claim

1 .- 11 . (canceled)

12 . A silicon nitride powder for a release agent of a polycrystalline silicon ingot casting mold, having
a specific surface area of 5 to 40 m 2 /g, wherein, assuming that a content ratio of oxygen present in a particle surface layer is FSO (mass %), a content ratio of oxygen present inside a particle is FIO (mass %), and the specific surface area is FS (m 2 /g),
FS/FSO is 8 to 30 and
FS/FIO is 22 or more,
and a ratio D10/D90 between a 10 vol % diameter D10 and a 90 vol % diameter D90 in a measurement of a particle size distribution on a volume basis by a laser diffraction particle size distribution meter of 0.05 to 0.20.

13 . The silicon nitride powder according to claim 12 , wherein Fe (iron) content is 10 ppm or less.

14 . The silicon nitride powder according to claim 12 , wherein FS/FSO is 15 to 30 and FS/FIO is 30 to 60.

15 . A method of producing the silicon nitride powder of claim 12 , comprising firing an amorphous Si—N(—H)-based compound with a specific surface area of 300 to 1,200 m 2 /g at a temperature of 1,400 to 1,700° C. in a nitrogen-containing inert gas atmosphere or a nitrogen-containing reducing gas atmosphere while flowing said amorphous Si—N(—H)-based compound in a continuous firing furnace, wherein
assuming that a specific surface area of said amorphous Si—N(—H)-based compound is RS (m 2 /g) and an oxygen content ratio is RO (mass %), RS/RO is 100 or more, and
at the time of said firing, said amorphous Si—N(—H)-based compound is heated at a temperature rise rate of 12 to 500° C./min in a temperature range of 1,100 to 1,400° C.

16 . A slurry containing the silicon nitride powder according to claim 12 obtained by mixing the silicon nitride powder with water.

17 . The slurry according to claim 16 , which does not contain a binder.

18 . A method of manufacturing a polycrystalline silicon ingot casting mold having a release layer, comprising:
a slurry forming step of mixing the silicon nitride powder according to claim 12 with water to form a slurry, a slurry applying step of coating a mold surface with said slurry, a slurry drying step of drying said slurry applied onto the mold surface, and a heat treatment step of heating, in an oxygen-containing atmosphere, the mold of which surface is coated with said slurry.

19 . The method according to claim 18 , wherein said slurry does not contain a binder.

20 . The method according to claim 18 , wherein said heat treatment is performed at a temperature of 400 to 800° C.

21 . A polycrystalline silicon ingot casting mold having, on an inner surface of the mold, a release layer composed of the silicon nitride powder according to claim 12 .

22 . A method of manufacturing a polycrystalline silicon ingot comprising:
casting a polycrystalline silicon ingot from a silicon melt with the polycrystalline silicon ingot casting mold according to claim 21 , and removing a cast polycrystalline silicon ingot from said mold.

Assignees

• Ube Industries

Inventors

• Yamao Takeshi
• Honda Michio
• Jida Shinsuke
• Fujii Takayuki

Classifications

• C01B21/068 Primary

  with silicon · CPC title

• C01P2004/51

  Particles with a specific particle size distribution · CPC title

• C01P2006/12

  Surface area · CPC title

• C01B33/021

  Preparation (chemical coating from the vapour phase C23C16/00) · CPC title

• B05D3/0413

  Heating with air · CPC title