CA2680780A1 - A coating composition for a mould - Google Patents
A coating composition for a mould Download PDFInfo
- Publication number
- CA2680780A1 CA2680780A1 CA002680780A CA2680780A CA2680780A1 CA 2680780 A1 CA2680780 A1 CA 2680780A1 CA 002680780 A CA002680780 A CA 002680780A CA 2680780 A CA2680780 A CA 2680780A CA 2680780 A1 CA2680780 A1 CA 2680780A1
- Authority
- CA
- Canada
- Prior art keywords
- coating
- silicon
- silicon nitride
- mould
- carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Abandoned
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/002—Crucibles or containers for supporting the melt
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
Abstract
A coating system for a mould for the directional solidification of silicon. The coating is applied as an aqueous slurry of silicon nitride particle, carbon black and microsilica.
Description
Title of Invention A coating composition for a mould.
Technical Field The present invention relates to a coating system for moulds used in the directional solidification of silicon ingots, and also a method of coating such moulds. The invention is particularly, but not exclusively, concerned with high purity silicon for use in solar cells.
Background Art When silicon is subjected to directional solidification in moulds e.g.
graphite moulds, the moulds would have to be coated in order to avoid contamination of the silicon ingot from contact with the mould material. It is also important that the silicon ingot is easily removed from the mould after solidification without damaging or even destroying the mould. The moulds are therefore coated, generally with silicon nitride particles, which may be sprayed, painted or otherwise applied, in the form of a slurry, on to the inner surface of the moulds.
In the case of graphite moulds, it has been observed that they often break during solidification of the silicon ingot due to the fact that silicon is a material which expands on solidification from liquid. If a mould breaks during solidification, it cannot be reused. Furthermore, and more importantly, there may be leakage of liquid silicon during the solidification process which may destroy the furnace in which the mould is located during the process. For economical reasons it is very important that graphite moulds (and moulds made from other materials) can be reused many times.
US Patent No. 5,431,869 describes a mould treatment in which the mould is first coated with a Si3N4 powder and then an alkaline earth metal halide melt film is additionally formed between the silicon nitride powder coating and the silicon melt. This procedure is, however, costly, and contaminates the silicon melt in an undesirable way with alkaline earth metal and, possibly, with other impurities from the alkaline earth metal halide mixture used.
US Patent No. 6, 615,425 describes a process in which a mould is coated with Si3N4 powder having a particular particle aspect ratio and oxygen content. It may be applied as an aqueous dispersion. However, the performance is not entirely satisfactory in that the coating is sometimes porous and allows infiltration of liquid metal in the coating.
It is therefore an object of the invention to provide a coating system for a mould which more reliably prevents damage to the mould material while at the same time enabling release of a silicon ingot from the mould without damage to the mould.
Description of Invention According to the invention, there is provided a coating composition for a mould for the directional solidification of silicon, which comprises silicon nitride particles, a source of carbon and an oxide and/or silicon powder.
The mould is preferably of a ceramic material, such as glassy carbon, silica, silicon nitride, or mullite, but the preferred material is graphite.
Preferably, in the coating composition, the carbon represents from 0.5 to 20 wt %, any oxide represents 1 to 50 wt %, any silicon represents 1 to 20 wt %
and silicon nitride represents at least 50 wt % and is the balance of the composition. The preferred oxide is Si02 and its preferred form is amorphous microsilica and amorphous fumed silica.
The term "microsilica" used in the specification and claims of this application is particulate to amorphous Si02 obtained from a process in which silica (quartz) is reduced to SiO-gas and the reduction product is oxidised in vapour phase to form amorphous silica. Microsilica may contain at least 70% by weight silica (Si02) and has a specific density of 2.1-2.3 g/cm3 and a surface area of 15-40 m2/g. The primary particles are substantially spherical and have an average size of about 0.15 m. Microsilica is preferably obtained as a co-product in the production of silicon or silicon alloys in electric reduction furnaces. In these processes large quantities of microsilica are formed. The microsilica is recovered in conventional manner using baghouse filters or other collection apparatus.
Other possible oxides include crystalline Si02, Ca containing oxide compounds, alumina and oxides of rare earths and oxides of transition metals.
Preferably, the carbon is carbon black, though other sources of carbon may be employed, such as graphite powder. Preferably, the silicon nitride particles consists of >90% alpha nitride and fall in the size range 0.1 to 2 microns size and more preferred in the size range 0.4 to 1.0 micron. The specific surface area of the silicon nitride powder is preferably 9-15 m2/g.
Preferably, the carbon source represents 1 to 15 wt% of the composition, and the oxide represents 2 to 25 wt% of the composition A preferred composition.comprises 2 wt% carbon black and 10 wt% microsilica, the balance being silicon nitride. Preferably the silicon powder represents 2 to wt% of the composition. The purpose of carbon, oxide and Si-powder addition is to favor the formation of silicon oxynitride and/or silicon carbide, which will provide a reaction product that acts as a bonding agent between the silicon nitride particles themselves and between silicon nitride and graphite.
Preferably, the coating composition is deployed as a liquid or slurry. It is more preferably dispersed in a liquid, which is preferably water. Preferably, the composition is an aqueous dispersion and further includes a binder, preferably an organic binder. The binder may be present as 0 to 70 wt%, based on the weight of dry solids, and is preferably an aqueous solution of polyvinyl alcohol (PVA). Another suitable binder is polyethylene glycol. The dispersion may also include a dispersant. Suitable dispersants include polyacrylate salts of ammonium or sodium. The dispersant may be present as 0.1 to 5 wt% based on the weight of solids and more preferred in an amount of 0.2-1.0 wt%, based on the weight of solids.
The invention also extends to a method of coating a mould for the directional solidification of silicon, which comprises applying a coating composition as described to the inner surface of the mould to form a mould coating.
Preferably the coating application is applied as an aqueous suspension. It may be applied by painting, spraying or dipping. It may be deployed as a series of sub-layers which are applied sequentially. The final thickness of the coating is preferably from 50 to 1000 microns, more preferably from 150 to 300 microns.
In addition, the coating may be covered by a further layer or layers. . The invention therefore contemplates the further step of applying a top layer composition to the base mould coating. Preferably, the top layer composition comprises silicon nitride and/or silicon carbide. Preferably, the silicon nitride represents 0 to 50 wt% of the top layer composition and the balance is silicon carbide,. The top layer may be, applied in the form of an aqueous suspension and by any convenient technique. It may include a binder, such as PVA.
The purpose of the base layer is to provide a dense tightly bonded layer on the surface of the mould which prevent metal infiltration. The objective of the top layer is to prevent metal infiltration and to provide easy release between ingot and mould.
In addition to a top coat, there may also be an intermediate coat or layer, between the base layer or basic coating and the top layer. The method of the invention may therefore also include the further step of applying an intermediate layer between the mould coating and the top layer. Preferably, 5 the intermediate layer composition comprises silicon nitride. Preferably, the intermediate layer composition is applied as an aqueous suspension.
The invention also extends to a mould (or crucible) per se, comprising a mould body coated with a coating composition as described, optionally applied by a method as described.
Detailed Description of the Invention The invention may be carried into practice in various ways and some embodiments will now be described in the following non-limiting examples.
Example 1 A coating composition comprising 10 wt% microsilica, 2 wt% carbon black and 88% silicon nitride was prepared as an aqueous dispersion with water, together with a solution of PVA as a binder and a polyacrylate salt of sodium in an amount of 0.5 wt% based on the weight of dry solids as a dispersant.
The dispersion was applied to a graphite mould inner sUrface, as a series multiple sub layers, each sub-layer being allowed to dry before application of the next.
The mould was filled with molten silicon held at a temperature of 1450 C and then slowly cooled from the bottom. Upon directional solidification, the silicon ingot was easily removed, without damage to the mould, and without any silicon infiltration, and the mould was immediately re-usable.
Technical Field The present invention relates to a coating system for moulds used in the directional solidification of silicon ingots, and also a method of coating such moulds. The invention is particularly, but not exclusively, concerned with high purity silicon for use in solar cells.
Background Art When silicon is subjected to directional solidification in moulds e.g.
graphite moulds, the moulds would have to be coated in order to avoid contamination of the silicon ingot from contact with the mould material. It is also important that the silicon ingot is easily removed from the mould after solidification without damaging or even destroying the mould. The moulds are therefore coated, generally with silicon nitride particles, which may be sprayed, painted or otherwise applied, in the form of a slurry, on to the inner surface of the moulds.
In the case of graphite moulds, it has been observed that they often break during solidification of the silicon ingot due to the fact that silicon is a material which expands on solidification from liquid. If a mould breaks during solidification, it cannot be reused. Furthermore, and more importantly, there may be leakage of liquid silicon during the solidification process which may destroy the furnace in which the mould is located during the process. For economical reasons it is very important that graphite moulds (and moulds made from other materials) can be reused many times.
US Patent No. 5,431,869 describes a mould treatment in which the mould is first coated with a Si3N4 powder and then an alkaline earth metal halide melt film is additionally formed between the silicon nitride powder coating and the silicon melt. This procedure is, however, costly, and contaminates the silicon melt in an undesirable way with alkaline earth metal and, possibly, with other impurities from the alkaline earth metal halide mixture used.
US Patent No. 6, 615,425 describes a process in which a mould is coated with Si3N4 powder having a particular particle aspect ratio and oxygen content. It may be applied as an aqueous dispersion. However, the performance is not entirely satisfactory in that the coating is sometimes porous and allows infiltration of liquid metal in the coating.
It is therefore an object of the invention to provide a coating system for a mould which more reliably prevents damage to the mould material while at the same time enabling release of a silicon ingot from the mould without damage to the mould.
Description of Invention According to the invention, there is provided a coating composition for a mould for the directional solidification of silicon, which comprises silicon nitride particles, a source of carbon and an oxide and/or silicon powder.
The mould is preferably of a ceramic material, such as glassy carbon, silica, silicon nitride, or mullite, but the preferred material is graphite.
Preferably, in the coating composition, the carbon represents from 0.5 to 20 wt %, any oxide represents 1 to 50 wt %, any silicon represents 1 to 20 wt %
and silicon nitride represents at least 50 wt % and is the balance of the composition. The preferred oxide is Si02 and its preferred form is amorphous microsilica and amorphous fumed silica.
The term "microsilica" used in the specification and claims of this application is particulate to amorphous Si02 obtained from a process in which silica (quartz) is reduced to SiO-gas and the reduction product is oxidised in vapour phase to form amorphous silica. Microsilica may contain at least 70% by weight silica (Si02) and has a specific density of 2.1-2.3 g/cm3 and a surface area of 15-40 m2/g. The primary particles are substantially spherical and have an average size of about 0.15 m. Microsilica is preferably obtained as a co-product in the production of silicon or silicon alloys in electric reduction furnaces. In these processes large quantities of microsilica are formed. The microsilica is recovered in conventional manner using baghouse filters or other collection apparatus.
Other possible oxides include crystalline Si02, Ca containing oxide compounds, alumina and oxides of rare earths and oxides of transition metals.
Preferably, the carbon is carbon black, though other sources of carbon may be employed, such as graphite powder. Preferably, the silicon nitride particles consists of >90% alpha nitride and fall in the size range 0.1 to 2 microns size and more preferred in the size range 0.4 to 1.0 micron. The specific surface area of the silicon nitride powder is preferably 9-15 m2/g.
Preferably, the carbon source represents 1 to 15 wt% of the composition, and the oxide represents 2 to 25 wt% of the composition A preferred composition.comprises 2 wt% carbon black and 10 wt% microsilica, the balance being silicon nitride. Preferably the silicon powder represents 2 to wt% of the composition. The purpose of carbon, oxide and Si-powder addition is to favor the formation of silicon oxynitride and/or silicon carbide, which will provide a reaction product that acts as a bonding agent between the silicon nitride particles themselves and between silicon nitride and graphite.
Preferably, the coating composition is deployed as a liquid or slurry. It is more preferably dispersed in a liquid, which is preferably water. Preferably, the composition is an aqueous dispersion and further includes a binder, preferably an organic binder. The binder may be present as 0 to 70 wt%, based on the weight of dry solids, and is preferably an aqueous solution of polyvinyl alcohol (PVA). Another suitable binder is polyethylene glycol. The dispersion may also include a dispersant. Suitable dispersants include polyacrylate salts of ammonium or sodium. The dispersant may be present as 0.1 to 5 wt% based on the weight of solids and more preferred in an amount of 0.2-1.0 wt%, based on the weight of solids.
The invention also extends to a method of coating a mould for the directional solidification of silicon, which comprises applying a coating composition as described to the inner surface of the mould to form a mould coating.
Preferably the coating application is applied as an aqueous suspension. It may be applied by painting, spraying or dipping. It may be deployed as a series of sub-layers which are applied sequentially. The final thickness of the coating is preferably from 50 to 1000 microns, more preferably from 150 to 300 microns.
In addition, the coating may be covered by a further layer or layers. . The invention therefore contemplates the further step of applying a top layer composition to the base mould coating. Preferably, the top layer composition comprises silicon nitride and/or silicon carbide. Preferably, the silicon nitride represents 0 to 50 wt% of the top layer composition and the balance is silicon carbide,. The top layer may be, applied in the form of an aqueous suspension and by any convenient technique. It may include a binder, such as PVA.
The purpose of the base layer is to provide a dense tightly bonded layer on the surface of the mould which prevent metal infiltration. The objective of the top layer is to prevent metal infiltration and to provide easy release between ingot and mould.
In addition to a top coat, there may also be an intermediate coat or layer, between the base layer or basic coating and the top layer. The method of the invention may therefore also include the further step of applying an intermediate layer between the mould coating and the top layer. Preferably, 5 the intermediate layer composition comprises silicon nitride. Preferably, the intermediate layer composition is applied as an aqueous suspension.
The invention also extends to a mould (or crucible) per se, comprising a mould body coated with a coating composition as described, optionally applied by a method as described.
Detailed Description of the Invention The invention may be carried into practice in various ways and some embodiments will now be described in the following non-limiting examples.
Example 1 A coating composition comprising 10 wt% microsilica, 2 wt% carbon black and 88% silicon nitride was prepared as an aqueous dispersion with water, together with a solution of PVA as a binder and a polyacrylate salt of sodium in an amount of 0.5 wt% based on the weight of dry solids as a dispersant.
The dispersion was applied to a graphite mould inner sUrface, as a series multiple sub layers, each sub-layer being allowed to dry before application of the next.
The mould was filled with molten silicon held at a temperature of 1450 C and then slowly cooled from the bottom. Upon directional solidification, the silicon ingot was easily removed, without damage to the mould, and without any silicon infiltration, and the mould was immediately re-usable.
Example 2 A mould was coated as in Example 1, but before filling the mould with molten silicon, a top layer of pure silicon nitride was applied, as an aqueous dispersion. After heating at 1450 C, the silicon was slowly cooled from the bottom. Upon solidification the silicon ingot was easily removed. Again, this was without damage to the mould, and without any silicon infiltration, and the mould was immediately re-usable.
Example 3 A mould was coated as in Example 1, but before filling the mould with molten silicon an additional layer consisting of more that 90% by weight of silicon carbide, the remaining being silicon nitride was applied on top of the base layer. After heating at 1450 C the silicon was slowly cooled from the bottom.
Upon solidification the sil,icon ingot was easily removed from the mould and the mould was ready for re-use.
Example 3 A mould was coated as in Example 1, but before filling the mould with molten silicon an additional layer consisting of more that 90% by weight of silicon carbide, the remaining being silicon nitride was applied on top of the base layer. After heating at 1450 C the silicon was slowly cooled from the bottom.
Upon solidification the sil,icon ingot was easily removed from the mould and the mould was ready for re-use.
Claims (27)
1. A coating for a mould for the directional solidification of silicon, which comprises an inner layer of silicon nitride particles, a source of carbon and an oxide and/or silicon powder, an intermediate layer comprising silicon nitride and a top layer comprising silicon nitride and/or silicon carbide.
2. A coating as claimed in Claim 1, in which the inner layer comprises 1 to 20 wt % carbon, 0.5 to 50 wt % oxide, 1 to 20 wt % silicon, at least 50 wt %
of silicon nitride and is the balance.
of silicon nitride and is the balance.
3. A coating as claimed in Claim 2, in which the oxide is SiO2.
4. A coating as claimed in Claim 2, in which the SiO2 is amorphous microsilica.
5. A coating as claimed in Claim 2, in which the SiO2 is amorphous fumed silica.
6. A coating according to Claim 2, in which the carbon is carbon black.
7. A coating as claimed in Claim 2, in which the silicon nitride particles fall in the size range 0.1 to 2 microns.
8. A coating as claimed in Claim 2, in which the silicon nitride particles fall in the size range 0.4 to 1 microns.
9. A coating as claimed in Claim 2, in which the carbon source represents 1 to 15 wt%.
10. A coating as claimed in Claim 2, in which the oxide represents 2 to 25 wt%.
11. A coating as claimed in Claim 2, which comprises 2 wt% carbon black and 10 wt% microsilica, the balance being silicon nitride.
12. A coating as claimed in Claim 2, in which the silicon powder represents 2 to 15 wt%.
13. A coating as claimed in any preceding Claim, dispersed in a liquid.
14. A coating as claimed in Claim 2, wherein the inner layer, the intermediate layer and the top layer are aqueous dispersions and further includes a binder.
15. A coating as claimed in Claim 14, in which the binder is present as up to 70 wt%, based on the weight of dry solids.
16. A coating as claimed in Claim 14 or Claim 15, in which the binder is polyvinylalcohol.
17. A coating as claimed in Claim 16, in which the binder is polyethylene glycol.
18. A coating as claimed in any preceding Claim, further comprising a dispersant.
19. A coating as claimed in Claim 18, in which the dispersant is present as 0.1 to 5wt% based on the weight of dry solids.
20. A coating as claimed in Claim 19, in which the dispersant is present as 0.2 to 1 wt% based on the weight of dry solids.
21. A coating as claimed in any of Claims 18 to 20, in which the dispersant is a polyacrylate salt of ammonium or sodium.
22. A method of coating a mould for the directional solidification of silicon, comprising applying an inner coating layer comprising silicon nitride particles, a source of carbon and an oxide and/or silicon powder, an intermediate coating layer comprising, silicon nitride and a top coating layer comprising silicon nitride and/or silicon carbide.
23. A method as claimed in Claim 22, in which the coating layers are applied as aqueous suspensions.
24. A method as claimed in Claim 23, in which the aqueous suspensions are applied by painting, spraying or dipping.
25. A method as claimed in Claim 22, in which top layer comprises 0 to 50 wt% silicon nitride and the balance is silicon carbide.
26. A mould for direction solidification of silicon comprising a mould body coated with an inner layer of silicon nitride particles, a source of carbon and an oxide and/or silicon powder, an intermediate layer comprising silicon nitride and a top layer comprising silicon nitride and/or silicon carbon.
27. A mould as claimed in Claim 26, in which the mould body is made from graphite.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| NO20071562 | 2007-03-26 | ||
| NO20071562A NO327122B1 (en) | 2007-03-26 | 2007-03-26 | A composition |
| PCT/NO2008/000103 WO2008118023A1 (en) | 2007-03-26 | 2008-03-17 | A coating composition for a mould |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2680780A1 true CA2680780A1 (en) | 2008-10-02 |
Family
ID=39788700
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002680780A Abandoned CA2680780A1 (en) | 2007-03-26 | 2008-03-17 | A coating composition for a mould |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US8147605B2 (en) |
| EP (1) | EP2139820A4 (en) |
| BR (1) | BRPI0808745A2 (en) |
| CA (1) | CA2680780A1 (en) |
| MY (1) | MY152179A (en) |
| NO (1) | NO327122B1 (en) |
| WO (1) | WO2008118023A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928980A (en) * | 2010-09-17 | 2010-12-29 | 浙江碧晶科技有限公司 | Seeding guidance die for growing silicon crystal by directional solidification method |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2543751A3 (en) | 2009-07-16 | 2013-06-26 | MEMC Singapore Pte. Ltd. | Coated crucibles and methods for preparing and use thereof |
| NO20092956A1 (en) * | 2009-09-03 | 2011-03-04 | Elkem As | Coating composition |
| US9620664B2 (en) * | 2010-05-25 | 2017-04-11 | Mossey Creek Technologies, Inc. | Coating of graphite tooling for manufacture of semiconductors |
| CN102776561B (en) * | 2012-04-01 | 2017-12-15 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystal silicon ingot and preparation method thereof, polysilicon chip and crucible used for polycrystalline silicon ingot casting |
| US9562304B2 (en) | 2012-04-01 | 2017-02-07 | Jiang Xi Sai Wei Ldk Solar Hi-Tech Co., Ltd. | Polycrystalline silicon ingot, preparation method thereof, and polycrystalline silicon wafer |
| CN103320854B (en) * | 2013-06-07 | 2016-03-02 | 英利集团有限公司 | Crucible coating structure, its preparation method and comprise its crucible |
| CN104928755A (en) * | 2014-03-19 | 2015-09-23 | 晶科能源有限公司 | Polysilicon ingot casting method |
| DE102018131811A1 (en) * | 2018-08-13 | 2020-02-13 | HÜTTENES-ALBERTUS Chemische Werke Gesellschaft mit beschränkter Haftung | Use of a size composition and corresponding method for producing a centrifugal casting mold with a size coating |
Family Cites Families (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53102300A (en) * | 1977-02-18 | 1978-09-06 | Toshiba Corp | Preparation of type silicon nitride powders |
| US4099924A (en) * | 1977-03-16 | 1978-07-11 | Rca Corporation | Apparatus improvements for growing single crystalline silicon sheets |
| JPS5825770B2 (en) * | 1979-06-13 | 1983-05-30 | 吉雄 村尾 | Draft roller clearer device |
| JPS6018638B2 (en) | 1979-08-17 | 1985-05-11 | 東芝セラミツクス株式会社 | Silicon single crystal pulling equipment |
| US4356152A (en) * | 1981-03-13 | 1982-10-26 | Rca Corporation | Silicon melting crucible |
| CN1007724B (en) * | 1985-06-24 | 1990-04-25 | 川崎制铁株式会社 | Method of producing alpha-silicon nitride powders |
| JPS63162511A (en) * | 1986-12-26 | 1988-07-06 | Toshiba Ceramics Co Ltd | Production of silicon nitride |
| JPS649806A (en) * | 1987-07-03 | 1989-01-13 | Toshiba Corp | Production of high-quality alpha type silicon nitride powder |
| US5431869A (en) * | 1993-01-12 | 1995-07-11 | Council Of Scientific & Industrial Research | Process for the preparation of polycrystalline silicon ingot |
| US5453317A (en) * | 1993-08-31 | 1995-09-26 | Borg-Warner Automotive, Inc. | Friction material comprising powdered phenolic resin and method of making same |
| US5538675A (en) * | 1994-04-14 | 1996-07-23 | The Dow Chemical Company | Method for producing silicon nitride/silicon carbide composite |
| US5730792A (en) * | 1996-10-04 | 1998-03-24 | Dow Corning Corporation | Opaque ceramic coatings |
| JP2001510434A (en) | 1997-02-06 | 2001-07-31 | バイエル・アクチエンゲゼルシヤフト | Melt pot with silicon protective layer, method of applying silicon protective layer and use thereof |
| WO1999005338A2 (en) | 1997-07-24 | 1999-02-04 | Toyo Tanso Usa, Inc. | Surface converted graphite components and methods of making same |
| DE69912668T2 (en) * | 1998-02-26 | 2004-09-30 | Mitsubishi Materials Corp. | Mold and process for the production of silicon rods |
| US6313056B1 (en) * | 1998-08-20 | 2001-11-06 | Harbison-Walker Refractories Company | Non-slumping sprayable refractory castables containing thermal black |
| JP2000202835A (en) | 1999-01-19 | 2000-07-25 | Hanano Shoji Kk | Powder mold-releasing agent for molding tire |
| US6896968B2 (en) * | 2001-04-06 | 2005-05-24 | Honeywell International Inc. | Coatings and method for protecting carbon-containing components from oxidation |
| UA81278C2 (en) * | 2002-12-06 | 2007-12-25 | Vessel for holding a silicon and method for its making | |
| US20040211496A1 (en) * | 2003-04-25 | 2004-10-28 | Crystal Systems, Inc. | Reusable crucible for silicon ingot growth |
| DE10342042A1 (en) * | 2003-09-11 | 2005-04-07 | Wacker-Chemie Gmbh | Process for producing a Si3N4 coated SiO2 shaped body |
| JP4493515B2 (en) * | 2005-02-14 | 2010-06-30 | 新日鉄マテリアルズ株式会社 | Silicone solidification mold with carbon release material |
| EP1739209A1 (en) * | 2005-07-01 | 2007-01-03 | Vesuvius Crucible Company | Crucible for the crystallization of silicon |
-
2007
- 2007-03-26 NO NO20071562A patent/NO327122B1/en not_active IP Right Cessation
-
2008
- 2008-03-17 WO PCT/NO2008/000103 patent/WO2008118023A1/en active Application Filing
- 2008-03-17 MY MYPI20093848 patent/MY152179A/en unknown
- 2008-03-17 CA CA002680780A patent/CA2680780A1/en not_active Abandoned
- 2008-03-17 BR BRPI0808745-8A patent/BRPI0808745A2/en not_active IP Right Cessation
- 2008-03-17 US US12/532,719 patent/US8147605B2/en active Active
- 2008-03-17 EP EP08741702A patent/EP2139820A4/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928980A (en) * | 2010-09-17 | 2010-12-29 | 浙江碧晶科技有限公司 | Seeding guidance die for growing silicon crystal by directional solidification method |
| CN101928980B (en) * | 2010-09-17 | 2012-10-03 | 浙江碧晶科技有限公司 | Seeding guidance die for growing silicon crystal by directional solidification method |
Also Published As
| Publication number | Publication date |
|---|---|
| US20100133415A1 (en) | 2010-06-03 |
| EP2139820A1 (en) | 2010-01-06 |
| BRPI0808745A2 (en) | 2014-08-12 |
| NO20071562L (en) | 2008-09-29 |
| US8147605B2 (en) | 2012-04-03 |
| MY152179A (en) | 2014-08-15 |
| WO2008118023A1 (en) | 2008-10-02 |
| NO327122B1 (en) | 2009-04-27 |
| EP2139820A4 (en) | 2012-03-07 |
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