CN102633260A - Silicon carbide synthesis method - Google Patents

Silicon carbide synthesis method Download PDF

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Publication number
CN102633260A
CN102633260A CN2012100685565A CN201210068556A CN102633260A CN 102633260 A CN102633260 A CN 102633260A CN 2012100685565 A CN2012100685565 A CN 2012100685565A CN 201210068556 A CN201210068556 A CN 201210068556A CN 102633260 A CN102633260 A CN 102633260A
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graphite powder
graphite
silit
powder
slurry
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CN2012100685565A
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CN102633260B (en
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赵建立
由远洪
孙福龙
白周义
牛景林
焦松强
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Shihezi Fengtuo Silicon Material Science and Technology Co., Ltd.
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XINJIANG YUFENG PHOTOVOLTAIC MATERIAL TECHNOLOGY Co Ltd
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Abstract

The invention discloses a silicon carbide synthesis method. The silicon carbide synthesis method includes procedures of filling packing, electrifying and heating, keeping constant power, naturally cooling and discharging. The silicon carbide synthesis method is characterized in that at least a graphite slurry layer is smeared on a burner graphite electrode on one side of a furnace heating cavity before conduction graphite powder is filled in the packing filling procedure, and then packing filling procedure for the conduction graphite powder is carried out. Compared with the prior art, the silicon carbide synthesis method has the advantages that melt can be prevented from being adhered on the surface of the graphite electrode, the surface of the graphite electrode can be cleaned quite easily before next loading, graphite powder and the melt which are smeared on the surface of the graphite electrode can be completely removed only by means of lightly scraping the surface of the graphite electrode by the aid of a scraper, further, water is used as a bonding agent during smearing and volatilizes when heated, conductivity between the graphite electrode and the graphite powder of a furnace core is unaffected, the surface of the graphite electrode cannot be damaged, accordingly, the service life of the graphite electrode is greatly prolonged, maintenance frequency is reduced, production efficiency is improved, and production cost is lowered.

Description

The silit compound method
Technical field
The present invention relates to a kind of silit compound method.
Background technology
When silit industry is synthetic, use the resistance furnace synthesis technique when particularly green silicon carbide industry is synthetic, resistance furnace comprises the body of heater that is provided with heating chamber; Two ends of body of heater heating chamber are provided with Graphite Electrodes, in synthetic production, a charge process are arranged at first; The i.e. furnace bottom compound after mixing such as refinery coke and silica sand of packing in body of heater, the conduction of packing into of the stove heart position between the Graphite Electrodes of two ends use Graphite Powder 99 then, around the electrically conductive graphite powder, loads reaction material and insulation material again; Through on the Graphite Electrodes of two ends, powering up, and then make conduction with the reaction material around the Graphite Powder 99 energising electric conduction of heating Graphite Powder 99, in heat-processed; Silica sand and Industrial Salt at high temperature melt, and melts can be bonded on the graphite electrode surface, and cooling back intensity is very big; Before next stove of filling,, must clear up in order to prevent these dung influence conductions; This removal treatment can cause Graphite Electrodes body surface layer and top layer dung to come off together, and generally after 3~5 months, Graphite Electrodes length can obviously shorten; The surface can be rough and uneven in surface, and the burner of must dismantling this moment is readjusted the Graphite Electrodes position; Because the Graphite Electrodes limited length, generally after adjustment 2~3 times, Graphite Electrodes promptly needs integral replacing.
Adjustment Graphite Electrodes position need stop to produce the use cost that integral replacing then also can increase manufacturing facilities greatly.
Summary of the invention
The purpose of this invention is to provide and a kind ofly can prevent effectively that melts is bonded in the Graphite Electrodes top layer, prolong the time limit of service of Graphite Electrodes greatly, and then the silit synthetic process of enhancing productivity and reducing production costs.
The objective of the invention is to realize: comprise charge, energising heating, permanent power maintenance, naturally cooling and go out material process through following technical scheme; Said charge process comprises: the furnace bottom branch is packed into and is comprised the compound of refinery coke and silica sand in body of heater; Stove heart position between the Graphite Electrodes of two ends conduction of packing into is used Graphite Powder 99 then; Reaction material and insulation material on around the electrically conductive graphite powder, loading successively again; Be characterized in: before the conduction of packing into of charge operation is with Graphite Powder 99, on the burner Graphite Electrodes of body of heater heating chamber one side, smear one deck Graphite Powder 99 slurry at least, and then carry out packing into of charge operation and conduct electricity and use Graphite Powder 99.
Above-mentioned Graphite Powder 99 slurry is preferably: Graphite Powder 99 and the water pulp that stirs; The Graphite Powder 99 of Graphite Powder 99 slurry and the proportioning of water are: 1 weight part Graphite Powder 99 adds 1~3 weight parts water; Smearing thickness is the coating of 2~30mm; Be preferably 10~30mm, it is identical with Graphite Powder 99 that the used Graphite Powder 99 of said Graphite Powder 99 slurry is preferably the conduction of being packed into stove heart position.
Graphite Powder 99 in the said Graphite Powder 99 slurry is preferably and is ground into≤powder of 1mm.
Preferably add 0.3~0.6 part dextrin and 0.05~0.2 part carbon black in the said Graphite Powder 99 slurry.
Described Graphite Powder 99 slurry is smeared before being preferably in charge 12h.
As improvement, said energising heating process is: progressively hoisting power and then gets into permanent power and keeps to ratings in greater than 1 hour time, and above-mentioned energising is preferably heat-up time: 1.5~2.5 hours.
Compared with prior art, the present invention leans on the furnace body inside surface partly at the burner Graphite Electrodes and smears the effect that the identical Graphite Powder 99 of packing into stove heart position can play isolation Graphite Electrodes and furnace charge, when furnace charge at high temperature melts; Melt is bonded on the graphite bisque of smearing, and can not be bonded on the graphite electrode surface, before charging next time; Cleaning is very easy to, as long as gently scrape Graphite Powder 99 and the melts that just can remove fully on the graphite electrode surface with scraper, and since when smearing the wedding agent of use be water; Being heated promptly vapors away, and does not influence the electroconductibility between Graphite Electrodes and the stove cardiolith ink powder, also can not damage graphite electrode surface; Thereby prolonged life-span of Graphite Electrodes greatly; Reduce maintenance, improved production efficiency, reduced production cost.
Embodiment
Embodiment 1: the furnace bottom compound of refinery coke and silica sand of packing in body of heater; Get 1 weight part Graphite Powder 99 to be ground into≤powder of 1mm; Add 2 weight parts waters and stir into muddy; On two burner Graphite Electrodess of body of heater heating chamber one side, smearing 20mm, packs into to conduct electricity and uses Graphite Powder 99 in the stove heart position between the Graphite Electrodes of two ends, around the electrically conductive graphite powder, loads reaction material and insulation material more successively; Energising is heated then, progressively hoisting power gets into permanent power afterwards and keeps the stage to ratings in 1.2 hours time.
Embodiment 2: the furnace bottom branch compound of refinery coke and silica sand of packing in body of heater, get 1 weight part Graphite Powder 99 to be ground into≤powder of 1mm.Add 3 weight parts waters and stir into muddy; On two burner Graphite Electrodess of body of heater heating chamber one side, smear the coating that forms 10mm; Stove heart position between the Graphite Electrodes of two ends conduction of packing into use Graphite Powder 99 then, reaction material and insulation material in the filling successively around the electrically conductive graphite powder again, and energising is heated then; Progressively hoisting power gets into permanent power afterwards and keeps the stage to ratings in 1 hour time.
Embodiment 3: the furnace bottom branch compound of refinery coke and silica sand of packing in body of heater, get 1 weight part Graphite Powder 99 to be ground into≤powder of 0.5mm.Add 1.2 weight parts waters and stir into muddy; On two burner Graphite Electrodess of body of heater heating chamber one side, smear the coating that forms 25mm; Stove heart position between the Graphite Electrodes of two ends conduction of packing into use Graphite Powder 99 then, reaction material and insulation material in the filling successively around the electrically conductive graphite powder again, and energising is heated then; Progressively hoisting power gets into permanent power afterwards and keeps the stage to ratings in 2 hours time.
Embodiment 4: the furnace bottom branch compound of refinery coke and silica sand of packing in body of heater, get 1 weight part Graphite Powder 99 to be ground into≤powder of 0.25mm.Add 3 weight parts waters and stir into muddy; On two burner Graphite Electrodess of body of heater heating chamber one side, smear the coating that forms 5mm; Stove heart position between the Graphite Electrodes of two ends conduction of packing into use Graphite Powder 99 then, reaction material and insulation material in the filling successively around the electrically conductive graphite powder again, and energising is heated then; Progressively hoisting power gets into permanent power afterwards and keeps the stage to ratings in greater than 1.5 hours time.
Embodiment 5: the furnace bottom branch compound of refinery coke and silica sand of packing in body of heater, get 1 weight part Graphite Powder 99 to be ground into≤powder of 0.38mm.Add 1.8 weight parts waters and stir into muddy; On two burner Graphite Electrodess of body of heater heating chamber one side, smear the coating that forms 25mm; Stove heart position between the Graphite Electrodes of two ends conduction of packing into use Graphite Powder 99 then, reaction material and insulation material in the filling successively around the electrically conductive graphite powder again, and energising is heated then; Progressively hoisting power gets into permanent power afterwards and keeps the stage to ratings in 1.8 hours time.
Embodiment 6: get 1 weight part and be ground into≤powder of 1mm with the identical Graphite Powder 99 of Graphite Powder 99 with conduction; Add 2 weight parts waters and stir into muddy, on the burner Graphite Electrodes, smear the coating that forms 20mm, after the 12h; After treating the dry sclerosis of said coating, carry out the charge operation again.
Embodiment 7: get 1 weight part and be ground into≤powder of 0.42mm with the identical Graphite Powder 99 of Graphite Powder 99 with conduction; Add 1.5 weight parts waters and stir into muddy, on the burner Graphite Electrodes, smear the coating that forms 30mm, after the 12h; Carry out the charge operation again; After the charge, progressively hoisting power gets into permanent power afterwards and keeps the stage to ratings in 0.5 hour time.
Embodiment 8: get 1 weight part and be ground into≤powder of 0.8mm with the identical Graphite Powder 99 of Graphite Powder 99 with conduction, mix with 0.3 part dextrin and 0.1 part carbon black, add 2.5 weight parts waters and stir into muddy; On the burner Graphite Electrodes, smear the coating that forms 30mm; After the 12h, treat to carry out the charge operation again after the dry sclerosis of said coating, after the charge; Progressively hoisting power gets into permanent power afterwards and keeps the stage to ratings in 0.4 hour time.
Embodiment 9: get 1 weight part and be ground into≤powder of 0.25mm with the identical Graphite Powder 99 of Graphite Powder 99 with conduction; Mix the back with the carbon black of 0.5 part dextrin and 0.2 part and add 2 weight parts waters and stir into muddy, on the burner Graphite Electrodes, smear the coating that forms 25mm, after the 12h; Treat to carry out the charge operation again after the dry sclerosis of said coating; After the charge, progressively hoisting power gets into permanent power afterwards and keeps the stage to ratings in 0.6 hour time.
Embodiment 10: get 1 weight part and be ground into≤powder of 0.5mm with the identical Graphite Powder 99 of Graphite Powder 99 with conduction, mixes back adding 1.5 weight parts waters with the carbon black of 0.6 part dextrin and 0.08 part and stir into muddy, on the burner Graphite Electrodes, smear the coating of formation 30mm; After the 12h; After treating the dry sclerosis of said coating, carry out the charge operation again, after the charge; Progressively hoisting power gets into permanent power afterwards and keeps the stage to ratings in 0.8 hour time.
Embodiment 11: get 1 weight part and be ground into≤powder of 0.18mm with the identical Graphite Powder 99 of Graphite Powder 99 with conduction, mixes back adding 2.5 weight parts waters with the carbon black of 0.4 part dextrin and 0.15 part and stir into muddy, on the burner Graphite Electrodes, smear the coating of formation 25mm; After the 12h; After treating the dry sclerosis of said coating, carry out the charge operation again, after the charge; Progressively hoisting power gets into permanent power afterwards and keeps the stage to ratings in 1.0 hours time.
Embodiment 12: get 1 weight part and be ground into≤powder of 0.35mm with the identical Graphite Powder 99 of Graphite Powder 99 with conduction, after the carbon black of 0.5 part dextrin and 0.2 part mixes, add 2 weight parts waters and stir into muddy; On the burner Graphite Electrodes, smear the coating that forms 30mm; After the 12h, carry out the charge operation again, after the charge; Progressively hoisting power gets into permanent power afterwards and keeps the stage to ratings in 0.5 hour time.
Embodiment 13: get 1 weight part and be ground into≤powder of 0.18mm with the identical Graphite Powder 99 of Graphite Powder 99 with conduction; Mix the back with the carbon black of 0.25 part dextrin and 0.12 part and add 2.5 weight parts waters and stir into muddy, on the burner Graphite Electrodes, smear the coating that forms 2mm, after the 6h; Treat to carry out the charge operation again after the dry sclerosis of said coating; After the charge, progressively hoisting power gets into permanent power afterwards and keeps the stage to ratings in 0.6 hour time.
Embodiment 14: get 1 weight part and be ground into≤powder of 0.15mm with the identical Graphite Powder 99 of Graphite Powder 99 with conduction, mixes back adding 2.5 weight parts waters with the carbon black of 0.35 part dextrin and 0.15 part and stir into muddy, on the burner Graphite Electrodes, smear the coating of formation 12mm; After the 12h; After treating the dry sclerosis of said coating, carry out the charge operation again, after the charge; Progressively hoisting power gets into permanent power afterwards and keeps the stage to ratings in 1.5 hours time.
Embodiment 15: get 1 weight part and be ground into≤powder of 0.18mm with the identical Graphite Powder 99 of Graphite Powder 99 with conduction, mixes back adding 2.2 weight parts waters with the carbon black of 0.45 part dextrin and 0.18 part and stir into muddy, on the burner Graphite Electrodes, smear the coating of formation 25mm; After the 12h; After treating the dry sclerosis of said coating, carry out the charge operation again, after the charge; Progressively hoisting power gets into permanent power afterwards and keeps the stage to ratings in 1.8 hours time.
Embodiment 16: get 1 weight part and be ground into≤powder of 0.25mm with the identical Graphite Powder 99 of Graphite Powder 99 with conduction, after the carbon black of 0.55 part dextrin and 0.18 part mixes, add 2.6 weight parts waters and stir into muddy; On the burner Graphite Electrodes, smear the coating that forms 30mm; After the 12h, carry out the charge operation again, after the charge; Progressively hoisting power gets into permanent power afterwards and keeps the stage to ratings in 1.5 hours time.

Claims (10)

1. silit compound method; Comprise charge, energising heating, permanent power maintenance, naturally cooling and go out material process; Said charge process comprises: the furnace bottom branch is packed into and is comprised the compound of refinery coke and silica sand in body of heater; Stove heart position between the Graphite Electrodes of two ends conduction of packing into use Graphite Powder 99 then, and reaction material and insulation material in the filling successively around the electrically conductive graphite powder is characterized in that: before conducting electricity with Graphite Powder 99 in packing into of charge operation at least again; On the burner Graphite Electrodes of body of heater heating chamber one side, smear one deck Graphite Powder 99 slurry, and then the conduction of packing into of carrying out the charge operation is used Graphite Powder 99.
2. silit compound method according to claim 1; It is characterized in that: described Graphite Powder 99 slurry is: Graphite Powder 99 and the water pulp that stirs; And the proportioning of Graphite Powder 99 and water is: 1 weight part Graphite Powder 99 adds 1~3 weight parts water, and smearing thickness is 2~30mm.
3. silit compound method according to claim 2 is characterized in that: the used Graphite Powder 99 of described Graphite Powder 99 slurry is identical with Graphite Powder 99 for the conduction of being packed into stove heart position.
4. silit compound method according to claim 3 is characterized in that: the Graphite Powder 99 in the said Graphite Powder 99 slurry is to be ground into≤powder of 1mm.
5. according to claim 1,2,3 or 4 described silit compound methods, it is characterized in that: add 0.3~0.6 part dextrin and 0.05~0.2 part carbon black in the said Graphite Powder 99 slurry.
6. according to claim 1,2,3 or 4 described silit compound methods, it is characterized in that: said energising heating process is: progressively hoisting power and then gets into permanent power and keeps to ratings in greater than 1 hour time.
7. silit compound method according to claim 5 is characterized in that: said energising heating process is: progressively hoisting power and then gets into permanent power and keeps to ratings in greater than 1 hour time.
8. silit compound method according to claim 6 is characterized in that: the energising of above-mentioned progressively hoisting power to ratings is heat-up time: 1.5~2.5 hours.
9. according to claim 1,2,3 or 4 described silit compound methods, it is characterized in that: described Graphite Powder 99 slurry was smeared before charge 12h.
10. silit compound method according to claim 5 is characterized in that: described Graphite Powder 99 slurry was smeared before charge 12h.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103553044A (en) * 2013-10-12 2014-02-05 台州市一能科技有限公司 Preparation method of high-purity silicon carbide
CN108002379A (en) * 2017-12-15 2018-05-08 吉林市松江炭素有限责任公司 A kind of method for increasing carbon black and recycling number
CN108083281A (en) * 2017-12-27 2018-05-29 江苏乐园新材料集团有限公司 A kind of protective layer metamorphosis formula carbonization silicon preparation method

Citations (1)

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Publication number Priority date Publication date Assignee Title
CN1049138A (en) * 1989-08-02 1991-02-13 山东省新泰市碳化硅厂 The method of hard coal and quartz sand smelting green silicon carbide

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
CN1049138A (en) * 1989-08-02 1991-02-13 山东省新泰市碳化硅厂 The method of hard coal and quartz sand smelting green silicon carbide

Non-Patent Citations (1)

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Title
王晓刚等: "《碳化硅合成理论与技术》", 30 September 2001, article "碳化硅电阻炉及其结构设计", pages: 114 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103553044A (en) * 2013-10-12 2014-02-05 台州市一能科技有限公司 Preparation method of high-purity silicon carbide
CN103553044B (en) * 2013-10-12 2015-07-08 台州市一能科技有限公司 Preparation method of high-purity silicon carbide
CN108002379A (en) * 2017-12-15 2018-05-08 吉林市松江炭素有限责任公司 A kind of method for increasing carbon black and recycling number
CN108083281A (en) * 2017-12-27 2018-05-29 江苏乐园新材料集团有限公司 A kind of protective layer metamorphosis formula carbonization silicon preparation method

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Address after: Bei Quan Zhen Qing Quan Shihezi city of the Xinjiang Uygur Autonomous Region province in 832012 administrative units under set

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