CN101311143B - Method for preparing charcoal/charcoal air supply nozzle of high temperature furnace - Google Patents
Method for preparing charcoal/charcoal air supply nozzle of high temperature furnace Download PDFInfo
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- CN101311143B CN101311143B CN2008100180282A CN200810018028A CN101311143B CN 101311143 B CN101311143 B CN 101311143B CN 2008100180282 A CN2008100180282 A CN 2008100180282A CN 200810018028 A CN200810018028 A CN 200810018028A CN 101311143 B CN101311143 B CN 101311143B
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Abstract
The invention relates to a preparation method for carbon/a carbon nozzle of air supple used in a high temperature furnace, which adopts a needling plain carbon cloth prefabricated body with a pseudo-three-dimensional structure; the prefabricated body is densified by chemical gas-phase permeation and resin impregnation-charing for a plurality of times; the densified blank carries out high-temperature treatment at a certain temperature to increase opening percentage on the surface, and then densification treatment is further carried out; the resin impregnation-charing densification technique isadopted until the density is equal to or more than 1.75g/cm<3>, finally mechanical workout is carried out after high-temperature purification treatment, and the surface is treated with CVD coating toproduce the carbon/the carbon nozzle of air supple. The method of the invention adopts the technique of the combination of chemical gas-phase permeation and resin impregnation-charing for densification to produce the material of the carbon/the carbon nozzle; when being applied to the nozzle of air supple in a polysilicon hydrogenation furnace, the material of the carbon/the carbon nozzle can effectively enhance the strength of the nozzle of air supple and scour resistance and corrosion resistance of the nozzle, prolong the service life of the nozzle and lower the replacing rate of the nozzle.
Description
Technical field
The invention belongs to polysilicon hydrogenation furnace and use nozzle of air supply material technology field, be specifically related to a kind of preparation method of charcoal/charcoal air supply nozzle of high temperature furnace.
Background technology
At present, the main method of producing polysilicon is the improvement Siemens Method, adopts the polysilicon of improvement Siemens Method production to account for more than 80% of global polysilicon ultimate production.When the improvement Siemens Method was produced polysilicon product, hydrogenation furnace was that the recycle system is the step that reaction product reclaims, and was about to generate the by product SiCl that the polysilicon product reaction produces
4With H
2Reaction generates SiHCl
3Raw material utilizes again.In the hydrogenation furnace, under 1250 ℃ of conditions, SiCl
4With H
2Mixed gas enter in the stove from nozzle with the speed of 30m/s and react, furnace pressure reaches 0.6MPa.Therefore require nozzle purity height, do not pollute polysilicon product, intensity height, anti-washing away.
At present, what polysilicon hydrogenation furnace mainly used with nozzle of air supply is high purity graphite, because graphite material intensity is low, a little less than the anti-scouring capability, so graphite nozzle is under the washing away of air volume, not only surface particles comes off easily, the high purity polycrystalline silicon product is produced pollution, and fracture easily, the work-ing life of reducing nozzle greatly, and the hydrogenation furnace continuous operating time is more than 2000 hours, so will have a strong impact on the continuous operating time of hydrogenation furnace the work-ing life of nozzle.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of densification is respond well, the preparation method of the charcoal/charcoal air supply nozzle of high temperature furnace of material use properties excellence and provide, with preparation Stability Analysis of Structures, intensity height, carbon/carbon composite nozzle of air supply that anti-scouring capability is strong, improve the work-ing life of nozzle, reduce the turnover rate of nozzle, thereby improve the hydrogenation furnace continuous operating time.
For achieving the above object, the technical solution adopted in the present invention is: a kind of preparation method of charcoal/charcoal air supply nozzle of high temperature furnace is characterized in that may further comprise the steps:
(1) adopt charcoal cloth and short carbon fiber net tire alternative stacked, adopt needling process to introduce vertical fortifying fibre at thickness direction, make full carbon fiber pseudo-three-dimensional structure precast body, the density of described precast body is 0.30～0.55g/cm
3
(2) chemical gas-phase permeation compaction is handled: with propylene or Sweet natural gas is raw material Pintsch process in chemical vapor deposition stove, the described precast body in the step (1) is carried out chemical gas-phase permeation compaction handle; Described high-temperature temperature is 940-1060 ℃;
(3) acetone-furfural resin or resin impregnating-charing: under the pressure of 1.5-2.0MPa, in impregnating autoclave, the precast body that carries out in the step (2) after chemical gas-phase permeation compaction is handled was flooded 3.5-4.5 hour, go out to change over to behind the jar and be cured processing in the curing oven, change over to again carry out in the charring furnace charing handle charcoal/carbon product;
(4) under hot conditions, the charcoal/carbon product that carries out in the step (3) after charing is handled is carried out pyroprocessing, described pyroprocessing temperature is 1800-2000 ℃;
(5) acetone-furfural resin or resin impregnating-charing densification technique is identical with step (3);
(6) charcoal/carbon product density 〉=1.75g/cm
3The time, densification technique finishes, and feeds chlorine or freonll-11 in purifying furnace, and charcoal/carbon product is carried out high temperature purification treatment, and described high temperature purification treatment temperature is 2300-2500 ℃;
(7) charcoal/carbon product that carries out in the step (6) after the high temperature purification treatment is carried out mechanical workout;
(8) be raw material with propylene or Sweet natural gas, in chemical vapor deposition stove, carry out the surface chemistry vapour deposition coating and handle, promptly make charcoal/charcoal air supply nozzle of high temperature furnace carrying out charcoal/carbon product after the mechanical workout in the step (7).
Charcoal cloth described in the step (1) is 3～24K plain weave charcoal cloth, and wherein K represents tow thousand radicals.
Solidification value is 190 ℃ described in the step (3), and carbonization temperature is 800-1000 ℃.
The chemical vapor deposited coatings treatment temp is 900-1100 ℃ described in the step (8).
Made charcoal/charcoal air supply nozzle dimensions is external diameter 30～100mm, thickness 5～20mm, height 150～500mm.
High Temperature Furnaces Heating Apparatus of the present invention is meant furnace temperature at the High Temperature Furnaces Heating Apparatus more than 1000 ℃, as polysilicon hydrogenation furnace etc.
The present invention replaces traditional graphite nozzle material with carbon/carbon composite as nozzle material.The tensile strength of acupuncture plain weave charcoal cloth carbon/carbon composite is more than the 60Mpa, ultimate compression strength is more than the 100Mpa, and the tensile strength of high purity graphite material is about 25MPa, ultimate compression strength is about 45MPa, therefore adopts acupuncture plain weave charcoal cloth carbon/carbon composite as nozzle material, after the coating processing is carried out on the surface, can improve the intensity of nozzle greatly, it is on the low side to have overcome graphite nozzle intensity, a little less than the anti-scouring capability, and the shortcoming that work-ing life is short.The present invention adopts advanced carbon/carbon composite compact technology, and the densification technique that chemical vapor infiltration and resin impregnation-charing combine makes density 〉=1.70g/cm
3The nozzle goods.This carbon/carbon composite nozzle article construction is stable, and the intensity height is difficult for reacting with the interior ambiance of hydrogenation furnace, can improve the work-ing life of nozzle greatly, reduces the turnover rate of nozzle, and has improved the hydrogenation furnace continuous operating time.
The present invention compared with prior art has the following advantages:
(1) adopts the full carbon fiber pseudo-three-dimensional structure precast body of acupuncture 3～24K plain weave charcoal cloth, can significantly strengthen the intensity of nozzle product.
(2) densification technique that adopts chemical vapor infiltration and resin impregnation-charing to combine, fine and close respond well, the deposit carbon Stability Analysis of Structures has good dimensional stability.
(3) adopt 2300-2500 ℃ high temperature purification treatment, not only can improve product purity, and can improve heat-shock resistance and structural stability greatly.
(4) the nozzle product after the machining is carried out surface chemistry vapour deposition (CVD) coating and handle, can effectively improve the erosion resistibility of nozzle product and at SiCl
4, the corrosion resistance in the HCl atmosphere.
(5) to have a volume little for the charcoal that makes with this Technology/charcoal nozzle, and thin thickness improves 2-3 work-ing life doubly, reduces the nozzle exchange rate, and hydrogenation furnace equipment continuous operating time is improved.
Description of drawings
Fig. 1 is preparation method's of the present invention process flow sheet.
Fig. 2 is the structural representation of the charcoal/charcoal air supply nozzle of high temperature furnace of the present invention's preparation.
Embodiment
The present invention will be further described below in conjunction with embodiment.
Embodiment 1
(1) adopt 12K plain weave charcoal cloth and short carbon fiber net tire alternative stacked, adopt needling process to introduce vertical fortifying fibre at thickness direction, make full carbon fiber pseudo-three-dimensional structure precast body, the density of precast body is 0.45g/cm
3
(2) chemical gas-phase permeation compaction is handled: with the propylene is raw material cracking at high temperature, the described precast body in the step (1) is carried out chemical gas-phase permeation compaction handle; Described high-temperature temperature is 940 ℃;
(3) acetone-furfural resin dipping-charing: under the pressure of 2.0MPa, in impregnating autoclave, the precast body that carries out in the step (2) after chemical gas-phase permeation compaction is handled was flooded 3.5 hours, go out to change over to behind the jar and be cured processing in the curing oven, solidification value is 190 ℃, change over to again carry out in the charring furnace charing handle charcoal/carbon product, carbonization temperature is 900 ℃;
(4) under hot conditions, the charcoal/carbon product that carries out in the step (3) after charing is handled is carried out pyroprocessing, described pyroprocessing temperature is 1800 ℃;
(5) acetone-furfural resin dipping-charing densification technique is identical with step (3);
(6) charcoal/carbon product density 〉=1.75g/cm
3The time, densification technique finishes, and under 2300 ℃ of conditions charcoal/carbon product is carried out high temperature purification treatment, more than 2000 ℃ the time, feeds chlorine in purifying furnace product inside impurity is reacted removing;
(7) charcoal/carbon product that carries out in the step (6) after the high temperature purification treatment is carried out mechanical workout;
(8) under 900 ℃ of conditions of temperature, be raw material, in chemical vapor deposition stove, carry out the surface chemistry vapour deposition coating and handle, promptly make charcoal/charcoal air supply nozzle of high temperature furnace carrying out charcoal/carbon product after the mechanical workout in the step (7) with the propylene.
The charcoal/charcoal air supply nozzle density of present embodiment preparation is 1.70g/cm
3, tensile strength is 60MPa, and ultimate compression strength is 100Mpa, and ash oontent is 27ppm, and its dimensions is external diameter 30mm, thickness 5mm, height 150mm.
Embodiment 2
(1) adopt 6K plain weave charcoal cloth and short carbon fiber net tire alternative stacked, adopt needling process to introduce vertical fortifying fibre at thickness direction, make full carbon fiber pseudo-three-dimensional structure precast body, the density of precast body is 0.55g/cm
3
(2) chemical gas-phase permeation compaction is handled: with the propylene is raw material cracking at high temperature, the described precast body in the step (1) is carried out chemical gas-phase permeation compaction handle; Described high-temperature temperature is 980 ℃;
(3) resin impregnating-charing: under the pressure of 1.5MPa, in impregnating autoclave, the precast body that carries out in the step (2) after chemical gas-phase permeation compaction is handled was flooded 4.5 hours, go out to change over to behind the jar and be cured processing in the curing oven, solidification value is 190 ℃, change over to again carry out in the charring furnace charing handle charcoal/carbon product, carbonization temperature is 800 ℃;
(4) under hot conditions, the charcoal/carbon product that carries out in the step (3) after charing is handled is carried out pyroprocessing, described pyroprocessing temperature is 2000 ℃;
(5) resin impregnating-charing densification technique is identical with step (3);
(6) charcoal/carbon product density 〉=1.75g/cm
3The time, densification technique finishes, and under 2500 ℃ of conditions charcoal/carbon product is carried out high temperature purification treatment, more than 2000 ℃ the time, feeds freonll-11 in purifying furnace product inside impurity is reacted removing;
(7) charcoal/carbon product that carries out in the step (6) after the high temperature purification treatment is carried out mechanical workout;
(8) under 1020 ℃ of conditions of temperature, be raw material, in chemical vapor deposition stove, carry out the surface chemistry vapour deposition coating and handle, promptly make charcoal/charcoal air supply nozzle of high temperature furnace carrying out charcoal/carbon product after the mechanical workout in the step (7) with the propylene.
The charcoal/charcoal air supply nozzle density of present embodiment preparation is 1.70g/cm
3, tensile strength is 65MPa, and ultimate compression strength is 115Mpa, and ash oontent is 29ppm, and its dimensions is external diameter 60mm, thickness 10mm, height 300mm.
Embodiment 3
(1) adopt 3K plain weave charcoal cloth and short carbon fiber net tire alternative stacked, adopt needling process to introduce vertical fortifying fibre at thickness direction, make full carbon fiber pseudo-three-dimensional structure precast body, the density of precast body is 0.40g/cm
3
(2) chemical gas-phase permeation compaction is handled: with the Sweet natural gas is raw material cracking at high temperature, the described precast body in the step (1) is carried out chemical gas-phase permeation compaction handle; Described high-temperature temperature is 1060 ℃;
(3) acetone-furfural resin dipping-charing: under the pressure of 2.0MPa, in impregnating autoclave, the precast body that carries out in the step (2) after chemical gas-phase permeation compaction is handled was flooded 4 hours, go out to change over to behind the jar and be cured processing in the curing oven, solidification value is 190 ℃, change over to again carry out in the charring furnace charing handle charcoal/carbon product, carbonization temperature is 1000 ℃;
(4) under hot conditions, the charcoal/carbon product that carries out in the step (3) after charing is handled is carried out pyroprocessing, described pyroprocessing temperature is 1900 ℃;
(5) acetone-furfural resin dipping-charing densification technique is identical with step (3);
(6) charcoal/carbon product density 〉=1.75g/cm
3The time, densification technique finishes, and under 2400 ℃ of conditions charcoal/carbon product is carried out high temperature purification treatment, more than 2000 ℃ the time, feeds chlorine in purifying furnace product inside impurity is reacted removing;
(7) charcoal/carbon product that carries out in the step (6) after the high temperature purification treatment is carried out mechanical workout;
(8) under 1100 ℃ of conditions of temperature, be raw material, in chemical vapor deposition stove, carry out the surface chemistry vapour deposition coating and handle, promptly make charcoal/charcoal air supply nozzle of high temperature furnace carrying out charcoal/carbon product after the mechanical workout in the step (7) with the Sweet natural gas.
The charcoal/charcoal air supply nozzle density of present embodiment preparation is 1.70g/cm
3, tensile strength is 70MPa, and ultimate compression strength is 125Mpa, and ash oontent is 39ppm, and its dimensions is external diameter 100mm, thickness 20mm, height 500mm.
Claims (5)
1. the preparation method of a charcoal/charcoal air supply nozzle of high temperature furnace is characterized in that may further comprise the steps:
(1) adopt charcoal cloth and short carbon fiber net tire alternative stacked, adopt needling process to introduce vertical fortifying fibre at thickness direction, make full carbon fiber pseudo-three-dimensional structure precast body, the density of described precast body is 0.30～0.55g/cm
3
(2) chemical gas-phase permeation compaction is handled: with propylene or Sweet natural gas is raw material Pintsch process in chemical vapor deposition stove, the described precast body in the step (1) is carried out chemical gas-phase permeation compaction handle; Described high-temperature temperature is 940-1060 ℃;
(3) acetone-furfural resin or resin impregnating-charing: under the pressure of 1.5-2.0MPa, in impregnating autoclave, the precast body that carries out in the step (2) after chemical gas-phase permeation compaction is handled was flooded 3.5-4.5 hour, go out to change over to behind the jar and be cured processing in the curing oven, change over to again carry out in the charring furnace charing handle charcoal/carbon product;
(4) under hot conditions, the charcoal/carbon product that carries out in the step (3) after charing is handled is carried out pyroprocessing, described pyroprocessing temperature is 1800-2000 ℃;
(5) acetone-furfural resin or resin impregnating-charing densification technique is identical with step (3);
(6) charcoal/carbon product density 〉=1.75g/cm
3The time, densification technique finishes, and feeds chlorine or freonll-11 in purifying furnace, and charcoal/carbon product is carried out high temperature purification treatment, and described high temperature purification treatment temperature is 2300-2500 ℃;
(7) charcoal/carbon product that carries out in the step (6) after the high temperature purification treatment is carried out mechanical workout;
(8) be raw material with propylene or Sweet natural gas, in chemical vapor deposition stove, carry out the surface chemistry vapour deposition coating and handle, promptly make charcoal/charcoal air supply nozzle of high temperature furnace carrying out charcoal/carbon product after the mechanical workout in the step (7).
2. the preparation method of a kind of charcoal/charcoal air supply nozzle of high temperature furnace according to claim 1 is characterized in that charcoal cloth described in the step (1) is 3～24K plain weave charcoal cloth, and wherein K represents tow thousand radicals.
3. the preparation method of a kind of charcoal/charcoal air supply nozzle of high temperature furnace according to claim 1 is characterized in that the solidified temperature is 190 ℃ described in the step (3), and carbonization temperature is 800-1000 ℃.
4. the preparation method of a kind of charcoal/charcoal air supply nozzle of high temperature furnace according to claim 1 is characterized in that the chemical vapor deposited coatings treatment temp is 900-1100 ℃ described in the step (8).
5. the preparation method of a kind of charcoal/charcoal air supply nozzle of high temperature furnace according to claim 1 is characterized in that made charcoal/charcoal air supply nozzle dimensions is external diameter 30～100mm, thickness 5～20mm, height 150～500mm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101638321B (en) * | 2009-05-15 | 2012-06-06 | 西安超码科技有限公司 | Method for preparing carbon/carbon composite profiles |
| CN101797646B (en) * | 2010-03-25 | 2011-10-19 | 西安超码科技有限公司 | Preparation method of high-strength charcoal/charcoal hot-pressing mould for vacuum hot-pressing furnace |
| CN104557098B (en) * | 2014-12-27 | 2016-09-28 | 西安超码科技有限公司 | A kind of carbon/carbon composite flange and preparation method thereof |
| CN105565838B (en) * | 2015-12-20 | 2019-01-22 | 西安航天动力研究所 | A kind of manufacturing method of coal chemical technology ceramic matric composite burner |
| CN107382355A (en) * | 2017-07-24 | 2017-11-24 | 苏州宏久航空防热材料科技有限公司 | A kind of fine and close C/C composite material and preparation method thereofs |
| CN110483048A (en) * | 2019-09-12 | 2019-11-22 | 北京动力机械研究所 | A kind of graphite heat storage and preparation method thereof |
| CN111099910A (en) * | 2019-12-31 | 2020-05-05 | 中国电子科技集团公司第三十八研究所 | Method for manufacturing non-metal heat dissipation plate of printed board |
| CN111807853B (en) * | 2020-07-07 | 2021-05-28 | 湖南碳谷新材料有限公司 | Carbon-carbon composite material and preparation process and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6399203B1 (en) * | 1999-06-08 | 2002-06-04 | Toyo Tanso Co., Ltd. | Pyrolytic carbon coated carbon fiber reinforced carbon composite and useful as components for pulling single crystal apparatus |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6399203B1 (en) * | 1999-06-08 | 2002-06-04 | Toyo Tanso Co., Ltd. | Pyrolytic carbon coated carbon fiber reinforced carbon composite and useful as components for pulling single crystal apparatus |
Non-Patent Citations (1)
| Title |
|---|
| 李永军等.晶体硅炉用C/C复合材料热场产品的研制.第二届晶体硅太阳电池及材料科学与技术国际研讨会论文集.2007,第126-128页. * |
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