CN102010231A - Method for preparing low-density carbon/carbon composite material surface coating - Google Patents
Method for preparing low-density carbon/carbon composite material surface coating Download PDFInfo
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- CN102010231A CN102010231A CN 201010516935 CN201010516935A CN102010231A CN 102010231 A CN102010231 A CN 102010231A CN 201010516935 CN201010516935 CN 201010516935 CN 201010516935 A CN201010516935 A CN 201010516935A CN 102010231 A CN102010231 A CN 102010231A
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Abstract
The invention discloses a method for preparing a low-density carbon/carbon composite material surface coating, which comprises the following steps of: 1, machining a low-density carbon/carbon composite material serving as a blank; 2, preparing suspension; 3, spraying or brushing a coating; 4, curing; and 5, drying and sintering. The method has simple process and good repeatability, can be used for batch production, and has significance for prolonging the service life of the low-density carbon/carbon composite material in high-temperature furnace equipment. The coating prepared by the method has thermal shock resistance and certain oxidation resistance, the coating is combined with the blank firmly, and dust is prevented from falling.
Description
Technical field
The invention belongs to crystalline silicon equipment thermal field material accessory technical field, be specifically related to a kind of method of low density carbon/carbon composite top coat.
Background technology
Along with the quick growth in solar cell market, silicon single crystal, polysilicon manufacturing were expanded rapidly in recent years, had greatly driven the demand of charcoal/charcoal thermal field material product.Charcoal/charcoal low-density composite is a requisite lagging material in monocrystaline silicon stove, polycrystalline silicon furnace and other industry High Temperature Furnaces Heating Apparatuss.Working temperature is more than 1500 ℃ in monocrystaline silicon stove, the polycrystalline silicon furnace, has the certain vacuum degree, because the cleanliness factor of ore is limited, what can produce oxidizing gas such as carbon monoxide, carbonic acid gas in the stove, and the perforate hole of low density charcoal/raw material of wood-charcoal material is more than 80%, therefore very easily be etched, to low density charcoal/charcoal material surface carry out sealing of hole, coating is handled is to solve a kind of main method of low density charcoal material surface erosive.
A kind of airplane carbon/carbon brake disc inoxidzable coating and coating processes thereof that be used for disclosed among the patent of invention CN1164689C that on September 1st, 2004 was announced.A kind of anti-oxidation protection of the part by carbonaceous Composite Preparation was disclosed among invention disclosed patent on the 30th CN101233341A July in 2008.A kind of preparation method of carbon/carbon compound material surface oxidation-resistant multiple phase coating is disclosed among the patent of invention CN1321092C that on June 13rd, 2007 was announced.A kind of preparation method of charcoal material surface coating for resisting high temperature oxidation is disclosed among the patent of invention CN1297515C that on January 31st, 2007 was announced.Above patent all is preparation methods of higher density charcoal material surface coating, and is not suitable for the crystalline silicon furnace atmosphere to ash content requirement harshness.
A kind of silicon crystal growth oven is disclosed among the patent of invention CN100567217C of on December 9th, 2009 bulletin with high purity cured felt making method, this method with base substrate after the chemical vapour deposition density, density improves surface hardening, use graphitiferous powder coating suspensions coating then, and carrying out the chemical vapour deposition intensive treatment, the high purity cured charcoal felt high-strength light and the steady quality of manufacturing use reliable, but complex technical process, the manufacturing cycle is long.
Summary of the invention
Technical problem to be solved by this invention is that at above-mentioned the deficiencies in the prior art a kind of technological process is simple, the method for the low density carbon/carbon composite top coat of good reproducibility mass production but provide.The coating of preparation has thermal-shock resistance and certain antioxidant property, and coating combines firmly with base substrate, and free from dust comes off, and for prolongation low density carbon/carbon composite important meaning is arranged the work-ing life in High Temperature Furnaces Heating Apparatus equipment.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of method of low density carbon/carbon composite top coat is characterized in that this method may further comprise the steps:
(1) adopting density is 0.2g/cm
3～1.0g/cm
3Carbon/carbon composite as base substrate, billet surface is carried out mechanical workout;
(2) with phenolic resinoid glue and sealing of hole particle by 1～20: 1 mass ratio mixes formation suspension; The mixed glue solution of mixed glue solution, acetone and phenolic resinoid that described phenolic resinoid glue is alcohol and phenolic resinoid or the mixed glue solution of water and water soluble phenol resin, the mass percent of phenolic resinoid or water soluble phenol resin is 10%～50% in the phenolic resinoid glue; Described sealing of hole particle is silica flour and/or Graphite Powder 99;
(3) billet surface that suspension described in the step (2) is sprayed or brushes after processing described in the step (1) forms coating;
(4) base substrate that surface described in the step (3) is formed coating dries and is placed in the baking oven, in temperature is to solidify 0.5h～2h under 160 ℃～250 ℃ the condition;
(5) base substrate after solidifying described in the step (4) is placed in the High Temperature Furnaces Heating Apparatus carbon/carbon composite after furnace cooling obtains coating after the drying and sintering under nitrogen or the argon shield; The condition of described drying and sintering is: be to be warming up to 900 ℃～2500 ℃ under the condition of 5 ℃/h～200 ℃/h at temperature rise rate, be incubated 2h～6h then.
Phenolic resinoid is ammonia resol, ba phenolic resin, boron bakelite resin or water soluble phenol resin described in the above-mentioned steps (2).
The particle diameter of silica flour described in the above-mentioned steps (2) is 200 orders～600 orders, and the particle diameter of described Graphite Powder 99 is 200 orders～600 orders.
The thickness of coating described in the above-mentioned steps (3) is 2 μ m～50 μ m.
The present invention compared with prior art has the following advantages:
(1) technological process is simple, good reproducibility, but mass production.
(2) adopt spraying or brushing, coat-thickness is controlled and coating is even.
(3) spray-on coating after drying sintering is handled the low density material sealing of hole, avoids low density raw material of wood-charcoal material is increased weight.
(4) Zhi Bei coating has thermal-shock resistance and certain antioxidant property, and coating combines firmly with base substrate, and free from dust comes off.The present invention has important meaning the work-ing life in High Temperature Furnaces Heating Apparatus equipment for prolonging the low density carbon/carbon composite.
Embodiment
Embodiment 1
(1) adopting density is 0.2g/cm
3Carbon/carbon composite as base substrate, billet surface is carried out mechanical workout;
(2) phenolic resinoid glue and sealing of hole particle are mixed formation suspension by 1: 1 mass ratio, the mixed glue solution of mixed glue solution, acetone and phenolic resinoid that described phenolic resinoid glue is alcohol and phenolic resinoid or the mixed glue solution of water and water soluble phenol resin, the mass percent of phenolic resinoid or water soluble phenol resin is 10% in the phenolic resinoid glue, described sealing of hole particle is silica flour and/or Graphite Powder 99, the particle diameter of described silica flour is 600 orders, and the particle diameter of described Graphite Powder 99 is 600 orders;
(3) suspension being sprayed at billet surface after the processing, to form thickness be the coating of 2 μ m;
(4) base substrate that the surface is formed coating dries and is placed in the baking oven, in temperature is to solidify 2h under 160 ℃ the condition;
(5) base substrate after will solidifying places in the High Temperature Furnaces Heating Apparatus, the carbon/carbon composite after furnace cooling obtains coating after the drying and sintering under protection of nitrogen gas, and the condition of described drying and sintering is: be to be warming up to 900 ℃ under the condition of 5 ℃/h at temperature rise rate, be incubated 6h then.
Carbon/carbon composite after the coating of present embodiment preparation as heat insulating assembly in the polysilicon hydrogenation furnace, uses 1000h under 1300 ℃ of conditions of temperature, top coat does not have and comes off weightless 1.2%.
Embodiment 2
(1) adopting density is 1.0g/cm
3Carbon/carbon composite as base substrate, billet surface is carried out mechanical workout;
(2) phenolic resinoid glue and sealing of hole particle are mixed formation suspension by 20: 1 mass ratio; The mixed glue solution of mixed glue solution, acetone and phenolic resinoid that described phenolic resinoid glue is alcohol and phenolic resinoid or the mixed glue solution of water and water soluble phenol resin, the mass percent of phenolic resinoid or water soluble phenol resin is 50% in the phenolic resinoid glue, described sealing of hole particle is silica flour and/or Graphite Powder 99, the particle diameter of described silica flour is 400 orders, and the particle diameter of described Graphite Powder 99 is 200 orders;
(3) suspension being sprayed at billet surface after the processing, to form thickness be the coating of 26 μ m;
(4) base substrate that the surface is formed coating dries and is placed in the baking oven, in temperature is to solidify 0.5h under 200 ℃ the condition;
(5) base substrate after will solidifying places in the High Temperature Furnaces Heating Apparatus; carbon/carbon composite after furnace cooling obtains coating after the drying and sintering under protection of nitrogen gas; the condition of described drying and sintering is: be to be warming up to 1700 ℃ under the condition of 200 ℃/h at temperature rise rate, be incubated 4h then.
Carbon/carbon composite after the coating of present embodiment preparation as heat insulating assembly in the polysilicon hydrogenation furnace, uses 1000h under 1200 ℃ of conditions of temperature, top coat does not have and comes off weightless 0.8%.
Embodiment 3
(1) adopting density is 0.6g/cm
3Carbon/carbon composite as base substrate, billet surface is carried out mechanical workout;
(2) phenolic resinoid glue and sealing of hole particle are mixed formation suspension by 10: 1 mass ratio; The mixed glue solution of mixed glue solution, acetone and phenolic resinoid that described phenolic resinoid glue is alcohol and phenolic resinoid or the mixed glue solution of water and water soluble phenol resin, the mass percent of phenolic resinoid or water soluble phenol resin is 30% in the phenolic resinoid glue, described sealing of hole particle is silica flour and/or Graphite Powder 99, the particle diameter of described silica flour is 300 orders, and the particle diameter of described Graphite Powder 99 is 400 orders;
(3) suspension being sprayed at billet surface after the processing, to form thickness be the coating of 50 μ m;
(4) base substrate that the surface is formed coating dries and is placed in the baking oven, in temperature is to solidify 1.2h under 180 ℃ the condition;
(5) base substrate after will solidifying places in the High Temperature Furnaces Heating Apparatus; carbon/carbon composite after furnace cooling obtains coating after the drying and sintering under the protection of argon gas; the condition of described drying and sintering is: be to be warming up to 2500 ℃ under the condition of 102 ℃/h at temperature rise rate, be incubated 2h then.
Carbon/carbon composite after the coating of present embodiment preparation as heat insulating assembly in the polysilicon hydrogenation furnace, uses 1000h under 1500 ℃ of conditions of temperature, top coat does not have and comes off weightless 1%.
Embodiment 4
(1) adopting density is 0.4g/cm
3Carbon/carbon composite as base substrate, billet surface is carried out mechanical workout;
(2) phenolic resinoid glue and sealing of hole particle are mixed formation suspension by 11: 1 mass ratio; The mixed glue solution of mixed glue solution, acetone and phenolic resinoid that described phenolic resinoid glue is alcohol and phenolic resinoid or the mixed glue solution of water and water soluble phenol resin, the mass percent of phenolic resinoid or water soluble phenol resin is 40% in the phenolic resinoid glue, described sealing of hole particle is silica flour and/or Graphite Powder 99, the particle diameter of described silica flour is 400 orders, and the particle diameter of described Graphite Powder 99 is 600 orders;
(3) the billet surface formation thickness of suspension being brushed after processing is the coating of 2 μ m;
(4) base substrate that the surface is formed coating dries and is placed in the baking oven, in temperature is to solidify 1h under 200 ℃ the condition;
(5) base substrate after will solidifying places in the High Temperature Furnaces Heating Apparatus; carbon/carbon composite after furnace cooling obtains coating after the drying and sintering under the protection of argon gas; the condition of described drying and sintering is: be to be warming up to 2500 ℃ under the condition of 200 ℃/h at temperature rise rate, be incubated 3h then.
Carbon/carbon composite after the coating of present embodiment preparation as heat insulating assembly in the polysilicon hydrogenation furnace, uses 2000h under 1500 ℃ of conditions of temperature, top coat does not have and comes off.
Embodiment 5
(1) adopting density is 0.2g/cm
3Carbon/carbon composite as base substrate, billet surface is carried out mechanical workout;
(2) phenolic resinoid glue and sealing of hole particle are mixed formation suspension by 15: 1 mass ratio; The mixed glue solution of mixed glue solution, acetone and phenolic resinoid that described phenolic resinoid glue is alcohol and phenolic resinoid or the mixed glue solution of water and water soluble phenol resin, the mass percent of phenolic resinoid or water soluble phenol resin is 20% in the phenolic resinoid glue, described sealing of hole particle is silica flour and/or Graphite Powder 99, the particle diameter of described silica flour is 200 orders, and the particle diameter of described Graphite Powder 99 is 200 orders;
(3) the billet surface formation thickness of suspension being brushed after processing is the coating of 50 μ m;
(4) base substrate that the surface is formed coating dries and is placed in the baking oven, in temperature is to solidify 0.5h under 160 ℃ the condition;
(5) base substrate after will solidifying places in the High Temperature Furnaces Heating Apparatus; carbon/carbon composite after furnace cooling obtains coating after the drying and sintering under protection of nitrogen gas; the condition of described drying and sintering is: be to be warming up to 900 ℃ under the condition of 100 ℃/h at temperature rise rate, be incubated 4h then.
Carbon/carbon composite after the coating of present embodiment preparation as heat insulating assembly in the polysilicon hydrogenation furnace, uses 2000h under 1450 ℃ of conditions of temperature, top coat does not have and comes off.
Embodiment 6
(1) adopting density is 0.8g/cm
3Carbon/carbon composite as base substrate, billet surface is carried out mechanical workout;
(2) phenolic resinoid glue and sealing of hole particle are mixed formation suspension by 20: 1 mass ratio; The mixed glue solution of mixed glue solution, acetone and phenolic resinoid that described phenolic resinoid glue is alcohol and phenolic resinoid or the mixed glue solution of water and water soluble phenol resin, the mass percent of phenolic resinoid or water soluble phenol resin is 50% in the phenolic resinoid glue, described sealing of hole particle is silica flour and/or Graphite Powder 99, the particle diameter of described silica flour is 400 orders, and the particle diameter of described Graphite Powder 99 is 400 orders;
(3) the billet surface formation thickness of suspension being brushed after processing is the coating of 30 μ m;
(4) base substrate that the surface is formed coating dries and is placed in the baking oven, in temperature is to solidify 1.5h under 205 ℃ the condition;
(5) base substrate after will solidifying places in the High Temperature Furnaces Heating Apparatus; carbon/carbon composite after furnace cooling obtains coating after the drying and sintering under the protection of argon gas; the condition of described drying and sintering is: be to be warming up to 1500 ℃ under the condition of 100 ℃/h at temperature rise rate, be incubated 2h then.
Carbon/carbon composite after the coating of present embodiment preparation as heat insulating assembly in the polysilicon hydrogenation furnace, uses 1700h under 1100 ℃ of conditions of temperature, top coat does not have and comes off weightless 0.5%.
Claims (4)
1. the method for a low density carbon/carbon composite top coat is characterized in that, this method may further comprise the steps:
(1) adopting density is 0.2g/cm
3～1.0g/cm
3Carbon/carbon composite as base substrate, billet surface is carried out mechanical workout;
(2) with phenolic resinoid glue and sealing of hole particle by 1～20: 1 mass ratio mixes formation suspension; The mixed glue solution of mixed glue solution, acetone and phenolic resinoid that described phenolic resinoid glue is alcohol and phenolic resinoid or the mixed glue solution of water and water soluble phenol resin, the mass percent of phenolic resinoid or water soluble phenol resin is 10%～50% in the phenolic resinoid glue; Described sealing of hole particle is silica flour and/or Graphite Powder 99;
(3) billet surface that suspension described in the step (2) is sprayed or brushes after processing described in the step (1) forms coating;
(4) base substrate that surface described in the step (3) is formed coating dries and is placed in the baking oven, in temperature is to solidify 0.5h～2h under 160 ℃～250 ℃ the condition;
(5) base substrate after solidifying described in the step (4) is placed in the High Temperature Furnaces Heating Apparatus carbon/carbon composite after furnace cooling obtains coating after the drying and sintering under nitrogen or the argon shield; The condition of described drying and sintering is: be to be warming up to 900 ℃～2500 ℃ under the condition of 5 ℃/h～200 ℃/h at temperature rise rate, be incubated 2h～6h then.
2. the method for a kind of low density carbon/carbon composite top coat according to claim 1 is characterized in that, phenolic resinoid is ammonia resol, ba phenolic resin, boron bakelite resin or water soluble phenol resin described in the step (2).
3. the method for a kind of low density carbon/carbon composite top coat according to claim 1 is characterized in that, the particle diameter of silica flour described in the step (2) is 200 orders～600 orders, and the particle diameter of described Graphite Powder 99 is 200 orders～600 orders.
4. the method for a kind of low density carbon/carbon composite top coat according to claim 1 is characterized in that, the thickness of coating described in the step (3) is 2 μ m～50 μ m.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276278A (en) * | 2011-05-26 | 2011-12-14 | 中材高新材料股份有限公司 | Preparation method of inorganic composite coating on surface of silica fiber-reinforced silica-based composite material |
| CN103058712A (en) * | 2013-01-10 | 2013-04-24 | 湖南南方搏云新材料有限责任公司 | C/SiC composite coating applied to surface of low-density carbon/carbon composite material and preparation process thereof |
| CN103722786A (en) * | 2013-09-11 | 2014-04-16 | 太仓派欧技术咨询服务有限公司 | Laminated hybrid heatproof composite structured material |
| CN105113002A (en) * | 2015-09-30 | 2015-12-02 | 吉林联科特种石墨材料有限公司 | Preparation method of monocrystalline silicon growth furnace guide cylinder integrally formed by functional carbon felt |
| CN105541364A (en) * | 2015-12-16 | 2016-05-04 | 浙江亚太机电股份有限公司 | Method for producing carbon-ceramic automobile brake disc through one-step densification production |
| CN106752644A (en) * | 2016-12-26 | 2017-05-31 | 上海东洋炭素有限公司 | One kind solidification felt surface self-healing anti-oxidation coating and preparation method thereof |
| CN108218460A (en) * | 2018-01-24 | 2018-06-29 | 航天睿特碳材料有限公司 | A kind of middle low-density surface of carbon/carbon composite Enhancement Method |
| CN109824380A (en) * | 2019-03-28 | 2019-05-31 | 山东众途复合材料有限公司 | A kind of preparation method of the carbon fiber thermal insulating material coated with anti-oxidant shock resistance coating |
| CN112624782A (en) * | 2020-12-11 | 2021-04-09 | 包头美科硅能源有限公司 | Application method of crucible edge coating |
| CN112723898A (en) * | 2020-12-30 | 2021-04-30 | 内蒙古栢特新材料科技有限公司 | Preparation method of carbon/carbon liner for natural gas chemical vapor deposition furnace |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276278B (en) * | 2011-05-26 | 2012-12-12 | 中材高新材料股份有限公司 | Preparation method of inorganic composite coating on surface of silica fiber-reinforced silica-based composite material |
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| CN103058712A (en) * | 2013-01-10 | 2013-04-24 | 湖南南方搏云新材料有限责任公司 | C/SiC composite coating applied to surface of low-density carbon/carbon composite material and preparation process thereof |
| CN103722786A (en) * | 2013-09-11 | 2014-04-16 | 太仓派欧技术咨询服务有限公司 | Laminated hybrid heatproof composite structured material |
| CN105113002A (en) * | 2015-09-30 | 2015-12-02 | 吉林联科特种石墨材料有限公司 | Preparation method of monocrystalline silicon growth furnace guide cylinder integrally formed by functional carbon felt |
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| CN105541364A (en) * | 2015-12-16 | 2016-05-04 | 浙江亚太机电股份有限公司 | Method for producing carbon-ceramic automobile brake disc through one-step densification production |
| CN106752644A (en) * | 2016-12-26 | 2017-05-31 | 上海东洋炭素有限公司 | One kind solidification felt surface self-healing anti-oxidation coating and preparation method thereof |
| CN108218460A (en) * | 2018-01-24 | 2018-06-29 | 航天睿特碳材料有限公司 | A kind of middle low-density surface of carbon/carbon composite Enhancement Method |
| CN109824380A (en) * | 2019-03-28 | 2019-05-31 | 山东众途复合材料有限公司 | A kind of preparation method of the carbon fiber thermal insulating material coated with anti-oxidant shock resistance coating |
| CN109824380B (en) * | 2019-03-28 | 2021-09-14 | 山东众途复合材料有限公司 | Preparation method of carbon fiber thermal insulation material coated with antioxidant impact-resistant coating |
| CN112624782A (en) * | 2020-12-11 | 2021-04-09 | 包头美科硅能源有限公司 | Application method of crucible edge coating |
| CN112723898A (en) * | 2020-12-30 | 2021-04-30 | 内蒙古栢特新材料科技有限公司 | Preparation method of carbon/carbon liner for natural gas chemical vapor deposition furnace |
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