CN103044077B - Carbon/carbon crucible side oxidation resistant coating and preparation method thereof - Google Patents
Carbon/carbon crucible side oxidation resistant coating and preparation method thereof Download PDFInfo
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- CN103044077B CN103044077B CN201310007859.0A CN201310007859A CN103044077B CN 103044077 B CN103044077 B CN 103044077B CN 201310007859 A CN201310007859 A CN 201310007859A CN 103044077 B CN103044077 B CN 103044077B
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Abstract
The invention discloses a carbon/carbon crucible side oxidation resistant coating, and a preparation method thereof. The oxidation resistant coating comprises the following raw materials by weight percentage: 10-40% of silicon carbide powder, 2-20% of silicon powder, 20-60% of resin, 20-35% of a diluent and 1-6% of a curing agent. The invention further discloses the preparation method of the carbon/carbon crucible side oxidation resistant coating. The carbon/carbon crucible side oxidation resistant coating is high in oxidation resistance; the binding strength between the coating and a matrix material is better; no crack exists; no powder falls; the preparation method of the carbon/carbon crucible side oxidation resistant coating does not requires high-temperature sintering treatment, and is shorter in preparation technology flow, and good in repeatability.
Description
Technical field
The present invention relates to the surface treatment of carbon/carbon composite, be specifically related to a kind of charcoal/charcoal crucible and help oxidation resistant coating and preparation method thereof.
Background technology
The crucible consisting of crucible side and crucible holder protects the major parts that crucible is silicon crystal growth oven thermal field system, protects the quartz crucible of the built-in dress silicon of crucible material.The growth temperature of silicon single-crystal is 1450 ℃ of left and right, corrosion and erosion that in crystal pulling process, crucible side need bear silicon oxide, silicon vapor for a long time, and intensity and the thermostability thereof of crucible side play a decisive role to the safety of thermal field system.Therefore,, for improving antioxidant property and the thermal stability of crucible side, to crucible, side carries out coating processing.SiC coating thermostability is high, and good with carbon matrix chemical compatibility, thermal expansivity is close, is the current main coating for Carbon Materials oxidation protection.
At present, the main method of preparation SiC coating has: entrapping method, chemical vapour deposition, plasma spraying method, but SiC coating prepared by this several method generally contains a lot of micro-holes and microcracks, and resistance of oxidation is not strong, and thermal shock resistance is not good enough.In order to improve resistance of oxidation and the thermal shock resistance of SiC coating, people adopt again diverse ways to carry out packing crackle, such as sol-gel processing shutoff etc., but whole process relative complex, economic benefit is low; Meanwhile, very harsh to ash content requirement in monocrystalline silicon stove, particularly metal ion directly affects the quality of crystal pulling, so coating formula is chosen extremely strict, to consider antioxidant effect, and will control foreign matter content, need technique simple, low cost of manufacture simultaneously.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of technique simple, low cost of manufacture, charcoal/charcoal crucible side oxidation resistant coating that resistance of oxidation is strong under hot conditions and preparation method thereof.
The technical scheme that the present invention solves its technical problem employing is:
Charcoal/charcoal crucible side oxidation resistant coating of the present invention, raw material by following weight percent is made: carborundum powder 10%～40%(preferably 20%～30%), silica flour 2%～20%(preferably 3%～10%), resin 20%～60%(preferably 25%～50%), thinner 20%～35%(preferably 25%～30%), solidifying agent 1%～6%(preferably 2%～5%).
The preparation method of charcoal/charcoal crucible side oxidation resistant coating of the present invention, comprises the following steps:
(1) smooth with 400～800 object sand paperings to the surface of charcoal/charcoal crucible side, with suction cleaner, suck floating dust;
(2) carborundum powder 10%～40%(preferably 20%～30% by weight ratio), silica flour 2%～20%(preferably 3%～10%), resin 20%～60%(preferably 25%～50%), thinner 20%～35%(preferably 25%～30%), solidifying agent 1%～6%(preferably 2%～5%) each raw material is mixed, stir, obtain slurry; With gained slurry, adopt the mode of spraying or brushing to be coated on the charcoal/charcoal crucible side surface after step (1) is processed, coating thickness 30～50 μ m;
(3) charcoal/charcoal crucible side after coating is processed is dried in the air after 1～2 hour at ambient temperature, be placed in curing oven and be cured processing, with the temperature rise rate of 50 ± 2 ℃/h, be warming up to after 120～260 ℃ (preferably 200～240 ℃) afterheat baking 1～2 hour;
(4) charcoal/charcoal crucible side after solidification treatment is inserted in chemical vapor deposition stove, coating is carried out to densification, chemical vapour deposition temperature is 900～1100 ℃, depositing time 10～20 hours, hydrocarbon gas flow is 30～50L/min (preferably 35～45L/min), and nitrogen flow is preferably 16～20L/min of 15～30L/min().
Further, in step (2), described carborundum powder is α-SiC, and granularity is 400～1200 orders, and silicon particle size is 400～800 orders.
Further, in step (2), described resin is furane resin, epoxy resin, resol or silicone resin.
Further, in step (2), described thinner is ethanol or acetone.
Further, in step (2), described solidifying agent is tosic acid.
Further, in step (4), described hydrocarbon gas is methane, propane or propylene.
Compared with prior art, the present invention has the following advantages: prepared oxidation resistant coating need not be processed through high temperature sintering, and preparation technology's flow process is shorter, reproducible; The good bonding strength of coating resistance of oxidation strong and coating and body material, flawless, without powder falling phenomenon.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
Charcoal/charcoal crucible side oxidation resistant coating of the present embodiment, is made by the raw material of following weight percent: carborundum powder 20%, silica flour 3%, resin 50%, thinner 25%, solidifying agent 2%.
The preparation method of charcoal/charcoal crucible side oxidation resistant coating of the present embodiment, comprises the following steps:
(1) adopting density is 1.5g/cm
3, external diameter is 540mm, internal diameter is 508mm, is highly charcoal/charcoal crucible side of 395mm, smooth with 400 object sand paperings to its surface, with suction cleaner, sucks floating dust;
(2) carborundum powder 20% by weight ratio, silica flour 3%, resin 50%, thinner 25%, solidifying agent 2% mixes each raw material, stirs, and obtains slurry; With gained slurry, adopt the mode of spraying to be coated on the charcoal/charcoal crucible side surface after step (1) is processed, coating thickness 40 μ m;
Described carborundum powder is α-SiC, and granularity is 400 orders; Silicon particle size is 800 orders; Described resin is resol; Described thinner is acetone; Described solidifying agent is tosic acid;
(3) charcoal/charcoal crucible side after coating is processed is dried in the air after 2 hours at ambient temperature, be placed in curing oven and be cured processing, with the temperature rise rate of 50 ± 2 ℃/h, be warming up to after 240 ℃ afterheat baking 1 hour;
(4) charcoal/charcoal crucible side after solidification treatment is inserted in chemical vapor deposition stove, coating is carried out to densification, chemical vapour deposition temperature is 1100 ℃, depositing time 20 hours, and hydrocarbon gas propane flow is 45L/min, nitrogen flow is 20L/min.
Charcoal/charcoal crucible prepared by the present embodiment side oxidation resistant coating, for silicon crystal growth oven thermal field system, is to use 1500 hours under the condition of 1500 ℃ in temperature, and top coat comes off, powder falling phenomenon, and weightless about 1.5%(is in Table 1).
Embodiment 2
Charcoal/charcoal crucible side oxidation resistant coating of the present embodiment, is made by the raw material of following weight percent: carborundum powder 30%, silica flour 10%, resin 25%, thinner 30%, solidifying agent 5%.
The preparation method of charcoal/charcoal crucible side oxidation resistant coating of the present embodiment, comprises the following steps:
(1) adopting density is 1.5g/cm
3, external diameter is 636mm, internal diameter is 616mm, is highly charcoal/charcoal crucible side of 255mm, smooth with 400 object sand paperings to its surface, surface, with suction cleaner, sucks floating dust;
(2) carborundum powder 30% by weight ratio, silica flour 10%, resin 25%, thinner 30%, solidifying agent 5% mixes each raw material, stirs, obtain slurry, the charcoal/charcoal crucible side that adopts the mode of spraying to be coated on after step (1) is processed with gained slurry is surperficial, coating thickness 40 μ m;
Described carborundum powder is α-SiC, and granularity is 400 orders; Silicon particle size is 800 orders; Described resin is furane resin; Described thinner is ethanol; Described solidifying agent is tosic acid;
(3) charcoal/charcoal crucible side after coating is processed is dried in the air after 1 hour at ambient temperature, be placed in curing oven and be cured processing, with the temperature rise rate of 50 ± 2 ℃/h, be warming up to after 220 ℃ afterheat baking 1.5 hours;
(4) charcoal/charcoal crucible side after solidification treatment is inserted in chemical vapor deposition stove, coating is carried out to densification, and chemical vapour deposition temperature is 980 ℃, depositing time 10 hours, in chemical vapor deposition process, propane flow is 35L/min, and nitrogen flow is 16L/min.
Charcoal/charcoal crucible prepared by the present embodiment side oxidation resistant coating, for silicon crystal growth oven thermal field system, is to use 1500 hours under the condition of 1500 ℃ in temperature, and top coat comes off, powder falling phenomenon, and weightless about 1.6%(is in Table 2).
Table 1 charcoal/charcoal crucible side antioxidant property test result
| Time (h) | 60 | 120 | 180 | … | 1380 | 1440 | 1500 |
| Rate of weight loss (%) | 0.5 | 0.52 | 0.52 | … | 1.42 | 1.45 | 1.51 |
Table 2 charcoal/charcoal crucible side antioxidant property test result
| Time (h) | 60 | 120 | 180 | … | 1380 | 1440 | 1500 |
| Rate of weight loss (%) | 0.48 | 0.51 | 0.52 | … | 1.56 | 1.57 | 1.59 |
Claims (7)
1. a preparation method for charcoal/charcoal crucible side oxidation resistant coating, is characterized in that, is made: carborundum powder 10%～40%, silica flour 2%～20%, resin 20%～60%, thinner 20%～35%, solidifying agent 1%～6% by the raw material of following weight percent;
Described charcoal/charcoal crucible is helped the preparation method of oxidation resistant coating, comprises the following steps:
(1) smooth with 400～800 object sand paperings to the surface of charcoal/charcoal crucible side, with suction cleaner, suck floating dust;
(2) carborundum powder 10%～40% by weight ratio, silica flour 2%～20%, resin 20%～60%, thinner 20%～35%, solidifying agent 1%～6% mixes each raw material, stirs, and obtains slurry; With gained slurry, adopt the mode of spraying or brushing to be coated on the charcoal/charcoal crucible side surface after step (1) is processed, coating thickness 30～50 μ m;
(3) charcoal/charcoal crucible side after coating is processed is dried in the air after 1～2 hour at ambient temperature, be placed in curing oven and be cured processing, with the temperature rise rate of 50 ± 2 ℃/h, be warming up to after 120～260 ℃ afterheat baking 1～2 hour;
(4) charcoal/charcoal crucible side after solidification treatment is inserted in chemical vapor deposition stove, coating is carried out to densification, and chemical vapour deposition temperature is 900～1100 ℃, depositing time 10～20 hours, hydrocarbon gas flow is 30～50L/min, and nitrogen flow is 15～30L/min.
2. charcoal/charcoal crucible according to claim 1 is helped the preparation method of oxidation resistant coating, it is characterized in that, is made: carborundum powder 20%～30% by the raw material of following weight percent, silica flour 3%～10%, resin 25%～50%, thinner 25%～30%, solidifying agent 2%～5%.
3. charcoal/charcoal crucible according to claim 1 and 2 is helped the preparation method of oxidation resistant coating, it is characterized in that, in step (2), described carborundum powder is α-SiC, and granularity is 400～1200 orders, and silicon particle size is 400～800 orders.
4. charcoal/charcoal crucible according to claim 1 and 2 is helped the preparation method of oxidation resistant coating, it is characterized in that, in step (2), described resin is furane resin, epoxy resin, resol or silicone resin.
5. charcoal/charcoal crucible according to claim 1 and 2 is helped the preparation method of oxidation resistant coating, it is characterized in that, in step (2), described thinner is ethanol or acetone.
6. charcoal/charcoal crucible according to claim 1 and 2 is helped the preparation method of oxidation resistant coating, it is characterized in that, in step (2), described solidifying agent is tosic acid.
7. charcoal/charcoal crucible according to claim 1 and 2 is helped the preparation method of oxidation resistant coating, it is characterized in that, in step (4), described hydrocarbon gas is methane, propane or propylene.
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| CN201310007859.0A CN103044077B (en) | 2013-01-10 | 2013-01-10 | Carbon/carbon crucible side oxidation resistant coating and preparation method thereof |
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| CN106065279B (en) * | 2016-06-02 | 2017-12-22 | 聊城鼎硕新材料有限公司 | A kind of antioxidizing paint and its application method |
| CN106431498B (en) * | 2016-09-05 | 2019-05-28 | 江苏协鑫特种材料科技有限公司 | A method of preparing graphite/carbon SiClx densified composite |
| CN109456063B (en) * | 2018-12-07 | 2022-07-12 | 烟台凯泊复合材料科技有限公司 | CF/Si of monocrystalline silicon drawing furnace3N4Composite material crucible side and preparation method thereof |
| CN110304946B (en) * | 2019-08-02 | 2022-02-01 | 航天特种材料及工艺技术研究所 | Wide-temperature-range antioxidant coating on surface of ceramic matrix composite and preparation method thereof |
| 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 |
| CN115073212B (en) * | 2022-06-02 | 2023-02-10 | 陕西美兰德炭素有限责任公司 | Aluminum silicate-silicon carbide high-temperature-resistant and silicon vapor corrosion-resistant coating and preparation method thereof |
| CN115449242B (en) * | 2022-09-20 | 2023-07-04 | 晶科能源股份有限公司 | Anti-overflow silicon paint, coating and single crystal furnace |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86108553A (en) * | 1986-12-17 | 1987-07-22 | 江西坩埚厂 | Induction furnace made of graphite component |
| CN87104145A (en) * | 1987-06-09 | 1988-03-16 | 天津市耐火器材厂 | Graphite crucible for smelting noble metals and manufacture method thereof |
| CN102260901A (en) * | 2011-06-29 | 2011-11-30 | 罗万前 | SiC composite crucible containing coating and preparation method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86108553A (en) * | 1986-12-17 | 1987-07-22 | 江西坩埚厂 | Induction furnace made of graphite component |
| CN87104145A (en) * | 1987-06-09 | 1988-03-16 | 天津市耐火器材厂 | Graphite crucible for smelting noble metals and manufacture method thereof |
| CN102260901A (en) * | 2011-06-29 | 2011-11-30 | 罗万前 | SiC composite crucible containing coating and preparation method |
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