CN103570378A - Method for direct deposition of silicon carbide (SiC) coating on carbon material surface in graphite heat-generating body heating furnace - Google Patents
Method for direct deposition of silicon carbide (SiC) coating on carbon material surface in graphite heat-generating body heating furnace Download PDFInfo
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Abstract
The invention provides a method for direct deposition of a silicon carbide (SiC) coating on a carbon material surface in a graphite heat-generating body heating furnace, and the method comprises the following steps: (1) vacuumizing the graphite heat-generating body heating furnace body as a deposition furnace to a vacuum degree reaching below 10<-1>Pa; (2) raising the temperature of the graphite heat-generating body heating furnace to 1000 to 1200 DEG C; (3) using hydrogen as a carrier gas, using a bubbling method to lead methyltrichlorosilane into a graphite heat-generating body heating furnace chamber, regulating the carrier gas flow rate, according to the furnace body size, to 200 ~ 800ml / min, at the same time, using argon with the flow rate of 200 ~ 800ml / min as a dilution gas, keeping the heating furnace chamber pressure to be 3*10<3>~10<5>Pa for deposition for 20 ~ 50 hours, and cooling to form the silicon carbide (SiC) coating on the carbon material surface. According to the method, no special chemical vapor deposition equipment is needed in a preparation process, and the prepared silicon carbide (SiC) coating is good in quality, and large, flexible and controllable in coating thickness.
Description
Technical field
The present invention relates to a kind of preparation method of SiC coated material, particularly relate to the method for carbon materials surface Direct precipitation SiC coating in a kind of graphite heater process furnace.
Background technology
Graphite has good conduction, heat conductivility, and hot strength is good, and in extraordinary industrial furnace, conventional graphite is as heating element.Along with the development in an all-round way of semi-conductor industry, refine silicon single crystal, monocrystalline germanium, the process furnace of the materials such as gallium arsenide, indium phosphide selects special graphite to make heating element, and the industrial furnace that some are special and experimental furnace Yong Tanbuhuo Graphite cloth make heating element.Except graphite heater, plumbago crucible, the carbon materialses such as charcoal element lagging material are used in a large number in extraordinary industrial furnace, especially in the wafer growth furnace in semi-conductor industry.The loss of carbon materials core component takies wafer manufacturing cost very at high proportion, and carbon graphite material parts consumption is very big, and belongs to attrition component, and this is also that wafer manufacturing cost is difficult to one of reason reducing.
Owing to usually will reaching 1500 ℃ of above working temperatures in wafer growth furnace, the carbon atom in carbon materials can continue volatilization in High Temperature Furnaces Heating Apparatus, thereby brings two negative impacts: the one, and carbon atom diffuses into wafer, causes wafer quality to decline; The 2nd, graphite surface produces macro-corrosion hole, and service life reduces.At present, along with wafer industry size sharply expands, in photovoltaic industry, improve quality, reduce costs the key that becomes industry development, an urgent demand extends the graphite field material military service time.It is to solve carbon atom volatilization that carbon materials in wafer growth furnace is carried out to coating processing, improves a kind of main method of its service life.Coat of silicon carbide novel material thermal conductivity is high, thermal expansivity is little, carbon diffusion coefficient is little, stable chemical performance, abrasion resistance properties are good, has high temperature resistant, anti-thermal shock, creep resistance, oxidation resistant advantage.At aerospace field, coat of silicon carbide has been used as the high temperature coating of carbon material and carbon/carbon composite, resists the gas-flow of 2500-3000 ℃, shows good anti-oxidant, anti-ablation characteristics.SiC coatings applications, to the carbon materialses such as graphite heater in wafer growth furnace in semi-conductor industry, is expected to wafer quality to improve 3～5 times, and the life-span of graphite nuclei parts is improved 6～10 times, and Business Economic Benefit can significantly promote.
Chemical vapour deposition (CVD) is to be applicable to one of major technique of preparation SiC coating.It is very high that CVD method is prepared SiC coating quality, and can realize large area deposition.In silicon wafer stove, carbon materials parts are a lot, and most of component shape is comparatively complicated.If carbon materials all parts is prepared separately to SiC coating, cost can increase considerably.
Summary of the invention
Problem to be solved by this invention is the method that proposes carbon materials surface Direct precipitation SiC coating in a kind of graphite heater process furnace.
Operating process:
A method for carbon materials surface Direct precipitation SiC coating in graphite heater process furnace, its feature comprises the step of following order:
(1) using graphite heater heating furnace body as cvd furnace, vacuumized, vacuum tightness reaches 10
-1below Pa;
(2) temperature in graphite heater process furnace is increased to 1000～1200 ℃, temperature rise rate is 8～12 ℃ of per minutes;
(3) take hydrogen as carrier gas, by Bubbling method, trichloromethyl silane is brought in graphite heater heating furnace chamber, carrier gas flux regulates according to body of heater size, flow is 200～800ml/min, using argon gas as diluent gas simultaneously, its flow is 200～800ml/min, and keeping heating furnace chamber internal pressure is 3 * 10
3～10
5pa, deposits 20～50 hours, cooling after, there is SiC coating in carbon materials surface.
Wherein:
Graphite heater process furnace can be the process furnace of smelting quartz glass, refines silicon single crystal, monocrystalline germanium, the process furnace of gallium arsenide, indium phosphide.
Carbon materials parts comprise plumbago crucible, graphite field material, charcoal element lagging material.
Diluent gas purity of argon is more than 99.999%.
The mol ratio of hydrogen and trichloromethyl silane is more than or equal to 10.
In the present invention, major advantage is: it is good that (1) prepares SiC coating quality; (2) coating preparation process does not need special-purpose chemical vapor depsotition equipment, and cost is low; (3) coat-thickness is large and controlled flexibly.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment is only not used in and limits the scope of the invention for the present invention is described, after having read the present invention, those skilled in the art all fall within the application's claims to the modification of the various equivalent form of values of the present invention and limit.
Embodiment 1
(1) using graphite heater heating furnace body as cvd furnace, vacuumized, vacuum tightness reaches 5 * 10
-2pa;
(2) temperature in graphite heater process furnace is increased to 1100 ℃, temperature rise rate is 8 ℃ of per minutes;
(3) take hydrogen as carrier gas, by Bubbling method, trichloromethyl silane being brought into diameter is that in the graphite heater heating furnace chamber of 1 meter, carrier gas flux is 400ml/min, usings 99.9999% argon gas simultaneously as diluent gas, its flow is 400ml/min, and keeping heating furnace chamber internal pressure is 5 * 10
4pa, deposits 40 hours, cooling after, there is SiC coating in carbon materials surface.
Embodiment 2
(1) using graphite heater heating furnace body as cvd furnace, vacuumized, vacuum tightness reaches 2 * 10
-2pa;
(2) temperature in graphite heater process furnace is increased to 1200 ℃, temperature rise rate is 12 ℃ of per minutes;
(3) take hydrogen as carrier gas, by Bubbling method, trichloromethyl silane being brought into diameter is that in the graphite heater heating furnace chamber of 1.5 meters, carrier gas flux is 800ml/min, usings 99.9999% argon gas simultaneously as diluent gas, its flow is 800ml/min, and keeping heating furnace chamber internal pressure is 10
5pa, deposits 50 hours, cooling after, there is SiC coating in carbon materials surface.
Above are only single embodiment of the present invention, but design concept of the present invention is not limited to this, allly utilizes this design to carry out the change of unsubstantiality to the present invention, all should belong to the behavior of invading the scope of protection of the invention.In every case be the content that does not depart from technical solution of the present invention, any type of simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (5)
1. a method for carbon materials surface Direct precipitation SiC coating in graphite heater process furnace, its feature comprises the step of following order:
(1) using graphite heater heating furnace body as cvd furnace, vacuumized, vacuum tightness reaches 10
-1below Pa;
(2) temperature in graphite heater process furnace is increased to 1000～1200 ℃, temperature rise rate is 8～12 ℃ of per minutes;
(3) take hydrogen as carrier gas, by Bubbling method, trichloromethyl silane is brought in graphite heater heating furnace chamber, carrier gas flux regulates according to body of heater size, flow is 200～800ml/min, using argon gas as diluent gas simultaneously, its flow is 200～800ml/min, and keeping heating furnace chamber internal pressure is 3 * 10
3～10
5pa, deposits 20～50 hours, cooling after, there is SiC coating in carbon materials surface.
2. according to the method described in claims 1, it is characterized in that graphite heater process furnace can be the process furnace of smelting quartz glass, refine silicon single crystal, monocrystalline germanium, the process furnace of gallium arsenide, indium phosphide.
3. according to the method described in claims 1, it is characterized in that carbon materials parts comprise plumbago crucible, graphite field material, charcoal element lagging material.
4. according to the method described in claims 1, it is characterized in that it is more than 99.999% high-purity argon gas that diluent gas is selected purity.
5. according to the method described in claims 1, it is characterized in that the mol ratio of hydrogen and trichloromethyl silane is more than or equal to 10.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210268835.6A CN103570378A (en) | 2012-08-01 | 2012-08-01 | Method for direct deposition of silicon carbide (SiC) coating on carbon material surface in graphite heat-generating body heating furnace |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210268835.6A CN103570378A (en) | 2012-08-01 | 2012-08-01 | Method for direct deposition of silicon carbide (SiC) coating on carbon material surface in graphite heat-generating body heating furnace |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104177113A (en) * | 2014-08-08 | 2014-12-03 | 苏州宏久航空防热材料科技有限公司 | SiC bonded ceramic matrix composite material and preparation method thereof |
| CN104176949A (en) * | 2014-08-18 | 2014-12-03 | 苏州宏久航空防热材料科技有限公司 | Preparation method of high-infrared-absorption glass fiber |
| CN105439645A (en) * | 2015-12-25 | 2016-03-30 | 苏州宏久航空防热材料科技有限公司 | Composite coating for graphite thermal-field surface and preparation method thereof |
| CN105568368A (en) * | 2015-06-16 | 2016-05-11 | 杭州海纳半导体有限公司 | Thermal field and method for protecting thermal field component to reduce loss |
| CN105622174A (en) * | 2015-12-25 | 2016-06-01 | 苏州宏久航空防热材料科技有限公司 | Method for preparing SiC-Si-Si3N4 coating on surface of graphite heat field |
| CN105732044A (en) * | 2016-02-03 | 2016-07-06 | 深圳市商德先进陶瓷有限公司 | High-purity silicon carbide ceramic manufacturing method and ceramic base material |
| CN108892539A (en) * | 2018-07-27 | 2018-11-27 | 湖南省长宁炭素股份有限公司 | A kind of graphite material and preparation method thereof with SiC coating |
| CN117702076A (en) * | 2023-12-25 | 2024-03-15 | 湖南德智新材料有限公司 | Graphite base and preparation method thereof |
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| CN201915043U (en) * | 2011-01-10 | 2011-08-03 | 湖南金博复合材料科技有限公司 | Heating element made of carbon materials |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104177113A (en) * | 2014-08-08 | 2014-12-03 | 苏州宏久航空防热材料科技有限公司 | SiC bonded ceramic matrix composite material and preparation method thereof |
| CN104176949A (en) * | 2014-08-18 | 2014-12-03 | 苏州宏久航空防热材料科技有限公司 | Preparation method of high-infrared-absorption glass fiber |
| CN105568368A (en) * | 2015-06-16 | 2016-05-11 | 杭州海纳半导体有限公司 | Thermal field and method for protecting thermal field component to reduce loss |
| CN105439645A (en) * | 2015-12-25 | 2016-03-30 | 苏州宏久航空防热材料科技有限公司 | Composite coating for graphite thermal-field surface and preparation method thereof |
| CN105622174A (en) * | 2015-12-25 | 2016-06-01 | 苏州宏久航空防热材料科技有限公司 | Method for preparing SiC-Si-Si3N4 coating on surface of graphite heat field |
| CN105732044A (en) * | 2016-02-03 | 2016-07-06 | 深圳市商德先进陶瓷有限公司 | High-purity silicon carbide ceramic manufacturing method and ceramic base material |
| CN108892539A (en) * | 2018-07-27 | 2018-11-27 | 湖南省长宁炭素股份有限公司 | A kind of graphite material and preparation method thereof with SiC coating |
| CN117702076A (en) * | 2023-12-25 | 2024-03-15 | 湖南德智新材料有限公司 | Graphite base and preparation method thereof |
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Application publication date: 20140212 |