CN103570377B - Method for preparation of silicon carbide (SiC) coating on carbon material surface in graphite heat-generating body heating furnace - Google Patents
Method for preparation of silicon carbide (SiC) coating on carbon material surface in graphite heat-generating body heating furnace Download PDFInfo
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- CN103570377B CN103570377B CN201210268834.1A CN201210268834A CN103570377B CN 103570377 B CN103570377 B CN 103570377B CN 201210268834 A CN201210268834 A CN 201210268834A CN 103570377 B CN103570377 B CN 103570377B
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Abstract
The invention provides a method for preparation 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) taking an appropriate amount of carbon felt and SiO2 powder in a molar ratio of 1:1; (2) putting the carbon felt and the SiO2 powder into hydrochloric acid for pickling, after pickling, using deionized water for water washing, after water washing, coating the SiO2 powder with the carbon felt, putting in an oven of 70 ~ 90 DEG C for processing; (3) putting the carbon felt coating the SiO2 powder into the graphite heat-generating body heating furnace, closing the graphite heat-generating body heating furnace; (4) raising the temperature of the heating furnace to 500 ~ 700 DEG C, pumping the air pressure to below 10<-2>Pa, maintaining for 2 ~ 3 hours; (5) raising the temperature of the heating furnace to 1450 ~ 1600 DEG C, performing heat insulation for 2 ~ 6 hours, stopping heat insulation, and cooling to obtain the silicon carbide (SiC) coating on the carbon material surface in the graphite heat-generating body heating furnace. The method is relatively simple in process, easy in operation and good in repeatability, metallurgical bonding of the coating and a substrate is achieved, and the coating binding force is strong.
Description
Technical field
The present invention relates to a kind of method preparing SiC coating, particularly relate to carbon materials surface in a kind of graphite heater process furnace and prepare the method for SiC coating.
Background technology
Graphite has excellent conduction, heat conductivility, and hot strength is good, and in special industrial stove, 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 material such as gallium arsenide, indium phosphide selects special graphite to make heating element, and some special industrial furnaces and experimental furnace charcoal cloth or Graphite cloth make heating element.Except graphite heater, plumbago crucible, the carbon materialses such as charcoal element lagging material use in a large number, in wafer growth stove especially in the semiconductor industry in special industrial stove.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 reduced.
Owing to usually will reach the working temperature of more than 1500 DEG C in wafer growth stove, the carbon atom in carbon materials can continue volatilization in High Temperature Furnaces Heating Apparatus, thus brings two negative impacts: one is that carbon atom diffuses into wafer, causes wafer quality to decline; Two is that 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 becoming industry development, an urgent demand extends the graphite field material military service time.Carrying out coating process to carbon materials in wafer growth stove is solve carbon atom volatilization, 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 DEG C, shows excellent anti-oxidant, anti-yaw damper feature.SiC is applied the coating to the carbon materialses such as the graphite heater in semi-conductor industry in wafer growth stove, be expected to wafer quality to improve 3 ~ 5 times, the life-span of graphite nuclei parts improves 6 ~ 10 times, and Business Economic Benefit can significantly promote.
Be prepared in the surperficial method preparing coat of silicon carbide of carbon materials at present to mainly contain: chemical Vapor deposition process, plasma spraying method etc.Current conventional chemical vapor sedimentation is a kind of technique of high cost, and operating process more complicated, need plant and instrument more.Although and plasma spraying method good manufacturability, its coatingsurface has certain porosity, and carbon diffusion coefficient is uprised, thus loses protected effect.Complex process, poor controllability, cost is high.In graphite heater process furnace, carbon materials parts are many, and complex-shaped, prepare the method for coat of silicon carbide according to tradition, are easy to cause cost to increase considerably.
Summary of the invention
Problem to be solved by this invention proposes carbon materials surface in a kind of graphite heater process furnace to prepare the method for SiC coating.
Operating process:
(1) appropriate carbon felt and SiO is got according to the mol ratio of 1: 1
2powder, in carbon felt, carbon content is more than or equal to 99.9%, SiO
2powder purity is more than or equal to 99.999%, SiO
2powder Particle Size is 200 ~ 500um;
(2) by carbon felt and SiO
2powder put into concentration be 3% ~ 6% hydrochloric acid carry out pickling, after pickling with deionized water washing, after washing by carbon felt SiO
2powder is coated, is placed in the baking oven of 70 ~ 90 DEG C and processes 2 ~ 5 hours;
(3) by coated Si O
2graphite heater process furnace put into by the carbon felt of powder, airtight process furnace;
(4) heating in-furnace temperature is increased to 500 ~ 700 DEG C, air pressure is evacuated to 10
-2below Pa, temperature rise rate is 3 ~ 5 DEG C of per minutes, keeps 2 ~ 3 hours;
(5) furnace temp is increased to 1450 ~ 1600 DEG C, temperature rise rate is 4 ~ 8 DEG C of per minutes, is incubated 2 ~ 6 hours, and stop insulation, after cooling, in process furnace, carbon materials surface has coat of silicon carbide.
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.
In silicon wafer stove, carbon materials comprises plumbago crucible, graphite field material, charcoal element lagging material.
In the present invention, major advantage is: (1) technological process is relatively simple, easy to operate, reproducible; (2) coating preparation process does not need specific equipment, and cost is low; (3) coating and matrix reach metallurgical binding, coating binding force is strong.
Embodiment
Below in conjunction with specific embodiment, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims and limited.
Embodiment 1
(1) appropriate carbon felt and SiO is got according to the mol ratio of 1: 1
2powder, in carbon felt, carbon content is 99.9%, SiO
2powder purity is 99.999%, SiO
2powder Particle Size is 500um;
(2) by carbon felt and SiO
2powder put into concentration be 5% hydrochloric acid carry out pickling, after pickling with deionized water washing, after washing by carbon felt SiO
2powder is coated, is placed in the baking oven of 80 DEG C and processes 3 hours;
(3) by coated Si O
2graphite heater process furnace put into by the carbon felt of powder, airtight process furnace;
(4) heating in-furnace temperature is increased to 600 DEG C, air pressure is evacuated to 5 × 10
-3pa, temperature rise rate is 4 DEG C of per minutes, keeps 2 hours;
(5) furnace temp is increased to 1500 DEG C, temperature rise rate is 5 DEG C of per minutes, is incubated 4 hours, and stop insulation, after cooling, in process furnace, carbon materials surface has coat of silicon carbide.
Embodiment 2
(1) appropriate carbon felt and SiO is got according to the mol ratio of 1: 1
2powder, in carbon felt, carbon content is 99.99%, SiO
2powder purity is 99.999%, SiO
2powder Particle Size is 400um;
(2) by carbon felt and SiO
2powder put into concentration be 4% hydrochloric acid carry out pickling, after pickling with deionized water washing, after washing by carbon felt SiO
2powder is coated, is placed in the baking oven of 90 DEG C and processes 4 hours;
(3) by coated Si O
2graphite heater process furnace put into by the carbon felt of powder, airtight process furnace;
(4) heating in-furnace temperature is increased to 700 DEG C, air pressure is evacuated to 3 × 10
-3pa, temperature rise rate is 5 DEG C of per minutes, keeps 3 hours;
(5) furnace temp is increased to 1550 DEG C, temperature rise rate is 8 DEG C of per minutes, is incubated 5 hours, and stop insulation, after cooling, in process furnace, carbon materials surface has coat of silicon carbide.
Above are only single embodiment of the present invention, but design concept of the present invention is not limited thereto, all changes utilizing this design the present invention to be carried out to unsubstantiality, all should belong to the behavior of invading the scope of protection of the invention.In every case be the content not departing from technical solution of the present invention, any type of simple modification, equivalent variations and the remodeling done above embodiment according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (3)
1. in graphite heater process furnace, a method for SiC coating is prepared on carbon materials surface, and its feature comprises the step of following order:
(1) appropriate carbon felt and SiO is got according to the mol ratio of 1: 1
2powder, in carbon felt, carbon content is more than or equal to 99.9%, SiO
2powder purity is more than or equal to 99.999%, SiO
2powder Particle Size is 200 ~ 500 μm;
(2) by carbon felt and SiO
2powder put into concentration be 3% ~ 6% hydrochloric acid carry out pickling, after pickling with deionized water washing, after washing by carbon felt SiO
2powder is coated, is placed in the baking oven of 70 ~ 90 DEG C and processes 2 ~ 5 hours;
(3) by coated Si O
2graphite heater process furnace put into by the carbon felt of powder, airtight process furnace;
(4) heating in-furnace temperature is increased to 500 ~ 700 DEG C, air pressure is evacuated to 10
-2below Pa, temperature rise rate is 3 ~ 5 DEG C of per minutes, keeps 2 ~ 3 hours;
(5) furnace temp is increased to 1450 ~ 1600 DEG C, temperature rise rate is 4 ~ 8 DEG C of per minutes, is incubated 2 ~ 6 hours, and stop insulation, after cooling, in process furnace, carbon materials surface has coat of silicon carbide.
2. the method according to claims 1, is characterized in that graphite heater process furnace is the process furnace of smelting quartz glass, refines silicon single crystal, monocrystalline germanium, the process furnace of gallium arsenide, indium phosphide.
3. the method according to claims 1, is characterized in that carbon materials parts comprise plumbago crucible, graphite field material, charcoal element lagging material.
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| CN201210268834.1A CN103570377B (en) | 2012-08-01 | 2012-08-01 | Method for preparation of silicon carbide (SiC) coating on carbon material surface in graphite heat-generating body heating furnace |
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| CN105503265B (en) * | 2015-12-25 | 2017-11-03 | 苏州宏久航空防热材料科技有限公司 | A kind of method that graphite field surface prepares SiC coatings in graphite heater furnace |
| CN107522487B (en) * | 2017-07-07 | 2020-02-18 | 中国人民解放军国防科学技术大学 | Graphite material with SiC doped layer and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101003942A (en) * | 2006-12-29 | 2007-07-25 | 哈尔滨工业大学 | Method for preparing coat of silicon carbide on surface of carbon fiber |
| CN102167623A (en) * | 2011-01-10 | 2011-08-31 | 廖寄乔 | Carbon material oxidation resistant coating and preparation method thereof |
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| JP3042297B2 (en) * | 1994-04-12 | 2000-05-15 | 王子製紙株式会社 | Method for producing silicon carbide material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101003942A (en) * | 2006-12-29 | 2007-07-25 | 哈尔滨工业大学 | Method for preparing coat of silicon carbide on surface of carbon fiber |
| CN102167623A (en) * | 2011-01-10 | 2011-08-31 | 廖寄乔 | Carbon material oxidation resistant coating and preparation method thereof |
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