CN101659412A - Preparation method of single crystal silicon carbide special materials - Google Patents
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Abstract
The invention relates to a preparation method of signal crystal silicon carbide special materials, which is characterized in that the prepration method comprises the steps of selecting silicon carbideof not greater than 10 meshes as raw materials, and using purified water for carrying out washing with water on the raw materials till that the water is clear; then sequentially carrying out the washing with sodium hydroxide, the washing with sulfuric acid, the washing with aqua regia and the washing with hydrofluoric acid on the silicon carbide after the washing with the water, then further washing with the water till neutrality, drying, and then arranging the silicon carbide in a heating device for heating and calcination, thereby obtaining the signal crystal silicon carbide special materials. The method can effectively remove dust, oil, carbon, silicon, silicon dioxide, Cu, Fe, Al, a small amount of inert metals and free carbon and other impurities in the silicon carbide raw materials,and all the steps complement each other, thereby leading the purity of finished products of the signal crystal silicon carbide special materials to achieve 99.99% and achieving the using requirementson a third generation of semiconductor materials.
Description
Technical field
The present invention relates to the preparation method of a kind of production method of silicon carbide, particularly a kind of single crystal silicon carbide special materials.
Background technology
Carborundum crystals is the state-of-the-art technology product that present silicon carbide is used, and is called as third generation semiconductor material, is called semiconductor material with wide forbidden band, high temperature semiconductors material etc. again, is present international research focus.They have characteristics such as high heat conductance, high critical breakdown electric field and low-k, become the preferred material of the semiconducter device of high temperature resistant, high-power, high pressure resistant, anti-irradiation, carborundum crystals is made the substrate of various electronic devices and components, and the development prospect of manufacturing silicon carbide semiconductor is wide.Growth SiC monocrystalline desired raw material purity should be greater than 99.99%, and domestic growth SiC crystal raw material mainly relies on import, thereby research and industrialization production 4H-SiC and 6H-SiC silicon carbide monocrystal growth have great importance with superb sic raw material.
Growth SiC monocrystalline desired raw material purity should be greater than 99.99%.SiC abrasive material commonly used needs to carry out purification processes because of containing a lot of impurity before the use.Owing to be subjected to the restriction of production technique, the requirement that the purity of the back raw material of purifying does not still reach growing crystal.The high-purity alpha-SiC raw material obtains by CVD method or extremely pure Si and the C of sintered semiconductor, though its purity is higher, what bring simultaneously also is expensive paying, unsuitable industrialization production.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, and the preparation method of the single crystal silicon carbide special materials that a kind of technology is reasonable, workable, product purity is high is provided.
Technical problem to be solved by this invention is to realize by following technical scheme.The present invention is a kind of preparation method of single crystal silicon carbide special materials, is characterized in, its step is as follows:
(1) choosing particle diameter, to be not more than 10 purpose silicon carbide be raw material, with pure water raw material washed, and it is limpid to be washed till water;
(2) silicon carbide that will wash is directly put into capacity with cover, place 8-12Kg silicon carbide in every 10L volumetrical capacity with cover, in capacity with cover, add pure water then and cover silicon carbide, slowly add purity again greater than 98% flaky sodium hydrate, stir, make the concentration of sodium hydroxide solution in the capacity with cover reach 8%-10%; Capacity with cover is put into water-bath, 80 ℃-90 ℃ water-bath 6-10 hour, stirred 1-2 time in every 1-3 hour; Be washed to neutrality with the silicon carbide of pure water after with pure water again with water-bath;
(3) silicon carbide after will washing is put into capacity with cover once more, places 8-12Kg silicon carbide in every 10L volumetrical capacity with cover, and the sulphuric acid soln that adds concentration then and be 10-20% in capacity with cover covers silicon carbide, stirs; Then capacity with cover is put into water-bath, 80 ℃-90 ℃ water-bath 6-10 hour, stirred 1-2 time in every 1-3 hour; Be washed to neutrality with the silicon carbide of pure water after again with water-bath;
(4) silicon carbide after will washing is put into capacity with cover once more, place 8-12Kg silicon carbide in every 10L volumetrical capacity with cover, in capacity with cover, add chloroazotic acid in the ratio that adds 300-500ml in every 8-12Kg silicon carbide then, add pure water again and cover silicon carbide, stir; Capacity with cover is put into water-bath, 80 ℃-90 ℃ water-bath 6-10 hour, stirred 1-2 time in every 1-3 hour; Be washed to neutrality with the silicon carbide of pure water after again with water-bath;
(5) silicon carbide after will washing is put into capacity with cover once more, place 8-12Kg silicon carbide in every 10L volumetrical capacity with cover, adding concentration in the ratio that adds 300-500ml in every 8-12Kg silicon carbide in capacity with cover then is the hydrofluoric acid of 35%-45%, add pure water again and cover silicon carbide, stir; Capacity with cover is put into water-bath, 80 ℃-90 ℃ water-bath 6-10 hour, stirred 1-2 time in every 1-3 hour; Be washed to neutrality with the silicon carbide of distilled water after again with water-bath;
(6) the silicon carbide drying after will washing places silicon carbide heating unit to carry out 1300 ℃ of-1800 ℃ of heating and calcinings then, charges into an amount of oxygen in heating and calcining in heating unit, promptly gets single crystal silicon carbide special materials.
In the above-described technical scheme: optimized technical scheme is:
1, in step (2): place 10Kg silicon carbide in every 10L volumetrical capacity with cover; Concentration of sodium hydroxide solution in the capacity with cover is 9%.
2, in step (3): place 10Kg silicon carbide in every 10L volumetrical capacity with cover, the concentration of the sulphuric acid soln that is added is 15%.
3, in step (4): place 10Kg silicon carbide in every 10L volumetrical capacity with cover, chloroazotic acid adds in capacity with cover in the ratio that adds 40ml in every 10Kg silicon carbide.
4, in step (5): place 10Kg silicon carbide in every 10L volumetrical capacity with cover, adding concentration in the ratio that adds 400ml in every 10Kg silicon carbide in capacity with cover then is 40% hydrofluoric acid.
5, in step (2), (3), (4) or (5): capacity with cover is put into water-bath, and 85 ℃ of water-baths 8 hours stirred 1 time in per 1 hour.
6, in step (6), the temperature that places heating unit to carry out heating and calcining in silicon carbide is 1600 ℃-1700 ℃.
7, in step (6), the time of heating and calcining can decide according to practical situation, is preferably 3-5 minute.
In the technical solution of the present invention: by the washing of step (1), its purpose is removed dust and a part of oil and the carbon in the sic raw material, the partial impurities in the preliminary flush away raw material; The alkali cleaning of step (2), its main purpose are for removing silicon and the silicon-dioxide impurity in the sic raw material; The pickling of step (3), its main purpose be for destroying the protective membrane that silicon carbide makes the reaction passivation, makes the ensuing acid-respons that adds can be cmpletely; The chloroazotic acid of step (4) is washed, and its main purpose is to remove Cu, Fe, Al and a small amount of inert metal that contains in the sic raw material; The white picking of step (5), its main purpose are the free silicas of removing in the sic raw material as much as possible; The heating and calcining of step (6), its main purpose are the uncombined carbons of further removing in the sic raw material.Each step complements each other, and can remove the various impurity in the sic raw material effectively, makes the purity of finished product single crystal silicon carbide special materials reach 99.99%, reaches the service requirements of third generation semiconductor material.
Compared with prior art, its concrete advantage is further described below:
1, the inventive method can be removed the carbon in the sic raw material effectively.
In the smelting procedure of the preparation method's of single crystal silicon carbide special materials of the present invention sic raw material; participate in reaction and react incomplete refinery coke with the form of carbon granule attached to the silicon-carbide particle surface; along with carrying out gradually of pulverizing process; carbon granule comes off from the silicon-carbide particle surface basically; exist with the uncombined carbon form, therefore uncombined carbon need be removed.Traditional de-carbon technology has two kinds of mechanical de-carbon and manual de-carbons, carbon content can be reduced in 0.2% when carbon content is in 0.5% in the raw material; When the carbon content in the raw material greater than 0.5% the time, the de-carbon effect is on the low side.The single crystal silicon carbide special materials of the present invention's preparation requires very high to carbon content, be difficult to reach by traditional de-carbon technology.By discovering of contriver, can remove the incomplete carbon of dereaction effectively by the mode of high-temperature calcination, when high temperature by to the slow aerating oxygen of feeding device, row when guaranteeing reaction effective.
2, the inventive method can be removed silicon and the silicon-dioxide impurity in the sic raw material effectively.
In the smelting procedure of sic raw material,, cause carborundum content on the low side because reaction is insufficient or silicon carbide is decomposed to form silicon and silicon-dioxide impurity under hot conditions.The technology of the present invention realizes the removal of silicon and silicon-dioxide impurity effectively by the control to temperature and naoh concentration.Stir 1 during water-bath and can guarantee that whole raw materials participate in the even of reaction and temperature, and the silicon carbide overall quality is stable.
3, the inventive method can be removed the metallic impurity in the sic raw material effectively.
In the smelting of sic raw material, pulverizing process, all can sneak into metallic impurity such as Cu, Fe, Al in the sic raw material.Metallic impurity are bigger to the harm of silicon carbide.
By control, realize the removal of metallic impurity in the inventive method to temperature and acid.Be the optimal reaction temperature of acid more than 80 ℃, reaction is thermopositive reaction, and stirring can guarantee that whole raw materials participate in the even of reaction and temperature, and the sic raw material overall quality is stable.
4, the present invention's another purpose of adopting sodium hydroxide and acid to clean is an acid-base neutralisation of being convenient to waste water because the input amount of sodium hydroxide and acid is suitable substantially in the technology of the present invention, neutralization after the simple process reusable edible economize on resources and production cost.
Embodiment
Below further describe concrete technical scheme of the present invention,, and do not constitute restriction its right so that those skilled in the art understands the present invention further.
Embodiment 1.A kind of preparation method of single crystal silicon carbide special materials, its step is as follows:
(1) choosing particle diameter, to be not more than 10 purpose silicon carbide be raw material, with pure water raw material washed, and it is limpid to be washed till water;
(2) silicon carbide that will wash is directly put into capacity with cover, place 8-Kg silicon carbide in every 10L volumetrical capacity with cover, in capacity with cover, add pure water then and cover silicon carbide, slowly add purity again greater than 98% flaky sodium hydrate, stir, make the concentration of sodium hydroxide solution in the capacity with cover reach 8%; Capacity with cover is put into water-bath, and 80 ℃ of water-baths 6 hours stirred 2 times in per 1 hour; Be washed to neutrality with the silicon carbide of pure water after with pure water again with water-bath;
(3) silicon carbide after will washing is put into capacity with cover once more, places 8Kg silicon carbide in every 10L volumetrical capacity with cover, adds concentration then and is 10% sulphuric acid soln in capacity with cover and cover silicon carbide, stirs; Then capacity with cover is put into water-bath, 80 ℃ of water-baths 6 hours stirred 2 times in per 1 hour; Be washed to neutrality with the silicon carbide of pure water after again with water-bath;
(4) silicon carbide after will washing is put into capacity with cover once more, places 8Kg silicon carbide in every 10L volumetrical capacity with cover, adds chloroazotic acid in the ratio that adds 300ml in every 8Kg silicon carbide in capacity with cover then, adds pure water again and covers silicon carbide, stirs; Capacity with cover is put into water-bath, and 80 ℃ of water-baths 6 hours stirred 2 times in per 1 hour; Be washed to neutrality with the silicon carbide of pure water after again with water-bath;
(5) silicon carbide after will washing is put into capacity with cover once more, place 8Kg silicon carbide in every 10L volumetrical capacity with cover, adding concentration in the ratio that adds 300ml in every 8Kg silicon carbide in capacity with cover then is 35% hydrofluoric acid, adds pure water again and covers silicon carbide, stirring; Capacity with cover is put into water-bath, and 80 ℃ of water-baths 6 hours stirred 2 times in per 1 hour; Be washed to neutrality with the silicon carbide of distilled water after again with water-bath;
(6) the silicon carbide drying after will washing places silicon carbide heating unit to carry out 1300 ℃ of heating and calcinings then, charges into an amount of oxygen in heating and calcining in heating unit, promptly gets single crystal silicon carbide special materials.
Embodiment 2.A kind of preparation method of single crystal silicon carbide special materials, its step is as follows:
(1) choosing particle diameter, to be not more than 10 purpose silicon carbide be raw material, with pure water raw material washed, and it is limpid to be washed till water;
(2) silicon carbide that will wash is directly put into capacity with cover, place 12Kg silicon carbide in every 10L volumetrical capacity with cover, in capacity with cover, add pure water then and cover silicon carbide, slowly add purity again greater than 98% flaky sodium hydrate, stir, make the concentration of sodium hydroxide solution in the capacity with cover reach 10%; Capacity with cover is put into water-bath, and 90 ℃ of water-baths 10 hours stirred 1 time in per 3 hours; Be washed to neutrality with the silicon carbide of pure water after with pure water again with water-bath;
(3) silicon carbide after will washing is put into capacity with cover once more, places 12Kg silicon carbide in every 10L volumetrical capacity with cover, adds concentration then and is 20% sulphuric acid soln in capacity with cover and cover silicon carbide, stirs; Then capacity with cover is put into water-bath, 90 ℃ of water-baths 10 hours stirred 1 time in per 3 hours; Be washed to neutrality with the silicon carbide of pure water after again with water-bath;
(4) silicon carbide after will washing is put into capacity with cover once more, place 12Kg silicon carbide in every 10L volumetrical capacity with cover, in capacity with cover, add chloroazotic acid in the ratio that adds 300-500ml in every 12Kg silicon carbide then, add pure water again and cover silicon carbide, stir; Capacity with cover is put into water-bath, and 90 ℃ of water-baths 10 hours stirred 1 time in per 3 hours; Be washed to neutrality with the silicon carbide of pure water after again with water-bath;
(5) silicon carbide after will washing is put into capacity with cover once more, place 12Kg silicon carbide in every 10L volumetrical capacity with cover, adding concentration in the ratio that adds 500ml in every 12Kg silicon carbide in capacity with cover then is 45% hydrofluoric acid, adds pure water again and covers silicon carbide, stirring; Capacity with cover is put into water-bath, and 90 ℃ of water-baths 10 hours stirred 1 time in per 3 hours; Be washed to neutrality with the silicon carbide of distilled water after again with water-bath;
(6) the silicon carbide drying after will washing places silicon carbide heating unit to carry out 1800 ℃ of heating and calcinings then, charges into an amount of oxygen in heating and calcining in heating unit, and heating and calcining promptly got single crystal silicon carbide special materials in 3 minutes.
Embodiment 3.A kind of preparation method of single crystal silicon carbide special materials, its step is as follows:
(1) choosing particle diameter, to be not more than 10 purpose silicon carbide be raw material, with pure water raw material washed, and it is limpid to be washed till water;
(2) silicon carbide that will wash is directly put into capacity with cover, place 10Kg silicon carbide in every 10L volumetrical capacity with cover, in capacity with cover, add pure water then and cover silicon carbide, slowly add purity again greater than 98% flaky sodium hydrate, stir, make the concentration of sodium hydroxide solution in the capacity with cover reach 9%; Capacity with cover is put into water-bath, and 85 ℃ of water-baths 8 hours stirred 1 time in per 1 hour; Be washed to neutrality with the silicon carbide of pure water after with pure water again with water-bath;
(3) silicon carbide after will washing is put into capacity with cover once more, places 10Kg silicon carbide in every 10L volumetrical capacity with cover, adds concentration then and is 15% sulphuric acid soln in capacity with cover and cover silicon carbide, stirs; Then capacity with cover is put into water-bath, 85 ℃ of water-baths 8 hours stirred 1 time in per 1 hour; Be washed to neutrality with the silicon carbide of pure water after again with water-bath;
(4) silicon carbide after will washing is put into capacity with cover once more, places 10Kg silicon carbide in every 10L volumetrical capacity with cover, adds chloroazotic acid in the ratio that adds 400ml in every 10Kg silicon carbide in capacity with cover then, adds pure water again and covers silicon carbide, stirs; Capacity with cover is put into water-bath, and 85 ℃ of water-baths 8 hours stirred 1 time in per 1 hour; Be washed to neutrality with the silicon carbide of pure water after again with water-bath;
(5) silicon carbide after will washing is put into capacity with cover once more, place 10Kg silicon carbide in every 10L volumetrical capacity with cover, adding concentration in the ratio that adds 400ml in every 10Kg silicon carbide in capacity with cover then is 40% hydrofluoric acid, adds pure water again and covers silicon carbide, stirring; Capacity with cover is put into water-bath, and 85 ℃ of water-baths 8 hours stirred 1 time in per 1 hour; Be washed to neutrality with the silicon carbide of distilled water after again with water-bath;
(6) the silicon carbide drying after will washing places silicon carbide heating unit to carry out 1600 ℃ of heating and calcinings then, charges into an amount of oxygen in heating and calcining in heating unit, and heating and calcining promptly got single crystal silicon carbide special materials in 5 minutes.
Embodiment 4.A kind of preparation method of single crystal silicon carbide special materials, its step is as follows:
(1) choosing particle diameter, to be not more than 10 purpose silicon carbide be raw material, with pure water raw material washed, and it is limpid to be washed till water;
(2) silicon carbide that will wash is directly put into capacity with cover, place 9Kg silicon carbide in every 10L volumetrical capacity with cover, in capacity with cover, add pure water then and cover silicon carbide, slowly add purity again greater than 98% flaky sodium hydrate, stir, make the concentration of sodium hydroxide solution in the capacity with cover reach 8.5%; Capacity with cover is put into water-bath, and 82 ℃ of water-baths 7 hours stirred 1 time in per 2 hours; Be washed to neutrality with the silicon carbide of pure water after with pure water again with water-bath;
(3) silicon carbide after will washing is put into capacity with cover once more, places 9Kg silicon carbide in every 10L volumetrical capacity with cover, adds concentration then and is 12% sulphuric acid soln in capacity with cover and cover silicon carbide, stirs; Then capacity with cover is put into water-bath, 82 ℃ of water-baths 7 hours stirred 1 time in per 2 hours; Be washed to neutrality with the silicon carbide of pure water after again with water-bath;
(4) silicon carbide after will washing is put into capacity with cover once more, places 9Kg silicon carbide in every 10L volumetrical capacity with cover, adds chloroazotic acid in the ratio that adds 350ml in every 9Kg silicon carbide in capacity with cover then, adds pure water again and covers silicon carbide, stirs; Capacity with cover is put into water-bath, and 82 ℃ of water-baths 7 hours stirred 1 time in per 2 hours; Be washed to neutrality with the silicon carbide of pure water after again with water-bath;
(5) silicon carbide after will washing is put into capacity with cover once more, place 9Kg silicon carbide in every 10L volumetrical capacity with cover, adding concentration in the ratio that adds 350ml in every 9Kg silicon carbide in capacity with cover then is 38% hydrofluoric acid, adds pure water again and covers silicon carbide, stirring; Capacity with cover is put into water-bath, and 82 ℃ of water-baths 7 hours stirred 1 time in per 2 hours; Be washed to neutrality with the silicon carbide of distilled water after again with water-bath;
(6) the silicon carbide drying after will washing places silicon carbide heating unit to carry out 1700 ℃ of heating and calcinings then, charges into an amount of oxygen in heating and calcining in heating unit, and heating and calcining promptly got single crystal silicon carbide special materials in 4 minutes.
Embodiment 5.A kind of preparation method of single crystal silicon carbide special materials, its step is as follows:
(1) choosing particle diameter, to be not more than 10 purpose silicon carbide be raw material, with pure water raw material washed, and it is limpid to be washed till water;
(2) silicon carbide that will wash is directly put into capacity with cover, place 11Kg silicon carbide in every 10L volumetrical capacity with cover, in capacity with cover, add pure water then and cover silicon carbide, slowly add purity again greater than 98% flaky sodium hydrate, stir, make the concentration of sodium hydroxide solution in the capacity with cover reach 9.5%; Capacity with cover is put into water-bath, and 88 ℃ of water-baths 9 hours stirred 2 times in per 3 hours; Be washed to neutrality with the silicon carbide of pure water after with pure water again with water-bath;
(3) silicon carbide after will washing is put into capacity with cover once more, places 11Kg silicon carbide in every 10L volumetrical capacity with cover, adds concentration then and is 18% sulphuric acid soln in capacity with cover and cover silicon carbide, stirs; Then capacity with cover is put into water-bath, 88 ℃ of water-baths 9 hours stirred 2 times in per 3 hours; Be washed to neutrality with the silicon carbide of pure water after again with water-bath;
(4) silicon carbide after will washing is put into capacity with cover once more, places 11Kg silicon carbide in every 10L volumetrical capacity with cover, adds chloroazotic acid in the ratio that adds 450ml in every 11Kg silicon carbide in capacity with cover then, adds pure water again and covers silicon carbide, stirs; Capacity with cover is put into water-bath, and 88 ℃ of water-baths 9 hours stirred 2 times in per 3 hours; Be washed to neutrality with the silicon carbide of pure water after again with water-bath;
(5) silicon carbide after will washing is put into capacity with cover once more, place 11Kg silicon carbide in every 10L volumetrical capacity with cover, adding concentration in the ratio that adds 450ml in every 11Kg silicon carbide in capacity with cover then is 42% hydrofluoric acid, adds pure water again and covers silicon carbide, stirring; Capacity with cover is put into water-bath, and 88 ℃ of water-baths 9 hours stirred 2 times in per 3 hours; Be washed to neutrality with the silicon carbide of distilled water after again with water-bath;
(6) the silicon carbide drying after will washing places silicon carbide heating unit to carry out 1500 ℃ of heating and calcinings then, charges into an amount of oxygen in heating and calcining in heating unit, and heating and calcining promptly got single crystal silicon carbide special materials in 8 minutes.
Claims (8)
1, a kind of preparation method of single crystal silicon carbide special materials is characterized in that, its step is as follows:
(1) choosing particle diameter, to be not more than 10 purpose silicon carbide be raw material, with pure water raw material washed, and it is limpid to be washed till water;
(2) silicon carbide that will wash is directly put into capacity with cover, place 8-12Kg silicon carbide in every 10L volumetrical capacity with cover, in capacity with cover, add pure water then and cover silicon carbide, slowly add purity again greater than 98% flaky sodium hydrate, stir, make the concentration of sodium hydroxide solution in the capacity with cover reach 8%-10%; Capacity with cover is put into water-bath, 80 ℃-90 ℃ water-bath 6-10 hour, stirred 1-2 time in every 1-3 hour; Again the silicon carbide behind the water-bath is washed to neutrality with pure water;
(3) silicon carbide after will washing is put into capacity with cover once more, places 8-12Kg silicon carbide in every 10L volumetrical capacity with cover, and the sulphuric acid soln that adds concentration then and be 10-20% in capacity with cover covers silicon carbide, stirs; Then capacity with cover is put into water-bath, 80 ℃-90 ℃ water-bath 6-10 hour, stirred 1-2 time in every 1-3 hour; Be washed to neutrality with the silicon carbide of pure water after again with water-bath;
(4) silicon carbide after will washing is put into capacity with cover once more, place 8-12Kg silicon carbide in every 10L volumetrical capacity with cover, in capacity with cover, add chloroazotic acid in the ratio that adds 300-500ml in every 8-12Kg silicon carbide then, add pure water again and cover silicon carbide, stir; Capacity with cover is put into water-bath, 80 ℃-90 ℃ water-bath 6-10 hour, stirred 1-2 time in every 1-3 hour; Be washed to neutrality with the silicon carbide of pure water after again with water-bath;
(5) silicon carbide after will washing is put into capacity with cover once more, place 8-12Kg silicon carbide in every 10L volumetrical capacity with cover, adding concentration in the ratio that adds 300-500ml in every 8-12Kg silicon carbide in capacity with cover then is the hydrofluoric acid of 35%-45%, add pure water again and cover silicon carbide, stir; Capacity with cover is put into water-bath, 80 ℃-90 ℃ water-bath 6-10 hour, stirred 1-2 time in every 1-3 hour; Be washed to neutrality with the silicon carbide of distilled water after again with water-bath;
(6) the silicon carbide drying after will washing places silicon carbide heating unit to carry out 1300 ℃ of-1800 ℃ of heating and calcinings then, charges into an amount of oxygen in heating and calcining in heating unit, promptly gets single crystal silicon carbide special materials.
2, silicon carbide micro-powder chemical purification method according to claim 1 is characterized in that, in step (2): place 10Kg silicon carbide in every 10L volumetrical capacity with cover; Concentration of sodium hydroxide solution in the capacity with cover is 9%.
3, silicon carbide micro-powder chemical purification method according to claim 1 is characterized in that, in step (3): place 10Kg silicon carbide in every 10L volumetrical capacity with cover, the concentration of the sulphuric acid soln that is added is 15%.
4, silicon carbide micro-powder chemical purification method according to claim 1 is characterized in that, in step (4): place 10Kg silicon carbide in every 10L volumetrical capacity with cover, chloroazotic acid adds in capacity with cover in the ratio that adds 40ml in every 10Kg silicon carbide.
5, silicon carbide micro-powder chemical purification method according to claim 1, it is characterized in that, in step (5): place 10Kg silicon carbide in every 10L volumetrical capacity with cover, adding concentration in the ratio that adds 400ml in every 10Kg silicon carbide in capacity with cover then is 40% hydrofluoric acid.
6, silicon carbide micro-powder chemical purification method according to claim 1 is characterized in that, in step (2), (3), (4) or (5): capacity with cover is put into water-bath, and 85 ℃ of water-baths 8 hours stirred 1 time in per 1 hour.
7, silicon carbide micro-powder chemical purification method according to claim 1 is characterized in that, in step (6), the temperature that places heating unit to carry out heating and calcining in silicon carbide is 1600 ℃-1700 ℃.
8, silicon carbide micro-powder chemical purification method according to claim 1 is characterized in that, in step (6), the time of heating and calcining is 3-5 minute.
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| US20160108553A1 (en) * | 2011-09-21 | 2016-04-21 | Sumitomo Electric Industries, Ltd. | Silicon carbide substrate and method of manufacturing the same |
| CN105948055A (en) * | 2016-05-30 | 2016-09-21 | 山田研磨材料有限公司 | Purification method of high-purity silicon carbide micro powder for semiconductor |
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