CN103058192A - Preparation method of silicon carbide micro-powder used in silicon carbide crystal growth - Google Patents
Preparation method of silicon carbide micro-powder used in silicon carbide crystal growth Download PDFInfo
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- CN103058192A CN103058192A CN2013100039740A CN201310003974A CN103058192A CN 103058192 A CN103058192 A CN 103058192A CN 2013100039740 A CN2013100039740 A CN 2013100039740A CN 201310003974 A CN201310003974 A CN 201310003974A CN 103058192 A CN103058192 A CN 103058192A
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- silicon carbide
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- carbide micro
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 33
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000000843 powder Substances 0.000 title claims abstract description 19
- 239000013078 crystal Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 42
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 32
- 235000013312 flour Nutrition 0.000 claims description 16
- 239000000377 silicon dioxide Substances 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 15
- 239000000428 dust Substances 0.000 claims description 15
- 229910052710 silicon Inorganic materials 0.000 claims description 13
- 239000010703 silicon Substances 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 9
- 230000002194 synthesizing effect Effects 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- 239000011863 silicon-based powder Substances 0.000 abstract 1
- 239000003595 mist Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000013467 fragmentation Methods 0.000 description 3
- 238000006062 fragmentation reaction Methods 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 240000003936 Plumbago auriculata Species 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention relates to a preparation method of silicon carbide micro-powder used in silicon carbide crystal growth. The method comprises the steps that: carbon powder and silicon powder are uniformly mixed, such that a mixture is obtained; and the mixture is added into a heating chamber, and is heated by using microwaves, such that the silicon carbide micro-powder used in silicon carbide crystal growth is obtained. According to the invention, microwave heating is adopted, and heating is uniform. The synthesized silicon carbide particles have good particle size homogeneity. The obtained product does not need to be crushed by using a traditional ball mill, such that secondary pollution is prevented, and product purity is ensured. Also, a single-time synthesizing amount is high, and efficiency is high.
Description
Technical field
The present invention relates to a kind of preparation method of silicon carbide micro-powder, relate in particular to a kind of preparation method of the silicon carbide micro-powder for growing silicon carbice crystals.
Background technology
Existing growing silicon carbice crystals adopts behind the induction heating sintering broken more with high purity micropowder, for example, and after silica flour and carbon dust mixed, be positioned in the plumbago crucible, synthesize by induction heating, synthesis temperature reaches more than 2000 ℃, carbon dust and the synthetic silicon carbide micro-powder of silica flour reaction.Adopt the synthetic silicon carbide micro-powder of this method to sinter block into, need to carry out again fragmentation, caused the secondary pollution of carborundum powder, synthetic micro mist globule size after fragmentation differs, and needs through screening, causes contamination and waste.And the single resultant quantity that induction heating synthesizes is less, and difficulty satisfies the scale operation requirement.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of the silicon carbide micro-powder for growing silicon carbice crystals, reduces the raw material building-up process and pollutes, and the single resultant quantity is large, and the synthesizing silicon carbide micro powder granule is even simultaneously, need not fragmentation.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of preparation method of the silicon carbide micro-powder for growing silicon carbice crystals may further comprise the steps:
(1) with the even mixing of carbon dust and silica flour, obtains mixture;
(2) described mixture is joined in the heating chamber, by microwave described mixture is heated, get final product to get described silicon carbide micro-powder for growing silicon carbice crystals.
The invention has the beneficial effects as follows: the present invention adopts microwave heating, homogeneous heating, and synthetic silicon-carbide particle uniform particle diameter is good, the product that obtains does not need to use traditional ball mill broken, stains without secondary, guarantees product purity, the single resultant quantity is large simultaneously, and efficient is high.
On the basis of technique scheme, the present invention can also do following improvement.
Further, in the step (1), described carbon dust purity is not less than 99.999%, granularity between 20 μ m to 1000 μ m, described silica flour purity is not less than 99.999%, granularity between 20 μ m to 1000 μ m, and described carbon dust and described silica flour according to molar mass than mixing for 1:1.
Further, in the step (2), the frequency of described microwave is 900～3000MHz.
Further, in the step (2), described heating may further comprise the steps:
A. the temperature in the described heating chamber is heated to 1400 ℃～1600 ℃, and kept 0.5～3 hour, the pressure in the described heating chamber remains between 1KPa～20KPa;
B. the temperature in the described heating chamber is heated to 2000 ℃～2200 ℃, and kept 1～5 hour, the pressure in the described heating chamber remains between 10KPa～60KPa.
The beneficial effect that adopts above-mentioned further scheme is that the silicon fusing point is 1483 ℃, reaches silica flour fusing after the described heating chamber temperature of step a, the silica flour of fusing immediately with carbon dust reaction Formed silicon carbide particle.About 2100 ℃ of silicon carbide sublimation temperature, the silicon-carbide particle that is generated by step a reach again distillation after the described heating chamber temperature of step b, and again crystallization in crucible, form the silicon-carbide particles of greater particle size, particle size 0.1mm-1mm.Under the specified temp, silicon carbide sublimation speed raises with pressure and reduces, and keeping furnace pressure is in order to control silicon carbide liter speed.
Further, in the step (2), in the described heat-processed, in described heating chamber, pass into argon gas.
The beneficial effect that adopts above-mentioned further scheme is to pass into argon gas to can be used as heat-transfer medium, plays simultaneously the not oxidation by air of protection graphite material.
Embodiment
Below principle of the present invention and feature are described, institute only gives an actual example and to be used for explanation the present invention, is not be used to limiting scope of the present invention.
Embodiment 1
(1) be that 99.999% carbon dust 1200g and the silica flour 2800g of purity 99.999% mix with purity;
(2) selecting the frequency of microwave is 900MHz, and the carbon dust and the silica flour that mix are put into heating chamber, passes into argon gas as shielding gas after vacuumizing;
(3) heating may further comprise the steps:
A. the pressure in the heating chamber is maintained 1KPa, the temperature in the heating chamber is heated to 1500 ℃, and kept 0.5 hour;
B. the pressure in the heating chamber is maintained 60KPa, the temperature in the heating chamber is heated to 2100 ℃, and kept 1 hour.
Obtain synthesizing silicon carbide micro mist 4000g after the cooling, purity is not less than 99.999%.
Embodiment 2
(1) be that 99.999% carbon dust 1200g and the silica flour 2800g of purity 99.999% mix with purity;
(2) selecting the frequency of microwave is 900MHz, and the carbon dust and the silica flour that mix are put into heating chamber, passes into argon gas as shielding gas after vacuumizing;
(3) heating may further comprise the steps:
A. the pressure in the heating chamber is maintained 1KPa, the temperature in the heating chamber is heated to 1500 ℃, and kept 1 hour;
B. the pressure in the heating chamber is maintained 60KPa, the temperature in the heating chamber is heated to 2100 ℃, and kept 2 hours.
Obtain synthesizing silicon carbide micro mist 4000g after the cooling, purity is not less than 99.999%.
Embodiment 3
(1) be that 99.9999% carbon dust 2400g and the silica flour 5600g of purity 99.999% mix with purity;
(2) selecting the frequency of microwave is 2000MHz, and the carbon dust and the silica flour that mix are put into heating chamber, passes into argon gas as shielding gas after vacuumizing;
(3) heating may further comprise the steps:
A. the pressure in the heating chamber is maintained 1KPa, the temperature in the heating chamber is heated to 1500 ℃, and kept 2 hours;
B. the pressure in the heating chamber is maintained 50KPa, the temperature in the heating chamber is heated to 2100 ℃, and kept 3 hours.
Obtain synthesizing silicon carbide micro mist 8000g after the cooling, purity is not less than 99.999%.
The above only is preferred embodiment of the present invention, and is in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. a preparation method who is used for the silicon carbide micro-powder of growing silicon carbice crystals is characterized in that, may further comprise the steps:
(1) with the even mixing of carbon dust and silica flour, obtains mixture;
(2) described mixture is joined in the heating chamber, by microwave described mixture is heated, get final product to get described silicon carbide micro-powder for growing silicon carbice crystals.
2. the preparation method of described silicon carbide micro-powder for growing silicon carbice crystals according to claim 1, it is characterized in that, in the step (1), described carbon dust purity is not less than 99.999%, granularity between 20 μ m to 1000 μ m, described silica flour purity is not less than 99.999%, granularity between 20 μ m to 1000 μ m, and described carbon dust and described silica flour according to molar mass than mixing for 1:1.
3. the preparation method of described silicon carbide micro-powder for growing silicon carbice crystals according to claim 1 is characterized in that in the step (2), the frequency of described microwave is 900～3000MHz.
4. the preparation method of described silicon carbide micro-powder for growing silicon carbice crystals according to claim 1 is characterized in that in the step (2), described heating may further comprise the steps:
A. the temperature in the described heating chamber is heated to 1400 ℃～1600 ℃, and kept 0.5～3 hour, the pressure in the described heating chamber remains between 1KPa～20KPa;
B. the temperature in the described heating chamber is heated to 2000 ℃～2200 ℃, and kept 1～5 hour, the pressure in the described heating chamber remains between 10KPa～60KPa.
5. according to claim 1 to the preparation method of 4 each described silicon carbide micro-powders for growing silicon carbice crystals, it is characterized in that, in the step (2), in the described heat-processed, in described heating chamber, pass into argon gas.
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| CN201310003974.0A CN103058192B (en) | 2013-01-06 | 2013-01-06 | A kind of preparation method of the silicon carbide micro-powder for growing silicon carbice crystals |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106882806A (en) * | 2015-12-12 | 2017-06-23 | 天津榛发科技有限责任公司 | A kind of preparation method of silicon carbide micro-powder |
| CN107128924A (en) * | 2017-06-13 | 2017-09-05 | 宁夏大学 | A kind of method that utilization microwave sintering prepares β SiC |
| CN107974712A (en) * | 2017-11-14 | 2018-05-01 | 山东天岳先进材料科技有限公司 | A kind of preparation method of Semi-insulating silicon carbide mono-crystal |
| CN108946735A (en) * | 2017-05-19 | 2018-12-07 | 新疆天科合达蓝光半导体有限公司 | A kind of synthetic method of the big partial size sic powder of growing silicon carbice crystals |
| CN111960420A (en) * | 2020-09-03 | 2020-11-20 | 上海第二工业大学 | Method for rapidly producing nano silicon carbide by microwave irradiation of electronic waste |
| CN115124040A (en) * | 2022-07-07 | 2022-09-30 | 安徽微芯长江半导体材料有限公司 | Solid-phase synthesis method for improving material ratio of large-particle-size silicon carbide powder |
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| US4117096A (en) * | 1976-08-20 | 1978-09-26 | Nippon Crucible Co., Ltd. | Process for producing powder of β-type silicon carbide |
| CN1037689A (en) * | 1988-04-28 | 1989-12-06 | 苏联科学院宏观动力学结构研究所 | Produce the method for silicon B-carbide |
| CN1636870A (en) * | 2004-12-30 | 2005-07-13 | 清华大学 | Nanometer SiC powder preparing process |
| CN101891192A (en) * | 2010-07-02 | 2010-11-24 | 山东大学 | Method for synthesizing carbide nano powder by solid-phase reaction |
| CN102701208A (en) * | 2012-06-21 | 2012-10-03 | 上海硅酸盐研究所中试基地 | High-temperature solid-phase synthesis method of high-purity silicon carbide powder |
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2013
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| US4117096A (en) * | 1976-08-20 | 1978-09-26 | Nippon Crucible Co., Ltd. | Process for producing powder of β-type silicon carbide |
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| 姜洪舟等: "《无机非金属材料热加工设备》", 31 July 2012, article "5.2.9材料的微波加热技术", pages: 423 * |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106882806A (en) * | 2015-12-12 | 2017-06-23 | 天津榛发科技有限责任公司 | A kind of preparation method of silicon carbide micro-powder |
| CN108946735A (en) * | 2017-05-19 | 2018-12-07 | 新疆天科合达蓝光半导体有限公司 | A kind of synthetic method of the big partial size sic powder of growing silicon carbice crystals |
| CN108946735B (en) * | 2017-05-19 | 2022-11-11 | 新疆天科合达蓝光半导体有限公司 | Synthesis method of large-particle-size silicon carbide powder for silicon carbide crystal growth |
| CN107128924A (en) * | 2017-06-13 | 2017-09-05 | 宁夏大学 | A kind of method that utilization microwave sintering prepares β SiC |
| CN107974712A (en) * | 2017-11-14 | 2018-05-01 | 山东天岳先进材料科技有限公司 | A kind of preparation method of Semi-insulating silicon carbide mono-crystal |
| CN111960420A (en) * | 2020-09-03 | 2020-11-20 | 上海第二工业大学 | Method for rapidly producing nano silicon carbide by microwave irradiation of electronic waste |
| CN115124040A (en) * | 2022-07-07 | 2022-09-30 | 安徽微芯长江半导体材料有限公司 | Solid-phase synthesis method for improving material ratio of large-particle-size silicon carbide powder |
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| CN103058192B (en) | 2016-05-25 |
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Address after: 102206, Changping District, Shahe, Beijing Town, North Village Road, West Bridge, Shahe industrial city Applicant after: Hebei Tongguang Crystal Co., Ltd. Address before: Four building B, building 071051, building six, Science Park, 5699 North Second Ring Road, Hebei, Baoding, Applicant before: Baoding Kerui Crystal Co., Ltd. |
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Denomination of invention: Preparation method of silicon carbide micro-powder used in silicon carbide crystal growth Effective date of registration: 20160826 Granted publication date: 20160525 Pledgee: Chinese for key construction fund limited Pledgor: Hebei Tongguang Crystal Co., Ltd. Registration number: 2016990000669 |
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Date of cancellation: 20201207 Granted publication date: 20160525 Pledgee: Chinese for key construction fund Ltd. Pledgor: HEBEI TONGGUANG CRYSTAL Co.,Ltd. Registration number: 2016990000669 |
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Address after: No. 6001, North Third Ring Road, Baoding City, Hebei Province Patentee after: Hebei Tongguang Semiconductor Co.,Ltd. Address before: 102206 West Shahe Industrial City, ZhuangQiao, beiercun Road, Shahe Town, Changping District, Beijing Patentee before: HEBEI TONGGUANG CRYSTAL Co.,Ltd. |