CN103058192B - A kind of preparation method of the silicon carbide micro-powder for growing silicon carbice crystals - Google Patents
A kind of preparation method of the silicon carbide micro-powder for growing silicon carbice crystals Download PDFInfo
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- CN103058192B CN103058192B CN201310003974.0A CN201310003974A CN103058192B CN 103058192 B CN103058192 B CN 103058192B CN 201310003974 A CN201310003974 A CN 201310003974A CN 103058192 B CN103058192 B CN 103058192B
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- silicon carbide
- carbide micro
- silicon
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 26
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000000843 powder Substances 0.000 title claims abstract description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 15
- 239000010703 silicon Substances 0.000 title claims abstract description 15
- 239000013078 crystal Substances 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 235000013312 flour Nutrition 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 16
- 239000000428 dust Substances 0.000 claims abstract description 16
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000012467 final product Substances 0.000 claims abstract description 3
- 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
- 238000000034 method Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 7
- 238000013467 fragmentation Methods 0.000 abstract description 5
- 238000006062 fragmentation reaction Methods 0.000 abstract description 5
- 239000000047 product Substances 0.000 abstract description 4
- 239000003595 mist Substances 0.000 description 5
- 230000002194 synthesizing effect Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000003825 pressing 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
- 239000002699 waste material Substances 0.000 description 1
Abstract
The preparation method who the present invention relates to a kind of silicon carbide micro-powder for growing silicon carbice crystals, comprises the following steps: by the even mixing of carbon dust and silica flour, obtain mixture; Again described mixture is joined in heating clamber, by microwave, described mixture is heated, get final product to obtain the described silicon carbide micro-powder for growing silicon carbice crystals. The present invention adopts heating using microwave, homogeneous heating, and synthetic silicon-carbide particle uniform particle diameter is good, and the product obtaining does not need to use traditional ball mill fragmentation, stains without secondary, ensures product purity, and single synthetic quantity is large simultaneously, 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 for carborundum crystalsThe preparation method of the silicon carbide micro-powder of growth.
Background technology
Existing growing silicon carbice crystals adopts after eddy-current heating sintering broken more with high purity micropowder, for example, and willSilica flour and carbon dust are positioned in black-fead crucible after mixing, and synthesize synthesis temperature by eddy-current heatingReach more than 2000 DEG C, carbon dust and silica flour react synthetic silicon carbide micro-powder. Adopt in this way syntheticSilicon carbide micro-powder sinters block into, need to carry out fragmentation again, has caused the secondary pollution of carborundum powder,Synthetic micro mist granule size after fragmentation differs, and needs through screening, causes and stains and waste. And senseThe single synthetic quantity that should add thermal synthesis is less, more difficultly meets large-scale production requirement.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of carborundum for growing silicon carbice crystalsThe preparation method of micro mist, reduces raw material building-up process and pollutes, and single synthetic quantity is large, simultaneously synthesizing silicon carbideMicro powder granule is even, without fragmentation.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of for growing silicon carbice crystalsThe preparation method of silicon carbide micro-powder, comprises the following steps:
(1) by the even mixing of carbon dust and silica flour, obtain mixture;
(2) described mixture is joined in heating clamber, by microwave, described mixture is heated,Get final product to obtain the described silicon carbide micro-powder for growing silicon carbice crystals.
The invention has the beneficial effects as follows: the present invention adopts heating using microwave homogeneous heating, synthetic carborundumGrain diameter homogeneity is good, and the product obtaining does not need to use traditional ball mill fragmentation, stain without secondary,Ensure product purity, single synthetic quantity is large simultaneously, and efficiency is high.
On the basis of technique scheme, the present invention can also do following improvement.
Further, in step (1), described carbon dust purity is not less than 99.999%, granularity between20 μ m are to 1000 μ m, and described silica flour purity is not less than 99.999%, and granularity is between 20 μ m to 1000μ m, and described carbon dust and described silica flour according to molal weight than mixing for 1:1.
Further, in step (2), described micro-wave frequency is 900～3000MHz.
Further, in step (2), described heating comprises the following steps:
A. the temperature in described heating clamber is heated to 1400 DEG C～1600 DEG C, and keeps 0.5～3 hour,Pressure in described heating clamber remains between 1KPa～20KPa;
B. the temperature in described heating clamber is heated to 2000 DEG C～2200 DEG C, and keeps 1～5 hour,Pressure in described heating clamber remains between 10KPa～60KPa.
The beneficial effect that adopts above-mentioned further scheme is that silicon fusing point is 1483 DEG C, reaches described in step a and addsSilica flour fusing after the temperature of hot cell, the silica flour of fusing reacts Formed silicon carbide particle immediately with carbon dust. CarborundumApproximately 2100 DEG C of sublimation temperatures, the silicon-carbide particle being generated by step a reaches heating clamber temperature described in step bAfter distillation again, and crystallization again in crucible, forms the silicon-carbide particles of greater particle size, particle size0.1mm-1mm. Under specified temp, silicon carbide sublimation speed raises and reduces with pressure, keeps pressing in stovePower is in order to control carborundum liter speed.
Further, in step (2), in described heating process, in described heating clamber, 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 simultaneouslyThe not oxidation by air of protection graphite material.
Detailed description of the invention
Below principle of the present invention and feature are described, example is only for explaining the present invention, andNon-for limiting scope of the present invention.
Embodiment 1
(1) the carbon dust 1200g that is 99.999% by purity mixes with the silica flour 2800g of purity 99.999%Evenly;
(2) selecting micro-wave frequency is 900MHz, and the carbon dust mixing and silica flour are put into heating clamber,After vacuumizing, pass into argon gas as protective gas;
(3) heating, comprises the following steps:
A. the pressure in heating clamber is maintained to 1KPa, the temperature in heating clamber is heated to 1500 DEG C,And keep 0.5 hour;
B. the pressure in heating clamber is maintained to 60KPa, the temperature in heating clamber is heated to 2100 DEG C,And keep 1 hour.
After cooling, obtain synthesizing silicon carbide micro mist 4000g, purity is not less than 99.999%.
Embodiment 2
(1) the carbon dust 1200g that is 99.999% by purity mixes with the silica flour 2800g of purity 99.999%Evenly;
(2) selecting micro-wave frequency is 900MHz, and the carbon dust mixing and silica flour are put into heating clamber,After vacuumizing, pass into argon gas as protective gas;
(3) heating, comprises the following steps:
A. the pressure in heating clamber is maintained to 1KPa, the temperature in heating clamber is heated to 1500 DEG C,And keep 1 hour;
B. the pressure in heating clamber is maintained to 60KPa, the temperature in heating clamber is heated to 2100 DEG C,And keep 2 hours.
After cooling, obtain synthesizing silicon carbide micro mist 4000g, purity is not less than 99.999%.
Embodiment 3
(1) the silica flour 5600g of the carbon dust 2400g that is 99.9999% by purity and purity 99.999% is mixedClose evenly;
(2) selecting micro-wave frequency is 2000MHz, and the carbon dust mixing and silica flour are put into heating clamber,After vacuumizing, pass into argon gas as protective gas;
(3) heating, comprises the following steps:
A. the pressure in heating clamber is maintained to 1KPa, the temperature in heating clamber is heated to 1500 DEG C,And keep 2 hours;
B. the pressure in heating clamber is maintained to 50KPa, the temperature in heating clamber is heated to 2100 DEG C,And keep 3 hours.
After cooling, obtain synthesizing silicon carbide micro mist 8000g, purity is not less than 99.999%.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, not all in the present inventionSpirit and principle within, any amendment of doing, be equal to replacement, improvement etc., all should be included in thisWithin bright protection domain.
Claims (4)
1. for a preparation method for the silicon carbide micro-powder of growing silicon carbice crystals, it is characterized in that,Comprise the following steps:
(1) by the even mixing of carbon dust and silica flour, obtain mixture;
(2) described mixture is joined in heating clamber, by microwave, described mixture is heated,Get final product to obtain the described silicon carbide micro-powder for growing silicon carbice crystals; Described heating comprises the following steps: a.Temperature in described heating clamber is heated to 1400 DEG C～1600 DEG C, and keeps 0.5～3 hour, described inPressure in heating clamber remains between 1KPa～20KPa; B. the temperature in described heating clamber is heated to2000 DEG C～2200 DEG C, and keep 1～5 hour, the pressure in described heating clamber remain on 10KPa～Between 60KPa.
2. according to claim 1 for the preparation method of the silicon carbide micro-powder of growing silicon carbice crystals,It is characterized in that, in step (1), described carbon dust purity is not less than 99.999%, and granularity is between 20μ m is to 1000 μ m, and described silica flour purity is not less than 99.999%, and granularity is between 20 μ m to 1000μ m, and described carbon dust is that 1:1 mixes with described silica flour according to mol ratio.
3. according to claim 1 for the preparation method of the silicon carbide micro-powder of growing silicon carbice crystals,It is characterized in that, in step (2), described micro-wave frequency is 900～3000MHz.
4. according to the silicon carbide micro-powder for growing silicon carbice crystals described in claims 1 to 3 any onePreparation method, it is characterized in that, in step (2), in described heating process, to described heating clamberIn pass into argon gas.
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| 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 |
| 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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| 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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| JPS5325300A (en) * | 1976-08-20 | 1978-03-08 | Nippon Crucible Co | Process for preparing betaatype silicon carbide particle |
| SU1706963A1 (en) * | 1988-04-28 | 1992-01-23 | Институт структурной макрокинетики АН СССР | Method for preparation @@@-silicium carbide |
| CN1304286C (en) * | 2004-12-30 | 2007-03-14 | 清华大学 | Nanometer SiC powder preparing process |
| CN101891192B (en) * | 2010-07-02 | 2012-01-18 | 山东大学 | Method for synthesizing carbide nano powder by solid-phase reaction |
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| 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 |
Non-Patent Citations (1)
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| Microwave synthesis of phase-pure,fine silicon carbide powder;L.N.Satapathy etc.;《Materials Research Bulletin》;20051006;第40卷(第10期);1871-1882 * |
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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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Free format text: CORRECT: APPLICANT; FROM: BAODING KERUI CRYSTAL CO., LTD. TO: HEBEI TONGGUANG 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. |