CN101704523A - Production technology of high purity silicon carbide - Google Patents
Production technology of high purity silicon carbide Download PDFInfo
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- CN101704523A CN101704523A CN200910218246A CN200910218246A CN101704523A CN 101704523 A CN101704523 A CN 101704523A CN 200910218246 A CN200910218246 A CN 200910218246A CN 200910218246 A CN200910218246 A CN 200910218246A CN 101704523 A CN101704523 A CN 101704523A
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Abstract
The invention provides a production technology of high purity silicon carbide, comprising the following steps of: mixing silicon dioxide and carbon black with the weight ratio of 1:1.2; preparing pulp from the mixture and sulfuric acid solution with the concentration of 60-80g/l according to the solid-liquid ratio of 1:4; putting the pulp in a pressurizing reactor; controlling the pressure in the reactor; stirring for 1-3h,and filtering to obtain mixing slag; washing the mixing slag to neutral; pelletizing the mixing slag, putting particles into an electric furnace; roasting the particles with the temperature of 1600 DEG C to 1800 DEG C; separating liquid and solid; cooling; crushing obtained silicon carbide; washing the crushed silicon carbide by sulfuric acid with the concentration of 80-120g/L; filtering, and drying to obtain the high purity silicon carbide with the impurity content less than 0.001 percent. The invention belongs to a smelting method for preparing the high purity silicon carbide by the silicon dioxide and the carbon black. After carrying out pressurization and acid leaching on the silicon dioxide and graphite, the electric furnace is utilized to roast, and the silicon dioxide and the graphite are separated, then the sulfuric acid is used to wash the silicon dioxide and the graphite to obtain the high purity silicon carbide. The invention has the advantages of simple equipment, short technological process, low production cost and environment protection.
Description
Technical field
The present invention relates to metallurgy, chemical field, specifically is a kind of technology by silicon-dioxide and production of carbon black high-purity silicon carbide.
Background technology
The silicon carbide molecular formula is SiC, and silicon carbide is the compound of typical covalent bonds, and the decomposition temperature under a normal atmosphere is 2400 ℃, no fusing point.The density of SiC is 3.18g/cm
3, its Mohs' hardness between 9.2～9.3, microhardness 3300kg/cm
2Silicon carbide is high temperature resistant, and with strong acid, the equal Fails To Respond of highly basic, electrical and thermal conductivity is good, has very strong capability of resistance to radiation.High-purity silicon carbide is because fine size, narrowly distributing, quality is even, thereby it is big to have specific surface area, the surfactivity height, chemical reaction is fast, and solubleness is big, and sintering temperature is low and sintering strength is high, characteristics such as the filler reinforcement performance is good, and unique electrically, magnetic, optical property etc., be widely used in national defense construction, high-performance ceramics, microelectronics and information material industry, market outlook are good.The purity of SiC directly influences its electrical properties, and the single-crystal silicon carbide of foreign matter content＜0.001% can be applied to semiconductor material, short-wavelength light electrical part and high temperature, radiation-resistant high-frequency high-power device.But owing to highly purified silicon carbide preparation cost height, complex process, technical requirements height, the present domestic independently throughput that do not have, the technology of suitability for industrialized production is by the monopolization of external major company, so market value is also higher, therefore, the high-purity carborundum of developing low-cost has great significance to breaking foreign technology monopolization for its application broad market prospect in the high-end technology field.
Summary of the invention
The present invention has overcome existing high-purity silicon carbide preparation method's deficiency, be simple and easy to silicon-dioxide and carbon black do raw material, provide that a kind of smelting process is simple, reliable easily goes and eco-friendly high-purity silicon carbide production technique.
Realize that step of the present invention is: (1) is with the silicon-dioxide and the carbon black of foreign matter content＜0.1%, cross the 0.0043mm sieve respectively, it is that the sulphuric acid soln of 60～80g/l is sized mixing by solid-to-liquid ratio 1: 4 and concentration that silicon-dioxide and carbon black mix the back with mass ratio 1: 1.2, place autoclave then, control still internal pressure is 1.2MPa, and 200 ℃ of temperature stirred 1～3 hour, slag liquid after sulfuric acid leaches filters to such an extent that mix slag, is washed with water to neutrality; (2) will mix slag and granulate, particle diameter is between 3～4cm, puts into the electric furnace roasting, temperature is between 1600～1800 ℃, some covers the product surface for silicon with liquid form reaction product, and silicon carbide is owing to descending the bed interface than great, and most impurity enter liquid-phase silicone simultaneously; Liquid-solid phase is separated, and cooling obtains silicon carbide; (3) with the silicon carbide fragmentation that obtains, be the sulfuric acid scrubbing of 80～120g/L with concentration, washing time is 4～8 hours, filters, oven dry obtains foreign matter content less than＜0.001% high-purity silicon carbide.
All per-cent, liquid-solid ratio and concentration content among the present invention except specializing, is mass percent example or mass percent concentration content.
Leach liquor after the autoclave acidleach and the washing lotion after the water washing are returned in the autoclave and are recycled.
Beneficial effect of the present invention is: be simple and easy to silicon-dioxide and carbon black as raw material, roasting behind the pressurized acid leaching, utilize the fusing point difference removal of impurities of silicon and silicon carbide to obtain high-purity silicon carbide, technical process is short, production cost is low, realize suitability for industrialized production easily, filtrate after the pickling simultaneously can recycle, and is free from environmental pollution.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Embodiment 1: with the foreign matter content of levigate mistake is that the carbon black of 0.05% silicon-dioxide and foreign matter content＜0.09% is crossed the 0.0043mm sieve respectively, mixing back and concentration with mass ratio 1: 1.2 is that the sulphuric acid soln of 60g/L is sized mixing, liquid-solid ratio is 4: 1, place autoclave then, control still internal pressure is 1.2MPa, and 200 ℃ of temperature stirred 1 hour, slag liquid after sulfuric acid leaches filters to such an extent that mix slag, is washed with water to neutrality; To mix slag and granulate, particle diameter is 3cm, puts into the electric furnace roasting, temperature with the silicon carbide fragmentation that obtains, is the sulphuric acid soln washing of 80g/L with concentration at 1600 degree, washing time is 4 hours, filters, and oven dry obtains foreign matter content less than＜0.001% high-purity silicon carbide.
Embodiment 2: with the foreign matter content of levigate mistake is that the carbon black of 0.05% silicon-dioxide and foreign matter content＜0.09% is crossed the 0.0043mm sieve respectively, mixing back and concentration with mass ratio 1: 1.2 is that the sulphuric acid soln of 60g/L is sized mixing, liquid-solid ratio is 4: 1, place autoclave then, control still internal pressure is 1.2MPa, and 200 ℃ of temperature stirred 1 hour, slag liquid after sulfuric acid leaches filters to such an extent that mix slag, is washed with water to neutrality; To mix slag and granulate, particle diameter is about 3cm, puts into the electric furnace roasting, temperature with the silicon carbide fragmentation that obtains, is the sulphuric acid soln washing of 80g/L with concentration at 1600 degree, washing time is 4 hours, filters, and oven dry obtains foreign matter content less than＜0.001% high-purity silicon carbide.
Embodiment 3: with the foreign matter content of levigate mistake is that the carbon black of 0.03% silicon-dioxide and foreign matter content＜0.05% is crossed the 0.0043mm sieve respectively, mixing back and concentration with mass ratio 1: 1.2 is that the sulphuric acid soln of 60g/L is sized mixing, liquid-solid ratio is 4: 1, place autoclave then, control still internal pressure is 1.2MPa, and 200 ℃ of temperature stirred 2 hours, slag liquid after sulfuric acid leaches filters to such an extent that mix slag, is washed with water to neutrality; To mix slag and granulate, particle diameter is 3cm, puts into the electric furnace roasting, temperature with the silicon carbide fragmentation that obtains, is the sulphuric acid soln washing of 100g/L with concentration at 1700 degree, washing time is 5 hours, filters, and oven dry obtains foreign matter content less than＜0.001% high-purity silicon carbide.
Embodiment 4: with the foreign matter content of levigate mistake is that the carbon black of 0.05% silicon-dioxide and foreign matter content＜0.07% is crossed the 0.0043mm sieve respectively, mixing back and concentration with mass ratio 1: 1.2 is that the sulphuric acid soln of 80g/L is sized mixing, liquid-solid ratio is 4: 1, place autoclave then, control still internal pressure is 1.2MPa, and 200 ℃ of temperature stirred 3 hours, slag liquid after sulfuric acid leaches filters to such an extent that mix slag, is washed with water to neutrality; To mix slag and granulate, particle diameter is 4cm, puts into the electric furnace roasting, temperature with the silicon carbide fragmentation that obtains, is the sulphuric acid soln washing of 120g/L with concentration at 1800 degree, washing time is 6 hours, filters, and oven dry obtains foreign matter content less than＜0.001% high-purity silicon carbide.
The invention belongs to the smelting process of producing high-purity silicon carbide by silicon-dioxide and carbon black, this method is by after carrying out pressurized acid leaching to silicon-dioxide and graphite, carry out roasting, separation with electric furnace, obtain high-purity silicon carbide with sulfuric acid scrubbing then, equipment is simple, technical process is short, and production cost is low, environmental friendliness.
Claims (1)
1. production technique that extracts high-purity silicon carbide by silicon-dioxide and carbon black, the steps include: that (1) cross the 0.0043mm sieve respectively with the silicon-dioxide of foreign matter content＜0.1% and carbon black, it is that the sulphuric acid soln of 60～80g/l is sized mixing by solid-to-liquid ratio 1: 4 and concentration that silicon-dioxide and carbon black mix the back with mass ratio 1: 1.2, place autoclave, control still internal pressure is 1.2MPa, and 200 ℃ of temperature stirred 1～3 hour, slag liquid after sulfuric acid leaches filters to such an extent that mix slag, is washed with water to neutrality; (2) will mix slag and granulate, particle diameter is between 3～4cm, puts into the electric furnace roasting, temperature is between 1600～1800 ℃, some covers the product surface for silicon with liquid form reaction product, and silicon carbide is owing to descending the bed interface than great, and most impurity enter liquid-phase silicone simultaneously; Liquid-solid phase is separated, and cooling obtains silicon carbide; (3) with the silicon carbide fragmentation that obtains, with concentration is the sulfuric acid scrubbing of 80～120g/L, washing time is 4～8 hours, filter, oven dry obtains foreign matter content less than＜0.001% high-purity silicon carbide, and all above-mentioned per-cents, liquid-solid ratio and concentration content are mass percent example or mass percent concentration content.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102303867A (en) * | 2011-08-16 | 2012-01-04 | 浙江大学 | Method for preparing porous silicon carbide by utilizing diatomite |
| CN102489218A (en) * | 2011-11-14 | 2012-06-13 | 朱胜利 | Method for granulating and forming silicon carbide fine powder and silicon carbide granule |
| CN107699955A (en) * | 2017-08-30 | 2018-02-16 | 昆明理工大学 | It is a kind of using microwave heat remove single-crystal silicon carbide defect in and surface organic impurities method |
| CN108840323A (en) * | 2018-07-10 | 2018-11-20 | 中喜（宁夏）新材料有限公司 | Coal ash for manufacturing for graphene chip method |
| CN110104651A (en) * | 2019-06-24 | 2019-08-09 | 深圳市动力创新科技企业（有限合伙） | A kind of high-purity silicon carbide, sic wafer and preparation method thereof |
| CN113912064A (en) * | 2021-11-26 | 2022-01-11 | 连云港市沃鑫高新材料有限公司 | Preparation method of silicon carbide powder |
| CN114261966A (en) * | 2021-12-13 | 2022-04-01 | 江西省矿产资源保障服务中心 | Method for synthesizing submicron silicon carbide spheres by using carbon-containing silicon dioxide powder with low energy consumption |
-
2009
- 2009-11-25 CN CN200910218246A patent/CN101704523A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102303867A (en) * | 2011-08-16 | 2012-01-04 | 浙江大学 | Method for preparing porous silicon carbide by utilizing diatomite |
| CN102489218A (en) * | 2011-11-14 | 2012-06-13 | 朱胜利 | Method for granulating and forming silicon carbide fine powder and silicon carbide granule |
| CN107699955A (en) * | 2017-08-30 | 2018-02-16 | 昆明理工大学 | It is a kind of using microwave heat remove single-crystal silicon carbide defect in and surface organic impurities method |
| CN108840323A (en) * | 2018-07-10 | 2018-11-20 | 中喜（宁夏）新材料有限公司 | Coal ash for manufacturing for graphene chip method |
| CN110104651A (en) * | 2019-06-24 | 2019-08-09 | 深圳市动力创新科技企业（有限合伙） | A kind of high-purity silicon carbide, sic wafer and preparation method thereof |
| CN110104651B (en) * | 2019-06-24 | 2022-12-06 | 深圳市本征方程石墨烯技术股份有限公司 | High-purity silicon carbide, silicon carbide wafer and preparation method thereof |
| CN113912064A (en) * | 2021-11-26 | 2022-01-11 | 连云港市沃鑫高新材料有限公司 | Preparation method of silicon carbide powder |
| CN113912064B (en) * | 2021-11-26 | 2022-11-22 | 连云港市沃鑫高新材料有限公司 | Preparation method of silicon carbide powder |
| CN114261966A (en) * | 2021-12-13 | 2022-04-01 | 江西省矿产资源保障服务中心 | Method for synthesizing submicron silicon carbide spheres by using carbon-containing silicon dioxide powder with low energy consumption |
| CN114261966B (en) * | 2021-12-13 | 2024-01-30 | 江西省矿产资源保障服务中心 | Method for synthesizing submicron silicon carbide balls by using carbon-containing silicon dioxide powder with low energy consumption |
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Open date: 20100512 |