CN104828825A - Low-cost method for synthesizing silicon carbide powder at low temperature - Google Patents
Low-cost method for synthesizing silicon carbide powder at low temperature Download PDFInfo
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Abstract
The invention relates to a low-cost method for synthesizing silicon carbide powder at low temperature. The method comprises the following steps: by using high-purity carbon fibers and high-purity silicon powder as raw materials, charging argon or an argon-hydrogen mixture into a growth chamber in a heightened crucible at 500-1000 DEG C under the vacuum degree of less than 10<-3>Pa until the pressure is 800-900mbar, and heating to 1000-1300 DEG C to perform synthesis. By adopting the one-step synthesis process, the method overcomes the defects of complex secondary synthesis procedure, long time consumption and artificial introduction of impurities and the like. The method can synthesize the large-particle-size silicon carbide powder of which the particle size is controllable within the range of 5-10kg. The method has the advantages of low cost and simple technique.
Description
Technical field
The present invention relates to a kind of method of the low cost low temperature synthesizing silicon carbide powder for silicon carbide monocrystal growth, belong to field of inorganic nonmetallic material.
Background technology
To have energy gap large because of it for single-crystal silicon carbide, breakdown electric field is high, thermal conductivity is large, electronics saturation drift velocity is high, specific inductivity is little, capability of resistance to radiation is strong, the characteristic that good chemical stability etc. are unique, obvious superiority has been compared with s-generation semiconductor material with first-generation semiconductor material, be considered to manufacture opto-electronic device, Deep trench termination, the semiconductor material that power electronic devices is desirable, at white-light illuminating, optical storage, screen display, space flight and aviation, hyperthermia radiation environment, petroleum prospecting, automatization, radar and communications, the aspects such as automotive circuit diagram are widely used.In single crystalline substrate, iso-epitaxy semiconductor film and device technology etc., development rapidly, is one of optimal third generation semiconductor material.
Sic powder quality plays a very important role when sublimation growth single-crystal silicon carbide, directly affects crystalline quality and the growth thickness of monocrystalline.Along with single-crystal silicon carbide substrate watt device and the extensive widespread use of power electronic devices, more and more urgent to the demand of major diameter single crystal, 4 inches by current widespread use expand to 6 inches even 8 inches.But along with the increase of substrate diameter, growth crucible size is larger, the source material carborundum powder needed increases thereupon, 6 inches of every heats of single crystal growing need charge amount up to 2-3kg, and current synthetic method cost is high, can not meet the needs that industrialization is produced, therefore by improving synthetic material technology, reduce costs, source material granularity is controlled, has become the difficult problem that growth large single crystal is urgently to be resolved hurrily at present.
Chinese patent document CN102701208A discloses the high temperature process heat method of high-purity silicon carbide powder, after high-purity silicon powder and high-purity carbon dust mix by the method, then hypertonic solutions is carried out, namely high purity inert gas is adopted to vacuumize cleaning under different pressures and differing temps, then carry out high―temperature nuclei at 1800-2100 DEG C, final acquisition nitrogen content is at the high-purity silicon carbide powder of below 15ppm.CN103708463A discloses the preparation method of feather weight high-pure SiC power, first the method carries out the pre-treatment of crucible plated film, silicon carbide film is plated after first plating carbon film, then put into intermediate-frequency heating furnace after silica flour and carbon dust being mixed, between 1500-1900 DEG C, high―temperature nuclei obtains feather weight high-purity silicon carbide powder.CN101302011A discloses the artificial synthesis of the high-pure SiC power for semiconductor single-crystal growth, main employing secondary synthesis method, after silica flour and carbon dust mixing, first time first low temperature 1500 DEG C synthesis, then increase the temperature to 1800-2000 DEG C after being mixed by the powder of single sintering and carry out secondary synthesis, the method effectively can remove the impurity element in silica flour and carbon dust.
The raw material adopted in the above existing method is pure silicon powder and carbon dust, and especially high-purity carbon dust belongs to external prohibited material, is important national defense applications starting material, expensive, and this is also the major reason causing single-crystal silicon carbide substrate price high.In addition, above-mentioned three kinds of methods all adopt high―temperature nuclei, and synthesis temperature is all more than 1500 DEG C, reach as high as 2100 DEG C, thus require very high to the equipment configuration of synthetic material, as high temperature realization, leak rate is little, vacuum tightness is high, cooling power is strong, thus equipment investment is large, cost is high.
Summary of the invention
The present invention is directed to the deficiency that prior art synthesizing silicon carbide powder exists, provide a kind of and can realize the large and preparation method of the sic powder of uniform, controllable of low cost, low temperature, low equipment investment, high yield, granularity.
Low cost low temperature prepares a method for sic powder, comprises the following steps:
(1) prepare burden:
Adopt high-purity carbon fiber and high-purity silicon powder to be raw material, the ratio of 1:1 mixes in molar ratio.
The purity of described high-purity carbon fiber and high-purity silicon powder raw material is all greater than 99%, carbon fiber diameter 7-10 μm, length 1-100mm, and silicon particle size is less than 500 μm;
(2) synthesize:
Described silica flour and carbon fiber are put into and increase crucible, be placed in Medium Frequency Induction Heating Furnace, process furnace growth room vacuumizes, and oxygen, nitrogen and water vapour in removing growth room, be increased to 500-1000 DEG C by temperature simultaneously; Then vacuumize, make vacuum tightness be less than 10
-3pa; In growth room, be filled with the mixed gas of argon gas or argon gas and hydrogen, pressure is 800-900mbar, and be warming up to 1000-1300 DEG C and synthesize, generated time is 5-10 hour, is then down to room temperature, can obtain the sic powder that epigranular is controlled.
Preferred according to the present invention, when being filled with the mixed gas of argon gas and hydrogen in step (2) in Medium Frequency Induction Heating Furnace growth room, the volume ratio of argon gas and hydrogen is 5 ~ 9:1.The mixing of nitrogen when hydrogen is conducive to suppressing synthetic material is passed into while being filled with argon gas.
Preferred according to the present invention, described in step (2), the purity of argon gas, hydrogen is all greater than 99.9%.
Preferred according to the present invention, during high―temperature nuclei described in step (2), pass into circulating water in heating furnace chamber, to control temperature of reaction.
Preferred according to the present invention, the crucible material in step (2) is common graphite or high purity graphite.By prior art.
Preferred according to the present invention, increasing crucible described in step (2), is highly 400-800mm, can disposable synthesis 5-10kg powder.This crucible can repeatedly use.
In the present invention, the process furnace of employing is Medium Frequency Induction Heating Furnace.
Method of the present invention can prepared sizes 50-1000 μm of regulatable SiC powder, and especially the volume particle size SiC powder of more than 450 μm particle diameters compensate for the SiC powder particles of prior art synthesis deficiency less than normal.The particularly preferably volume particle size SiC powder of particle diameter 500-1000 μm.
The sic powder that the present invention obtains is applicable to the preparation of silicon carbide monocrystal growth and silicon carbide ceramics.
Excellent results of the present invention:
1, present method does not use high-purity carbon dust can realize the batch production of sic powder by high temperature process heat method, effectively can reduce the production cost of silicon carbide products.
2, present method synthesis temperature is low, lower than 1300 DEG C, takes full advantage of the mechanism of raw material self-propagating reaction heat release, has saved the step that high temperature more than 1500 DEG C makes grain growth, energy-conservation, and drop into equipment and relevant configuration and greatly reduce, processing step is simple.
3, the present invention adopts single sintering method, overcomes the shortcomings such as secondary synthesis complex procedures, length consuming time, artificial introducing impurity.Can the controlled sic powder of disposable synthesis granularity, the method cost is low, can disposable synthesis 5-10kg powder, can be mass.
4, can obtain volume particle size sic powder under low temperature of the present invention, when growing for SiC single crystal, under same crucible size, macrobead SiC powder is conducive to increasing charge amount, improves material utilization ratio, thus greatly improves SiC single crystal productive rate.
Accompanying drawing explanation
Fig. 1 is the XRD figure of synthesizing silicon carbide powder in embodiment 1.X-coordinate is 2 θ (°), and ordinate zou is intensity (a.u.).
Fig. 2 is the SEM figure of synthesizing silicon carbide powder in embodiment 1.Wherein, (B) figure is the partial enlarged drawing of (A) figure.
Fig. 3 increases plumbago crucible schematic diagram.Wherein, 1, crucible, 2, silica flour and carbon fiber mixing raw material.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, but be not limited thereto.
The raw materials used market that is of embodiment is bought, and the purity of high-purity carbon fiber and high-purity silicon powder is all greater than 99%, and the purity of argon gas, hydrogen is all greater than 99.9%.
Embodiment 1
Low cost low temperature prepares a method for carborundum powder, and concrete steps are as follows:
(1) prepare burden: raw material adopts high-purity carbon fiber and high-purity silicon powder, and the ratio of 1:1 mixes in molar ratio.Carbon fiber diameter 7 μm, length 1mm.Silicon particle size is 50 μm.
(2) synthesize: described silica flour and carbon fiber are put into highly be 400mm increase crucible, then Medium Frequency Induction Heating Furnace is placed in, vacuumize the growth room of process furnace, oxygen, nitrogen and water vapour etc. in removing growth room, be increased to 800 DEG C simultaneously by temperature; Then vacuumize, make vacuum tightness be less than 10
-3pa.In growth room, be filled with high-purity argon gas or argon gas and hydrogen volume than the mixed gas for 5:1, the purity of argon gas, hydrogen is all greater than 99.9%, and pressure is 800mbar, raised temperature to 1800 DEG C, generated time is 5 hours, is then down to room temperature, can obtain even-grained sic powder.
Adopt powder diffraction method (XRD) to carry out material phase analysis to synthetic product, obtain XRD figure as shown in Figure 1, can see that building-up reactions is complete, SEM figure shows even particle size distribution, and granularity is 50-100 μm, is suitable for silicon carbide monocrystal growth.
The purity of synthetic product sic powder is greater than 99%.
Crucible of increasing used is common graphite crucible, is of a size of 130mm × 130mm × 400mm, can disposable synthesis 5kg sic powder.
Embodiment 2
As described in Example 1, institute's difference is, carbon fiber diameter used 10 μm, length 100mm.Silicon particle size is 400 μm.By two kinds of raw materials in molar ratio 1:1 put into highly for 800mm increase crucible, be placed in Medium Frequency Induction Heating Furnace, the growth room of process furnace vacuumized, removing growth room in oxygen, nitrogen and water vapour etc., temperature is increased to 1300 DEG C simultaneously; Then vacuumize, make vacuum tightness be less than 10
-3pa.In growth room, be filled with the mixed gas of high-purity argon gas or argon gas and hydrogen, the purity of argon gas, hydrogen is all greater than 99.9%, and the volume ratio of argon gas and hydrogen is 9:1.Pressure is 900mbar, raised temperature to 2000 DEG C, and generated time is 20 hours.The crucible adopted is high purity graphite crucible, is of a size of 130mm × 130mm × 800mm, can disposable synthesis 10kg sic powder; Carborundum granularity is at 900-1000 μm; Purity is greater than 99%.
Embodiment 3
As described in Example 1, institute's difference is, carbon fiber diameter 9 μm, length 50mm.Silicon particle size is 200 μm.By two kinds of raw materials in molar ratio 1:1 put into highly for 640mm increase crucible, be placed in Medium Frequency Induction Heating Furnace, the growth room of process furnace vacuumized, removing growth room in oxygen, nitrogen and water vapour etc., temperature is increased to 1100 DEG C simultaneously; Then vacuumize, make vacuum tightness be less than 10
-3pa.In growth room, be filled with the mixed gas of high-purity argon gas or argon gas and hydrogen, the volume ratio of argon gas and hydrogen is 8:1.Pressure is 850mbar, raised temperature to 1900 DEG C, and generated time is 10 hours.The crucible adopted is high purity graphite crucible, is of a size of 130mm × 130mm × 640mm, can disposable synthesis 8kg sic powder.Carborundum granularity is at 500-600 μm; Purity is greater than 99%.
Claims (6)
1. a preparation method for carborundum powder, comprises the following steps:
(1) prepare burden:
Adopt high-purity carbon fiber and high-purity silicon powder to be raw material, the ratio of 1:1 mixes in molar ratio;
The purity of described high-purity carbon fiber and high-purity silicon powder raw material is all greater than 99%, carbon fiber diameter 7-10 μm, length 1-100mm, and silicon particle size is less than 500 μm;
(2) synthesize:
Described silica flour and carbon fiber are put into and increase crucible, be placed in Medium Frequency Induction Heating Furnace, process furnace growth room vacuumizes, and oxygen, nitrogen and water vapour in removing growth room, be increased to 500-1000 DEG C by temperature simultaneously; Then vacuumize, make vacuum tightness be less than 10
-3pa; In growth room, be filled with the mixed gas of argon gas or argon gas and hydrogen, pressure is 800-900mbar, and be warming up to 1000-1300 DEG C and synthesize, generated time is 5-10 hour, is then down to room temperature, can obtain the sic powder that epigranular is controlled.
2. the preparation method of carborundum powder as claimed in claim 1, when it is characterized in that being filled with the mixed gas of argon gas and hydrogen in step (2) in Medium Frequency Induction Heating Furnace growth room, the volume ratio of argon gas and hydrogen is 5 ~ 9:1.
3. the preparation method of carborundum powder as claimed in claim 1, is characterized in that the purity of argon gas, hydrogen described in step (2) is all greater than 99.9%.
4. the preparation method of carborundum powder as claimed in claim 1, when it is characterized in that the high―temperature nuclei described in step (2), passes into circulating water in heating furnace chamber.
5. the preparation method of carborundum powder as claimed in claim 1, is characterized in that the crucible material adopted in step (2) is common graphite or high purity graphite.
6. the preparation method of carborundum powder as claimed in claim 1, it is characterized in that increasing crucible described in step (2), is highly 400mm-800mm, disposable synthesis 5kg-10kg powder.
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| CN107324338A (en) * | 2017-07-24 | 2017-11-07 | 南京施密特光学仪器有限公司 | A kind of speculum silicon carbide powder and preparation method thereof |
| 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 |
| CN108130592A (en) * | 2017-11-14 | 2018-06-08 | 山东天岳先进材料科技有限公司 | A kind of preparation method of high-purity semi-insulating silicon carbide monocrystalline |
| CN108290796A (en) * | 2015-11-25 | 2018-07-17 | 日本碍子株式会社 | The manufacturing method of the ceramic structure of the method for replacing of non-active gas and the method for replacing of use non-active gas |
| 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 |
| CN109989103A (en) * | 2019-05-23 | 2019-07-09 | 广州南砂晶圆半导体技术有限公司 | A kind of method of circulating-heating synthesis bulky grain SiC powder |
| CN110203933A (en) * | 2019-04-28 | 2019-09-06 | 河北同光晶体有限公司 | A kind of method of nitrogen impurity content in reduction silicon carbide powder |
| RU2784758C1 (en) * | 2022-05-17 | 2022-11-29 | Федеральное государственное бюджетное учреждение науки Институт металлургии и материаловедения им. А.А. Байкова Российской академии наук (ИМЕТ РАН) | Method for producing highly dispersed silicon carbide powder |
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| 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 |
| CN108130592B (en) * | 2017-11-14 | 2019-11-12 | 山东天岳先进材料科技有限公司 | A kind of preparation method of high-purity semi-insulating silicon carbide monocrystalline |
| CN108130592A (en) * | 2017-11-14 | 2018-06-08 | 山东天岳先进材料科技有限公司 | A kind of preparation method of high-purity semi-insulating silicon carbide monocrystalline |
| CN110203933A (en) * | 2019-04-28 | 2019-09-06 | 河北同光晶体有限公司 | A kind of method of nitrogen impurity content in reduction silicon carbide powder |
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| CN109989103A (en) * | 2019-05-23 | 2019-07-09 | 广州南砂晶圆半导体技术有限公司 | A kind of method of circulating-heating synthesis bulky grain SiC powder |
| RU2784758C1 (en) * | 2022-05-17 | 2022-11-29 | Федеральное государственное бюджетное учреждение науки Институт металлургии и материаловедения им. А.А. Байкова Российской академии наук (ИМЕТ РАН) | Method for producing highly dispersed silicon carbide powder |
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