CN105417541A - Method for preparing high-purity silicon carbide powder - Google Patents
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Abstract
The invention discloses a method for preparing high-purity silicon carbide powder, and relates to a high-purity silicon carbide powder preparation method which realizes ultra-high purity SiC powder and is simple in working procedure. The method comprises the following steps: putting mixed raw materials in a high-purity graphite crucible, and putting the graphite crucible in a high-frequency sensing heating furnace; injecting high-purity H2 into a furnace cavity to 800 mbar when heating is not started, then maintaining the pressure at 800 mbar, and continuously charging H2 for 1 h; vacuumizing the equipment, so that the vacuum degree reaches 5x10<-6> mbar, then slowing warming until the temperature is slightly lower than 1000 DEG C, remaining for a certain period of time, so that the vacuum degree reaches 5x10<-6> mbar again; then slowly raising the temperature to 1000-1200 DEG C, and continuously carrying out a synthetic reaction for 10 h; at the temperature of 1200 DEG C, injecting high-purity H2 into the furnace cavity, maintaining the pressure at 800 mbar for 1 h, injecting high-purity Ar and H2 into the furnace cavity at the flow ratio of 10: 1, maintaining the pressure at 800 mbar, and then quickly warming until the temperature is 1900-2100 DEG C for carrying out a conversion synthetic reaction for 10 h. The purity of a synthetic environment is greatly improved.
Description
Technical field
The present invention relates to power electronics industry, field of semiconductor materials, especially single-crystal silicon carbide material, relate more specifically to a kind of high-pure SiC power preparation method for material for silicon carbide monocrystal growth.
Background technology
Power electronics is the important support technology in national economy and national security field, along with the fast development of information industry and the progress of microelectronics, new electronic component is to high pressure resistant, Large Copacity, high frequency, high reliability and highly integrated future development, SiC single crystal is as third generation wide bandgap semiconductor materials, there is broad stopband, high heat conductance, the saturated rate of migration of high electronics, the character such as high breakdown electric field, be considered to manufacture opto-electronic device, Deep trench termination, the semiconductor material that high-temperature electronic device is desirable, at white-light illuminating, optical storage, screen display, space flight and aviation, petroleum prospecting, automatization, radar and communications, the aspects such as automotive circuit diagram are widely used.Due to these excellent specific properties of silicon carbide, many countries all in succession drop into substantial contribution and further investigate it in recent years, and achieve breakthrough in growing silicon carbice crystals technology, Primary Component technique, photoelectric device exploitation, silicon carbide integrated circuit manufacture etc.The preparation of current SiC single crystal generally adopts PVT (physical vapor transport) method, and wherein the purity of SiC powder and other parameters play vital effect to the crystalline quality of the standby SiC single crystal of PVT legal system especially N-type and high purity semi-insulating single crystal and electrical properties.In general, the method for SiC powder synthesis mainly contains three kinds: Acheson method, organic synthesis method and self-propagating method.Acheson method is that SiO2 is reduced by C under high temperature, highfield effect, first generates β-SiC, is transformed into α-SiC under high temperature.The SiC powder of this method synthesis needs the operations such as pulverizing, pickling, and foreign matter content is higher, and its purity cannot reach the level of growing semiconductor monocrystalline.Organic synthesis method is mainly for the preparation of nano grade Sic powder, Determination of Multi-Impurities is had in the raw material of synthesis, although the very high high-purity alpha-SiC powder of purity can be obtained by subsequent disposal, but subsequent processes is complicated, difficulty collected by micro mist, is not suitable for a large amount of production and application, and easily produce harmful material, in addition, the SiC powder particles of this method synthesis is too little, can have a strong impact on the crystalline quality of SiC single crystal.Self-propagating high-temperature method be utilize substance reaction heat from conduction, make, between material, chemical reaction occurs, formed in very short time compound high―temperature nuclei reaction.Self-propagating method is the method that C powder Si powder directly contacts the generation SiC that reacts.Current the method has been widely used in high-purity alpha-SiC preparation.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.CN104828825A discloses the method with high-purity carbon fiber and high-purity Si powder low-temperature silicon carbide synthesization powder.CN103508454B discloses the method for three synthesis high-purity silicon carbide powders, and first at high temperature utilize the first synthesizing silicon carbide of high-purity C powder Si powder, after and then crushing, high temperature oxidation forms secondary silicon carbide, and final high temperature vacuum outgas, forms three sic powders.Three sic powders obtained also need through wet chemistry Metallurgical processing art breading.Finally obtain high-purity silicon carbide powder.CN102674357A discloses and utilizes high-purity C powder and Si powder first through pretreatment process, then by the method for high―temperature nuclei operation synthesis high-purity silicon carbide powder.Be high purity carbon material and the mixing of high-purity Si powder in the above existing method, and synthesize SiC powder in the gas mixture environment being full of rare gas element or rare gas element and reducing gas.Due to used high purity carbon material and high-purity Si Powder Particle Size little, mutual gap is little, after crucible is put in mixing, the gas of raw material inside is difficult to be taken away completely under vacuo, in addition, although due to selected rare gas element and reducing gas purity very high, but, still containing a small amount of foreign gas, therefore, select under the gas mixture environment being full of rare gas element or rare gas element and reducing gas during synthesizing silicon carbide powder, foreign gas element can be mixed in C, Si reaction process, thus the purity of impact synthesis SiC powder.In addition, patent CN101302011A and CN103508454B discloses the method for secondary synthesis and three synthesis SiC powders, Purity of Coke Powder can be improved although it is so, but complex procedures, add preparation cost, although and patent CN104828825A adopts low temperature method synthesis SiC powder to save cost, this method can only synthesizing β-SiC (3C phase SiC), synthesis powder thing is mutually single, to the selection of powder crystal formation when being difficult to meet growing silicon carbide single crystal.
Summary of the invention
The present invention is directed to the deficiency that prior art synthesizing silicon carbide powder exists, provide one and can realize ultra-high purity SiC powder and the simple high-pure SiC power preparation method for material of operation.
The present invention solves above technical problem by the following technical programs:
A method prepared by high-purity silicon carbide powder, comprises the following steps:
The first step, selection high purity graphite powder (purity > 99.999%) carry out Homogeneous phase mixing with high-purity Si powder (purity 99.999%) with mol ratio 1:1.02;
Second step, selection polytetrafluoroethylene powder (purity > 99.999%) mix with mass ratio 1:100 with mixed raw material, and described (1) and (2) can be carried out simultaneously;
3rd step, the raw material mixed is placed in high purity graphite crucible, plumbago crucible is placed in Medium Frequency Induction Heating Furnace; In furnace chamber, injecting high-purity H2 to 800mbar when not starting to heat, then keeping pressure 800mbar, and keeping H2 to continue to be filled with 1 hour;
4th step, equipment to be vacuumized, make vacuum tightness reach 5 × 10-6mbar, be slowly warming up to a little less than 1000 DEG C subsequently, stop certain hour, make vacuum tightness again reach 5 × 10-6mbar.And then be slowly warming up to 1000 DEG C-1200 DEG C, carry out building-up reactions, generated time continues 10h;
After 5th step, above-mentioned reaction, at 1200 DEG C, high-purity H2 is injected furnace chamber, keep pressure at 800mbar, keep 1h, high-purity Ar and H2 are injected furnace chamber with throughput ratio 10:1, keep pressure at 800mbar, then be rapidly heated to 1900 DEG C-2100 DEG C and carry out Synthesis reaction, generated time continues 10h;
6th step, at the protection borehole cooling of Ar and H2 to room temperature.
After building-up reactions terminates, breaking of vacuum temperature, to room temperature, can obtain high-purity β-SiC powder; And then carry out subsequent step after building-up reactions terminates and then can obtain high-purity α-SiC powder.
Gained Purity of Coke Powder is very high, meets high-purity semi-insulating silicon carbide single crystal growing demand completely, and present method technique is simple, is suitable for producing in enormous quantities.The first all-pass H2 to 800mbar when not heating, then pressure 800mbar is kept, and keep H2 to continue to be filled with 1 hour, when selecting not heat, all-pass H2 is because its molecular volume is little, can effectively infiltrate raw material gap, thus the air particularly nitrogen can effectively discharged between raw material accumulation inside and gap, greatly improve the purity of synthetic environment.Add tetrafluoroethylene in high-purity silicon carbide powder synthesis technique, because tetrafluoroethylene is heated can be analyzed to gas, decomposition temperature lower than the synthesis temperature of SiC, and can not pollute raw material after decomposing.When tetrafluoroethylene decomposes becomes gas, space can be formed in the raw material inside of piling up, can farthest make like this air of accumulation raw material inside particularly nitrogen detached chamber by vacuum pump, greatly improve the purity of powder synthetic environment.Synthesizing β-SiC under vacuum environment; The self-propagating synthesis sic powder method in the past reported is synthesizes β or α-SiC powder under chamber is full of inert gas environment, because used rare gas element has certain impurity, will certainly affect the purity of synthesis SiC powder like this.We find that α-SiC is high due to synthesis temperature, are much higher than the volatilization temperature of Si, therefore, cannot synthesize under high vacuum environment.But the synthesis temperature of β-SiC is significantly less than the volatilization temperature of Si, can synthesize under high vacuum environment completely, and don't as causing Si to volatilize.Therefore, we select synthesizing β-SiC under high vacuum environment, and the purity of synthesis is very high.First synthesizing β-SiC under a high vacuum, then α-SiC is grown under 800mbar pressure; The purity that α-SiC effectively can improve α-SiC is synthesized on the basis of synthesizing β-SiC under vacuo.Because α-SiC is transformed along with temperature raises by β-SiC, therefore, the purity of β-SiC determines the degree of α-SiC to a certain extent.In addition, in the process that β-SiC transforms to α-SiC, the carrier gas of certain pressure must being passed into, prevent SiC from decomposing, in order to ensure the purity of SiC powder, generally selecting argon gas and hydrogen as carrier gas.Logical H2 ratio first leads to 100%, and then Ar and the H2 of logical 10:1, after selecting β-SiC end of synthesis, first all-pass H2 at 1200 DEG C, and then Ar and the H2 of logical 10:1 is because under hot environment, H2 too high levels can be incubated with graphite reacts with plumbago crucible, thus causes the consumption of graphite piece.
Embodiment
The present invention is described in detail below:
A method prepared by high-purity silicon carbide powder, comprises the following steps:
The first step, selection high purity graphite powder (purity > 99.999%) carry out Homogeneous phase mixing with high-purity Si powder (purity 99.999%) with mol ratio 1:1.02;
Second step, selection polytetrafluoroethylene powder (purity > 99.999%) mix with mass ratio 1:100 with mixed raw material, and described (1) and (2) can be carried out simultaneously;
3rd step, the raw material mixed is placed in high purity graphite crucible, plumbago crucible is placed in Medium Frequency Induction Heating Furnace; In furnace chamber, injecting high-purity H2 to 800mbar when not starting to heat, then keeping pressure 800mbar, and keeping H2 to continue to be filled with 1 hour;
4th step, equipment to be vacuumized, make vacuum tightness reach 5 × 10-6mbar, be slowly warming up to a little less than 1000 DEG C subsequently, stop certain hour, make vacuum tightness again reach 5 × 10-6mbar.And then be slowly warming up to 1000 DEG C-1200 DEG C, carry out building-up reactions, generated time continues 10h;
After 5th step, above-mentioned reaction, at 1200 DEG C, high-purity H2 is injected furnace chamber, keep pressure at 800mbar, keep 1h, high-purity Ar and H2 are injected furnace chamber with throughput ratio 10:1, keep pressure at 800mbar, then be rapidly heated to 1900 DEG C-2100 DEG C and carry out Synthesis reaction, generated time continues 10h;
6th step, at the protection borehole cooling of Ar and H2 to room temperature.
Example 1 high-purity β-SiC synthesis technique
With high purity graphite powder (purity > 99.999%) and high-purity Si powder (purity > 99.999%) for raw material, tetrafluoroethylene is additive, high purity graphite powder and high-purity Si powder carry out Homogeneous phase mixing according to mol ratio 1:1.02, and tetrafluoroethylene and mixed raw material add according to mass ratio 1:100.Raw material after proportioning is placed in high purity graphite crucible (purity > 99.9995%), plumbago crucible and graphite is incubated and is placed in Medium Frequency Induction Heating Furnace and heats.First before heating, in furnace chamber, inject high-purity H2 (purity > 99.999%) to 800mbar, then keep pressure 800mbar, and keep H2 to continue to be filled with 1 hour.Then equipment is vacuumized, make vacuum tightness reach 5 × 10-6mbar, be slowly warming up to a little less than 1000 DEG C subsequently, stop certain hour, make vacuum tightness again reach 5 × 10-6mbar.And then be warming up to 1000 DEG C-1200 DEG C (this temperature range be C, Si react synthesis SiC scope, in this interval, along with the rising of synthesis temperature, the SiC granularity of synthesis will increase thereupon.Therefore, a temperature value can be preset according to experiment demand) stop 10h.Be cooled to room temperature under a high vacuum subsequently.Compound experiment terminates.
Example 2 high-purity α-SiC synthesis technique
With high purity graphite powder (purity > 99.999%) and high-purity Si powder (purity > 99.999%) for raw material, tetrafluoroethylene is additive, high purity graphite powder and high-purity Si powder carry out Homogeneous phase mixing according to mol ratio 1:1.02, and tetrafluoroethylene and mixed raw material add according to mass ratio 1:100.Raw material after proportioning is placed in high purity graphite crucible (purity > 99.9995%), plumbago crucible and graphite is incubated and is placed in Medium Frequency Induction Heating Furnace and heats.First before heating, in furnace chamber, inject high-purity H2 (purity > 99.999%) to 800mbar, then keep pressure 800mbar, and keep H2 to continue to be filled with 1 hour.Then equipment is vacuumized, make vacuum tightness reach 5 × 10-6mbar, be slowly warming up to a little less than 1000 DEG C subsequently, stop certain hour, make vacuum tightness again reach 5 × 10-6mbar.And then be warming up to 1000 DEG C-1200 DEG C, stop 10h.Now, C, Si complete reaction generation β-SiC.Subsequently, at 1200 DEG C, high-purity H2 is injected furnace chamber, keeps pressure at 800mbar, keep 1h, then Ar and H2 is continued to inject furnace chamber according to throughput ratio 10:1, make furnace chamber pressure remain on 800mbar, being rapidly heated to 1900 DEG C-2100 DEG C, (this temperature range is the scope that β-SiC starts to be converted into α-SiC, in this interval, along with the rising of temperature, the α-SiC granularity be transformed will increase thereupon.Therefore, a temperature value can be preset according to experiment demand) keep 10h.Subsequently at the protection borehole cooling of Ar and H2 to room temperature, compound experiment terminates.
Claims (2)
1. the method prepared of high-purity silicon carbide powder, comprises the following steps:
The first step, selection high purity graphite powder (purity > 99.999%) carry out Homogeneous phase mixing with high-purity Si powder (purity 99.999%) with mol ratio 1:1.02;
Second step, selection polytetrafluoroethylene powder (purity > 99.999%) mix with mass ratio 1:100 with mixed raw material, and described (1) and (2) can be carried out simultaneously;
3rd step, the raw material mixed is placed in high purity graphite crucible, plumbago crucible is placed in Medium Frequency Induction Heating Furnace; In furnace chamber, injecting high-purity H2 to 800mbar when not starting to heat, then keeping pressure 800mbar, and keeping H2 to continue to be filled with 1 hour;
4th step, equipment to be vacuumized, make vacuum tightness reach 5 × 10-6mbar, be slowly warming up to a little less than 1000 DEG C subsequently, stop certain hour, make vacuum tightness again reach 5 × 10-6mbar.
2. be and then slowly warming up to 1000 DEG C-1200 DEG C, carry out building-up reactions, generated time continues 10h;
After 5th step, above-mentioned reaction, at 1200 DEG C, high-purity H2 is injected furnace chamber, keep pressure at 800mbar, keep 1h, high-purity Ar and H2 are injected furnace chamber with throughput ratio 10:1, keep pressure at 800mbar, then be rapidly heated to 1900 DEG C-2100 DEG C and carry out Synthesis reaction, generated time continues 10h;
6th step, at the protection borehole cooling of Ar and H2 to room temperature.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108083281A (en) * | 2017-12-27 | 2018-05-29 | 江苏乐园新材料集团有限公司 | A kind of protective layer metamorphosis formula carbonization silicon preparation method |
| CN108483447A (en) * | 2018-04-28 | 2018-09-04 | 北京科技大学 | A kind of preparation method of micro/nano level spherical carbide silicon materials |
| CN109987606A (en) * | 2019-05-13 | 2019-07-09 | 穆建东 | It is a kind of to utilize silicon powder and high purity graphite powder synthesizing β-SiC technique for producing miropowder |
| CN111484019A (en) * | 2020-04-27 | 2020-08-04 | 山西烁科晶体有限公司 | Preparation method of high-purity silicon carbide powder for single crystal growth |
| CN113371712A (en) * | 2021-07-27 | 2021-09-10 | 北京天科合达半导体股份有限公司 | Preparation method of silicon carbide powder with low nitrogen content and silicon carbide single crystal |
| CN113479889A (en) * | 2021-08-20 | 2021-10-08 | 中电化合物半导体有限公司 | Synthesis method of 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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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108083281A (en) * | 2017-12-27 | 2018-05-29 | 江苏乐园新材料集团有限公司 | A kind of protective layer metamorphosis formula carbonization silicon preparation method |
| CN108483447A (en) * | 2018-04-28 | 2018-09-04 | 北京科技大学 | A kind of preparation method of micro/nano level spherical carbide silicon materials |
| CN109987606A (en) * | 2019-05-13 | 2019-07-09 | 穆建东 | It is a kind of to utilize silicon powder and high purity graphite powder synthesizing β-SiC technique for producing miropowder |
| CN111484019A (en) * | 2020-04-27 | 2020-08-04 | 山西烁科晶体有限公司 | Preparation method of high-purity silicon carbide powder for single crystal growth |
| CN113371712A (en) * | 2021-07-27 | 2021-09-10 | 北京天科合达半导体股份有限公司 | Preparation method of silicon carbide powder with low nitrogen content and silicon carbide single crystal |
| CN113479889A (en) * | 2021-08-20 | 2021-10-08 | 中电化合物半导体有限公司 | Synthesis method of silicon carbide powder |
| CN113479889B (en) * | 2021-08-20 | 2022-12-09 | 中电化合物半导体有限公司 | Synthesis method of 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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Application publication date: 20160323 |