CN104401995A - Method using polysilicon block and flake graphite for preparation of high purity silicon carbide powder - Google Patents
Method using polysilicon block and flake graphite for preparation of high purity silicon carbide powder Download PDFInfo
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- CN104401995A CN104401995A CN201410570173.7A CN201410570173A CN104401995A CN 104401995 A CN104401995 A CN 104401995A CN 201410570173 A CN201410570173 A CN 201410570173A CN 104401995 A CN104401995 A CN 104401995A
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- polysilicon block
- flake graphite
- silicon carbide
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- crystalline flake
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Abstract
The invention relates to a method using a polysilicon block and flake graphite for preparation of high purity silicon carbide powder. The method is as follows: (1) according to the mass ratio, putting the polysilicon block on the bottom of a graphite crucible, and evenly spreading the flake graphite on the polysilicon block; (2) putting the crucible in aninduction furnace for vacuumizing for 4-10 hours; (3) rising the temperature to 1300-1600 DEG C, and keeping warm for 2-4 hours under the conditions of argon flow rate of 0.1-5L / min, hydrogen flow rate of 0-1L / min and the pressure of 3-20mbar; (4) rising the temperature to 1800 to 2300 DEG C at the heating rate of 10-30 DEG C / min, and keeping warm for 2-10 hours; and (5) taking silicon carbide powder for grinding in a graphite mortar to obtain the high purity silicon carbide powder. The high purity silicon carbide powder prepared by the method is light yellow or yellow-black, and the silicon carbide content is no less than 99.9%. The method has the advantages of simple process, low production cost, short production cycle and high purity of SiC powder.
Description
Technical field
The present invention relates to the method for synthesizing silicon carbide powder, be specifically related to a kind of method utilizing polysilicon block and crystalline flake graphite to prepare high-pure SiC power.
Background technology
Silicon carbide (SiC) material is a kind of novel semiconductor material, belongs to third generation semiconductor material.It has the features such as broad-band gap, high heat conductance, high critical breakdown electric field, the saturated drift of high carrier, and the application potential in high temperature, high-power, high frequency, photoelectron and radioprotective etc. is larger.
Typical SiC crystal structure is generally divided into two large classes: a class is cube SiC crystal formation of the zincblende lattce structure being called 3C or β-SiC, another kind of is be called the hexangle type of a-SiC or the large period structure of diamond structure, and typical crystal formation has 6H-SiC, 4H-SiC, 15R-SiC etc.Because the bond energy of β-SiC is minimum, lattice free energy is maximum, therefore its also the easiest nucleation, and the temperature required for growth is also relatively minimum.Chemically in nature, because spacing is substantially equal between carbon silicon stack lamination, different SiC polytype is identical in the lattice arrangement in the double-deck solid matter face of S1-C, so the chemical property that they have is substantially identical; And for physical properties, owing to having very high energy barrier between these homogeneity polytypes, therefore, even if when basal component is identical, the physical properties between them, particularly characteristic of semiconductor is also different.In addition, β-SiC is one of the hardest high performance material being only second to diamond, and its ultrahigh hardness and density make it can be ideally suited for standing the parts of high wearing and tearing and skimming wear, are applicable to various grinding, especially ultraprecision grinding.
Carbothermic reduction reaction is one of main method of current synthesizing silicon carbide powder, is called Acheson method in industrial production.Traditional method adopts quartz sand, silicon-dioxide powdery, silica flour as silicon source; Graphite, carbon dust and some are as blue or green as carbon source in starch, resol, Zhejiang containing carbon macromolecule.In recent years in order to obtain the silicon carbide powder of different-shape, also have and adopt the resinous material with fibrous texture as carbon source, can find out, the own foreign matter content in silicon source used in the method is many, be unfavorable for obtaining the higher product of purity, the carbon source used is also very limited.Therefore exist silicon source foreign matter content high, react insufficient, the problem such as SiC content is low.
Summary of the invention
The present invention is directed to prior art Problems existing, propose a kind of method utilizing polysilicon block and crystalline flake graphite to prepare high-pure SiC power.
The present invention is achieved through the following technical solutions: a kind of method utilizing polysilicon block and crystalline flake graphite to prepare high-pure SiC power, is characterized in that: comprise the steps:
Step one. by crystalline flake graphite and polysilicon block in mass ratio for 1:2-1:2.5 loads in plumbago crucible, polysilicon block is placed in plumbago crucible bottom, then crystalline flake graphite uniform spreading is dispersed in above polysilicon block;
Step 2. the plumbago crucible that crystalline flake graphite and polysilicon block are housed is put into induction furnace, vacuumizes 4-10 hour, vacuum tightness reaches 10
-5mbar;
Step 3. temperature is risen to 1300-1600 DEG C rapidly, is filled with the mixed gas of argon gas or argon gas and hydrogen, argon flow amount is 0.1-5L/min, and hydrogen flowing quantity is 0-1L/min, and pressure is 3-20mbar, and is incubated 2-4 hour;
Step 4. temperature is risen to 1800-2300 DEG C rapidly, and temperature rise rate is 10-30 DEG C/min, insulation 2-10 hour;
Step 5. take out synthetic carborundum powder and pulverize in graphite mortar, namely obtain high-pure SiC power.
The invention has the beneficial effects as follows: the high-purity alpha-SiC powder utilizing the method to prepare is faint yellow or yellow black powder, and the content of silicon carbide is not less than 99.9%.Present irregular grain shape under an optical microscope.The method has that technique is simple, production cost is low, with short production cycle and SiC powder purity high.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1: a kind of its step of method utilizing polysilicon block and crystalline flake graphite to prepare high-pure SiC power is as follows:
(1) load in plumbago crucible after crystalline flake graphite 150g and polysilicon block 350g being mixed, polysilicon block is placed in plumbago crucible bottom, then crystalline flake graphite uniform spreading is dispersed in above polysilicon block.
(2) plumbago crucible that crystalline flake graphite and polysilicon block are housed is put into induction furnace, vacuumize 5 hours, vacuum tightness reaches 10
-5mbar.
(3) temperature is raised to rapidly 1300 DEG C, is filled with argon gas, argon flow amount is 3L/min, and pressure is 5mbar, and is incubated 2 hours.
(4) temperature is risen to rapidly 1800 DEG C, temperature rise rate is 30 DEG C/min, is incubated 10 hours.
(5) take out synthetic carborundum powder to pulverize in graphite mortar, namely obtain high-pure SiC power.
Embodiment 2: a kind of its step of method utilizing polysilicon block and crystalline flake graphite to prepare high-pure SiC power is as follows:
(1) load in plumbago crucible after crystalline flake graphite 160g and polysilicon block 350g being mixed, polysilicon block is placed in plumbago crucible bottom, then crystalline flake graphite uniform spreading is dispersed in above polysilicon block.
(2) plumbago crucible that crystalline flake graphite and polysilicon block are housed is put into induction furnace, vacuumize 5 hours, vacuum tightness reaches 10
-5mbar.
(3) temperature is raised to rapidly 1500 DEG C, is filled with argon gas and hydrogen gas mixture, argon flow amount is 3L/min, and hydrogen flowing quantity is 0.2L/min, and pressure is 10mbar, and is incubated 2 hours.
(4) temperature is risen to rapidly 2000 DEG C, temperature rise rate is 30 DEG C/min, is incubated 7 hours.
(5) take out synthetic carborundum powder to pulverize in graphite mortar, namely obtain high-pure SiC power.
Embodiment 3: a kind of its step of method utilizing polysilicon block and crystalline flake graphite to prepare high-pure SiC power is as follows:
(1) load in plumbago crucible after crystalline flake graphite 165g and polysilicon block 350g being mixed, polysilicon block is placed in plumbago crucible bottom, then crystalline flake graphite uniform spreading is dispersed in above polysilicon.
(2) plumbago crucible that crystalline flake graphite and polysilicon block are housed is put into induction furnace, vacuumize 5 hours, vacuum tightness reaches 10
-5mbar.
(3) temperature is raised to rapidly 1600 DEG C, is filled with argon gas and hydrogen gas mixture, argon flow amount is 2L/min, and hydrogen flowing quantity is 0.5L/min, and pressure is 20mbar, and is incubated 2 hours.
(4) temperature is risen to rapidly 2300 DEG C, temperature rise rate is 20 DEG C/min, is incubated 5 hours.
(5) take out synthetic carborundum powder to pulverize in graphite mortar, namely obtain high-pure SiC power.
The present invention passes through above-described embodiment, plumbago crucible bottom is placed in by polysilicon block, then crystalline flake graphite uniform spreading is dispersed in above polysilicon, when temperature reaches temperature of reaction, Formed SiClx after the Si atmosphere that polysilicon produces starts and crystalline flake graphite above reacts.Carborundum grain increases along with the raising of temperature of reaction and the increase of soaking time.Finally obtain the carborundum powder that content is not less than 99.9%.
Claims (1)
1. utilize polysilicon block and crystalline flake graphite to prepare a method for high-pure SiC power, it is characterized in that:
Its step is as follows:
Step one. by crystalline flake graphite and polysilicon block in mass ratio for 1:2-1:2.5 loads in plumbago crucible, polysilicon block is placed in plumbago crucible bottom, then crystalline flake graphite uniform spreading is dispersed in above polysilicon block;
Step 2. the plumbago crucible that crystalline flake graphite and polysilicon block are housed is put into induction furnace, vacuumizes 4-10 hour, vacuum tightness reaches 10
-5mbar;
Step 3. temperature is risen to 1300-1600 DEG C rapidly, is filled with the mixed gas of argon gas or argon gas and hydrogen, argon flow amount is 0.1-5L/min, and hydrogen flowing quantity is 0-1L/min, and pressure is 3-20mbar, and is incubated 2-4 hour;
Step 4. temperature is risen to 1800-2300 DEG C rapidly, and temperature rise rate is 10-30 DEG C/min, insulation 2-10 hour;
Step 5. take out synthetic carborundum powder and pulverize in graphite mortar, namely obtain high-pure SiC power.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410570173.7A CN104401995A (en) | 2014-10-23 | 2014-10-23 | Method using polysilicon block and flake graphite for preparation of high purity silicon carbide powder |
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|---|---|---|---|
| CN201410570173.7A CN104401995A (en) | 2014-10-23 | 2014-10-23 | Method using polysilicon block and flake graphite for preparation of high purity silicon carbide powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106479601A (en) * | 2016-10-10 | 2017-03-08 | 北京三联创业科技发展有限公司 | The technique for preparing internal combustion engine moving sealing silicon-carbon crystallite composite |
| CN107640773A (en) * | 2017-10-30 | 2018-01-30 | 中国电子科技集团公司第四十六研究所 | A kind of method for directly synthesizing bulky grain carborundum powder |
Citations (5)
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| JPH06298514A (en) * | 1993-04-09 | 1994-10-25 | Sanyo Electric Co Ltd | Production of highly pure silicon carbide |
| CN102674357A (en) * | 2012-05-29 | 2012-09-19 | 上海硅酸盐研究所中试基地 | Method for synthesizing high-purity silicon carbide raw material for growing silicon carbide single crystals |
| 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 |
| CN102730687A (en) * | 2012-07-05 | 2012-10-17 | 浙江理工大学 | Preparation method of SiC nanowire with expandable graphite as carbon source |
| CN103708463A (en) * | 2013-10-25 | 2014-04-09 | 北京华进创威电子有限公司 | Preparation method of kilogram-grade high-purity silicon carbide powder |
-
2014
- 2014-10-23 CN CN201410570173.7A patent/CN104401995A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06298514A (en) * | 1993-04-09 | 1994-10-25 | Sanyo Electric Co Ltd | Production of highly pure silicon carbide |
| CN102674357A (en) * | 2012-05-29 | 2012-09-19 | 上海硅酸盐研究所中试基地 | Method for synthesizing high-purity silicon carbide raw material for growing silicon carbide single crystals |
| 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 |
| CN102730687A (en) * | 2012-07-05 | 2012-10-17 | 浙江理工大学 | Preparation method of SiC nanowire with expandable graphite as carbon source |
| CN103708463A (en) * | 2013-10-25 | 2014-04-09 | 北京华进创威电子有限公司 | Preparation method of kilogram-grade high-purity silicon carbide powder |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106479601A (en) * | 2016-10-10 | 2017-03-08 | 北京三联创业科技发展有限公司 | The technique for preparing internal combustion engine moving sealing silicon-carbon crystallite composite |
| CN107640773A (en) * | 2017-10-30 | 2018-01-30 | 中国电子科技集团公司第四十六研究所 | A kind of method for directly synthesizing bulky grain carborundum powder |
| CN107640773B (en) * | 2017-10-30 | 2020-06-02 | 中国电子科技集团公司第四十六研究所 | Method for directly synthesizing large-particle silicon carbide powder |
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Application publication date: 20150311 |