CN100415644C - Industrial preparation method for silica carbide crystal whisker and micropowder - Google Patents
Industrial preparation method for silica carbide crystal whisker and micropowder Download PDFInfo
- Publication number
- CN100415644C CN100415644C CNB031146724A CN03114672A CN100415644C CN 100415644 C CN100415644 C CN 100415644C CN B031146724 A CNB031146724 A CN B031146724A CN 03114672 A CN03114672 A CN 03114672A CN 100415644 C CN100415644 C CN 100415644C
- Authority
- CN
- China
- Prior art keywords
- industrial
- silicon carbide
- raw material
- carbide whisker
- micro mist
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 13
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000013078 crystal Substances 0.000 title abstract 3
- 239000000377 silicon dioxide Substances 0.000 title description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical class [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 239000010439 graphite Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 15
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000003723 Smelting Methods 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- 239000003595 mist Substances 0.000 claims description 11
- 239000003245 coal Substances 0.000 claims description 6
- 238000009776 industrial production Methods 0.000 claims description 6
- 239000000571 coke Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000003786 synthesis reaction Methods 0.000 claims description 4
- 239000006004 Quartz sand Substances 0.000 claims description 3
- 239000002802 bituminous coal Substances 0.000 claims description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 238000013467 fragmentation Methods 0.000 claims description 2
- 238000006062 fragmentation reaction Methods 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- -1 vitriol Chemical compound 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 16
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 239000000203 mixture Substances 0.000 abstract description 3
- 230000001788 irregular Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 240000003936 Plumbago auriculata Species 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005261 decarburization Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 208000030208 low-grade fever Diseases 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to a method for preparing silicon carbide whiskers and miropowder in industry. The method comprises the steps: mixing graphite with other industrial carbonaceous raw material and siliceous raw material, loading the mixture into an industrial SiC smelting furnace for synthetic reaction, and using the graphite as a conductive heating body to prepare silicon carbide whiskers and miropowder. The method has abundant and cheap material source, is simple in production process and is suitable for mass industrialized production. The crystal whisker prepared by the method has uniform diameter, large length-to-diameter ratio and few crystals in an irregular shape. Therefore, the method has the characteristics of simple preparation process, little equipment investment, low production cost and good product quality.
Description
Technical field
The present invention relates to a kind of silicon carbide whisker and micropowder preparing process, relate in particular to the method for a kind of industrial preparation silicon carbide whisker and micro mist.
Background technology
Premium propertiess such as silicon carbide whisker and micro mist have high-melting-point, high strength, high-modulus, coefficient of thermal expansion is low and corrosion-resistant, wear-resisting, senior raw material as the strengthening and toughening agent of matrix materials such as metal matrix, ceramic base and structural ceramics, high grade refractory, coated material is widely used in fields such as machinery, electronics, aerospace and the energy.But in the prior preparation method, as domestic frequent employing be the acid treatment carbonization rice husk, add SiO
2Adjust raw material, and add composite catalyst and pack in the plumbago crucible, put into High Temperature Furnaces Heating Apparatus, feed protective gas Ar gas, under high temperature, carry out carbothermic reduction reaction and prepare silicon carbide whisker; Patent of invention " a kind of preparation method of nanometer silicon carbide whiskers " (application number 99110846.9) then adopts another kind of method: carbonaceous and siliceous clean raw material are made colloidal sol, thorough mixing, drying make the binary xerogel and place plumbago crucible in proportion, put into High Temperature Furnaces Heating Apparatus, feed argon gas, carry out carbothermic reduction reaction at 1300-1600 ℃, make silicon carbide whisker.All there is following defective in above-mentioned two kinds of methods: 1, material purity and cost height; 2, the High Temperature Furnaces Heating Apparatus complex structure that uses in the production, the cost height; 3, complex manufacturing, synthetic difficulty are big; 4, high-temperature heating process belongs to the raw material indirect heating, and it is inhomogeneous therefore to be heated, and heat-up time is short, and the abnormity of generation is brilliant more; 5, owing to above reason causes its production cost height, output little, be difficult to mass industrialized production.
Summary of the invention
For overcoming above-mentioned defective, but the object of the present invention is to provide that a kind of production cost is low, the simple mass industrialized production silicon carbide whisker of production technique and micropowder preparing process.The diameter of whiskers that this method is produced is even, and length-to-diameter ratio is big, good product quality.
The present invention realizes with following method for achieving the above object: (1) with graphite and other industrial carbonaceous and siliceous raw material fragmentation after thorough mixing, the ratio range of its carbon raw material gross weight and siliceous raw material gross weight is: 1: 1.1-2.5; (2) reaction material that mixes is packed into carry out building-up reactions in the industrial SiC smelting furnace, its smelting furnace adopts and becomes power or the power supply of permanent power, and make conductive heating unit with graphite this moment, extinguishes until the body of heater flare, and building-up reactions finishes to close stove; (3) silicon carbide whisker for preparing and micro mist are come out of the stove back purifying.
The industrial carbon raw material that uses in preparation process comprises one or more mixing in hard coal, bituminous coal, graphite, carbon black or the refinery coke; Industrial siliceous raw material comprises that in quartz sand, Pure Silicon Metal or the organosilicon one or more mix.The reaction material that mixes can be added catalyzer when synthetic going into stove, also can not add, and catalyzer can be the single or two or more combinations of sodium salt, vitriol, silicate, metal oxide during interpolation, and even with the reaction material thorough mixing.
The CO (carbon monoxide converter) gas that produces in the building-up reactions in the above-mentioned steps (2) can be used as shielding gas, need not to add argon gas again, and its synthesis temperature is 1400-2000 ℃, and reaction times 2-60 hour, the building-up reactions equation was: SiO
2+ 3C=SiC+2CO ↑.
After building-up reactions in the stove finished, the silicon carbide whisker product for preparing can adopt decarburization, takes off silicon-dioxide, the chemical treatment method purifying of deferrization.
The present invention compared with prior art adopts the production of industrial raw material and SIC industry smelting furnace, and its raw material sources are abundant cheap, and synthetic furnace is simple in structure, can realize industrialized mass; The alternative argon gas of CO gas that produces in the building-up process is as shielding gas; simultaneously, production process adopts graphite to make the heat conduction heating element, and the inner unlimited low-grade fever source of raw material evenly generates heat in the stove; its generated time is long, thus even, the special-shaped crystalline substance of product diameter less, length-to-diameter ratio is big.Therefore, the present invention have that preparation technology is simple, facility investment is little, production cost is low, product diameter quotient height, the measured characteristics of matter.
Embodiment
Embodiment 1:(1) refinery coke of fixed carbon content 90%, the ash content of coal 0.2%, volatile content 8.7% and the graphite of carbon containing 98% are broken into 1MM with interior powder, with S
iO
2The quartz sand of content 99.3% is broken into 1.5MM with interior powder; Press C: S
iO
2=0.56: 1 ratio with carrying out thorough mixing after the two class powder proportionings, becomes reaction material.(2) 0.05% cobalt chloride with 0.15% sodium-chlor of reaction material amount and reaction material amount adds in the reaction material as catalyzer, and thorough mixing is even.(3) the above-mentioned reaction material of getting ready is packed into industrial SIC smelting furnace adopts permanent power power supply to smelt, and this moment, synthesis reaction temperature was 1400 ℃, and in about 2 hours of reaction times, the CO that produces in synthetic can play shielding gas, and the body of heater flare extinguishes the back and closes stove.Purifying after the mixture primary products of silicon carbide whisker that (4) prepares and differential are come out of the stove.
Embodiment 2:(1) hard coal of fixed carbon content 88%, the ash content of coal 3%, volatile content 6% and the graphite of carbon containing 98% are broken for the 0-1.5MM particulate, with S
iO
2The silica of content 99.3% is broken for the particulate of 0-2.0MM, two class raw materials is pressed C: S
iO
2=0.6: 1 ratio batching, and carry out thorough mixing.(2) 0.1% 0.2% the salt that mills English sand and dosage with dosage adds in the above-mentioned batching as catalyzer, and thorough mixing is even.(3) reaction material of getting ready is packed in the compound electrode multicore SIC smelting furnace, adopt permanent power power supply, graphite heating in the stove; this moment, synthesis reaction temperature was 1800 ℃; about 30 hours reaction times, the synthetic middle CO that produces plays shielding gas, and the body of heater flare extinguishes the back and closes stove.(4) product that makes is elementary silicon carbide whisker and the micro mist of content 40-50%, with the primary products purifying of coming out of the stove.
Embodiment 3: the bituminous coal coke of fixed carbon content 89%, the ash content of coal 4.6%, volatile content 5% and the graphite of industrial carbon containing 99% are broken for the 0-0.5MM particulate, with S
iO
2The silica sand of content 99% is broken for the particulate of 0-0.5MM, two class raw materials is pressed C: S
iO
2=0.7: 1.0 ratio batching, and carry out thorough mixing.(2) reaction material of getting ready is packed in the compound electrode multicore SIC smelting furnace, adopt permanent power power supply, graphite heating in the stove; this moment, temperature of reaction was 2000 ℃; about 60 hours of synthesising reacting time, the CO that produces in the building-up process can play shielding gas, and flare extinguishes the pass stove in stove.(3) product that makes is the elementary silicon carbide whisker and the differential of content about 50%, with the primary products purifying of coming out of the stove.
Claims (5)
1. the industrial production process of silicon carbide whisker and micro mist is characterized in that concrete steps are as follows:
(1) with thorough mixing after graphite and other industrial carbonaceous and the siliceous raw material fragmentation, the ratio range of its carbon raw material gross weight and siliceous raw material gross weight is: 1: 1.1-2.5; (2) reaction material that mixes is packed into carry out building-up reactions in the industrial SiC smelting furnace, its smelting furnace adopts and becomes power or the power supply of permanent power, and make conductive heating unit with graphite this moment, extinguishes until the body of heater flare, and building-up reactions finishes the back and closes stove; (3) silicon carbide whisker for preparing and micro mist are come out of the stove back purifying.
2. the industrial production process of a kind of silicon carbide whisker according to claim 1 and micro mist is characterized in that the industrial carbon raw material that uses in the described step (1) comprises hard coal, bituminous coal, carbon black or refinery coke; Industrial siliceous raw material comprises quartz sand, Pure Silicon Metal or organosilicon.
3. the industrial production process of a kind of silicon carbide whisker according to claim 1 and micro mist it is characterized in that adding in the described reaction material the single or combination catalyst of sodium-chlor, vitriol, silicate, metal oxide, and thorough mixing is even.
4. the industrial production process of a kind of silicon carbide whisker according to claim 1 and micro mist is characterized in that the synthesis reaction temperature in the industrial SiC smelting furnace described in the step (2) is 1400-2000 ℃, and the reaction times is 2-60 hour.
5. the industrial production process of a kind of silicon carbide whisker according to claim 1 and micro mist is characterized in that the CO (carbon monoxide converter) gas that produces in the building-up reactions in the described step (2) substitutes other inert protective gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031146724A CN100415644C (en) | 2003-05-09 | 2003-05-09 | Industrial preparation method for silica carbide crystal whisker and micropowder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031146724A CN100415644C (en) | 2003-05-09 | 2003-05-09 | Industrial preparation method for silica carbide crystal whisker and micropowder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1449994A CN1449994A (en) | 2003-10-22 |
| CN100415644C true CN100415644C (en) | 2008-09-03 |
Family
ID=28684133
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB031146724A Expired - Lifetime CN100415644C (en) | 2003-05-09 | 2003-05-09 | Industrial preparation method for silica carbide crystal whisker and micropowder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100415644C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100415951C (en) * | 2006-01-17 | 2008-09-03 | 浙江大学 | A suitable method for SiC whisker growth |
| CN100360400C (en) * | 2006-06-27 | 2008-01-09 | 河南醒狮高新技术股份有限公司 | Dedicated blade materials for line cutting of semiconductor materials |
| CN103387231B (en) * | 2013-07-19 | 2015-05-27 | 张兴材 | Synthesis method of beta-SiC micro-powder and whiskers |
| CN104328478B (en) * | 2014-08-14 | 2016-08-31 | 郑州航空工业管理学院 | A kind of preparation method of SiC whisker |
| CN106087061B (en) * | 2016-07-28 | 2018-05-22 | 李志文 | The method that powder quartz ore processes cubic silicon carbide whisker |
| CN109127559B (en) * | 2018-07-16 | 2021-06-08 | 淮安利泰碳化硅微粉有限公司 | Silicon carbide micro powder cleaning device and cleaning method thereof |
| CN114772600A (en) * | 2022-04-13 | 2022-07-22 | 闵庆武 | Formula and preparation method of various raw materials for smelting silicon carbide |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5207263A (en) * | 1989-12-26 | 1993-05-04 | Bp America Inc. | VLS silicon carbide whisker reinforced metal matrix composites |
| US5246894A (en) * | 1991-03-29 | 1993-09-21 | Tokai Carbon Co., Ltd. | Silicon carbide reinforced composite material |
| CN1077182A (en) * | 1992-11-28 | 1993-10-13 | 祝长宇 | 12H-alpha-sic whisker and method for making thereof |
| CN1078507A (en) * | 1992-05-08 | 1993-11-17 | 成都科技大学 | Preparation method of silicon carbide whisker raw material |
| CN1257944A (en) * | 1999-12-22 | 2000-06-28 | 天津大学 | Process for preparing nm-class silicon carbonite whisker/fibre |
| CN1276340A (en) * | 2000-07-14 | 2000-12-13 | 清华大学 | Process for preparing silicon carbide crystal whisker from river sand |
-
2003
- 2003-05-09 CN CNB031146724A patent/CN100415644C/en not_active Expired - Lifetime
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5207263A (en) * | 1989-12-26 | 1993-05-04 | Bp America Inc. | VLS silicon carbide whisker reinforced metal matrix composites |
| US5246894A (en) * | 1991-03-29 | 1993-09-21 | Tokai Carbon Co., Ltd. | Silicon carbide reinforced composite material |
| CN1078507A (en) * | 1992-05-08 | 1993-11-17 | 成都科技大学 | Preparation method of silicon carbide whisker raw material |
| CN1077182A (en) * | 1992-11-28 | 1993-10-13 | 祝长宇 | 12H-alpha-sic whisker and method for making thereof |
| CN1257944A (en) * | 1999-12-22 | 2000-06-28 | 天津大学 | Process for preparing nm-class silicon carbonite whisker/fibre |
| CN1276340A (en) * | 2000-07-14 | 2000-12-13 | 清华大学 | Process for preparing silicon carbide crystal whisker from river sand |
Non-Patent Citations (4)
| Title |
|---|
| 双重加热法合成碳化硅晶须的研究. 戴长虹等.人工晶体学报，第32卷第1期. 2003 |
| 双重加热法合成碳化硅晶须的研究. 戴长虹等.人工晶体学报，第32卷第1期. 2003 * |
| 粉末电热体加热法合成碳化硅晶须的研究. 戴长虹等.硅酸盐学报，第31卷第4期. 2003 |
| 粉末电热体加热法合成碳化硅晶须的研究. 戴长虹等.硅酸盐学报，第31卷第4期. 2003 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1449994A (en) | 2003-10-22 |
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