CN100500612C - Method for producing high resistance constant pressure sintering silicon carbide products - Google Patents
Method for producing high resistance constant pressure sintering silicon carbide products Download PDFInfo
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- CN100500612C CN100500612C CNB2007100549112A CN200710054911A CN100500612C CN 100500612 C CN100500612 C CN 100500612C CN B2007100549112 A CNB2007100549112 A CN B2007100549112A CN 200710054911 A CN200710054911 A CN 200710054911A CN 100500612 C CN100500612 C CN 100500612C
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- silicon carbide
- slip
- powder
- sintering
- pressure sintering
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 40
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000005245 sintering Methods 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 7
- 239000007921 spray Substances 0.000 claims abstract description 7
- 238000000746 purification Methods 0.000 claims abstract description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 4
- 238000003825 pressing Methods 0.000 claims abstract description 4
- 239000003595 mist Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- -1 polyoxyethylene Polymers 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 150000003673 urethanes Chemical class 0.000 claims description 3
- 239000003643 water by type Substances 0.000 claims description 3
- 239000002002 slurry Substances 0.000 abstract 5
- 238000005469 granulation Methods 0.000 abstract 3
- 230000003179 granulation Effects 0.000 abstract 3
- 229910052580 B4C Inorganic materials 0.000 abstract 1
- 239000002202 Polyethylene glycol Substances 0.000 abstract 1
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 abstract 1
- 229920001223 polyethylene glycol Polymers 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
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- Ceramic Products (AREA)
Abstract
The present invention discloses a production method for high-resistance normal-pressure sintering SiC products, which mainly comprises the following steps: the first step is purification, namely, water is added to silicon carbide powder (particle size is: d50 is more than or equal to 3.5 mum); then the silicon carbide powder is confected into mixed acid for purification, by using nitric acid and hydrofluoric acid according to weight ratio of 1:1; the second step is fining, namely, the purified silicon carbide slurry is milled into submicron powders; the third step: polyvinyl alcohol, polyethylene glycol and boron carbide are added to the submicron powders to confect the slurry for spray granulation; the fourth step: the slurry is pumped out by a slurry pump and driven into the top of a spray granulation tower by a spray gun, and then the slurry falls on the bottom of the spray granulation tower to get 80-240 mu silicon carbide powders; the fifth step: the silicon carbide powders are placed in a mold and pressed into a perform by using a pressing machine; the sixth step is sintering, that is, the perform is placed into a vacuum resistance furnace for sintering, so as to get the normal-pressure sintering SiC product which reaches as high as 108-1010/0.01-0.2 ohm-cm in volume resistivity value. The product can fully meet the requirements of the IT industry as well as the electrical equipment industry.
Description
Technical field
The present invention relates to the production method of constant pressure sintering silicon carbide products, especially relate to a kind of production method of high resistance constant pressure sintering silicon carbide products.
Background technology
Constant pressure sintering silicon carbide is a kind of novel high-quality non-metallic material with high strength, high rigidity, characteristic such as high temperature resistant, corrosion-resistant, wear-resistant, be widely used among the every field of national product, along with science and technology development, its Application Areas is also in further expansion.But; when carrying out work in the environment of strong current is arranged, the protecting materials that needs should have wear-resisting, corrosion-resistant, resistant to elevated temperatures characteristic, necessary again good insulation preformance; and common constant pressure sintering silicon carbide material only has wear-resisting, corrosion-resistant, resistant to elevated temperatures characteristic now, and volume resistance only is 10
2-10
6/ 0.01-0.2ohm-cm, its insulating property are unsatisfactory, therefore, must make constant pressure sintering silicon carbide products have higher volume resistance to satisfy the requirement of IT and electrician trade.
Summary of the invention
The object of the present invention is to provide a kind of production method that can satisfy the high resistance constant pressure sintering silicon carbide products of IT and electrician trade specific demand.
For achieving the above object, the present invention can take following technical proposals:
The production method of high resistance constant pressure sintering silicon carbide products of the present invention, it comprises the steps:
The first step: purify
With granularity is that the carborundum powder of d50 〉=3.5 μ m adds water and mixes to stir in the container of stainless steel or liner urethanes and make slip, get nitric acid, hydrofluoric acid is mixed with mix acid liquor according to the ratio of weight part 1:1,5-10% according to carborundum powder weight adds mix acid liquor, make itself and slip thorough mixing, water waters down then, this process is 2-3 time repeatedly, can fully remove impurity contained in the carborundum powder;
Second step: beat thin
Silicon carbide slip after the first step purification was put into grinding machine for grinding 300-400 hour, silicon-carbide particle is crushed to inferior micro powder grade, make d50≤0.5 μ m;
The 3rd step: preparation mist projection granulating slip
The second step gained slip is added water to stir, the weight part proportioning that makes water and silicon carbide micro-powder is 52-48:48-52, and the norbide that adds polyoxyethylene glycol, the 0.3-2 weight part of polyvinyl alcohol, the 0.5-4 weight part of 3-12 weight part more therein stirs that to make slip standby;
The 4th step: mist projection granulating integer
The slip that the 3rd step prepared is extracted out with slush pump, squeeze into the mist projection granulating top of tower by spray gun, the slip drop by hot air dries, promptly becomes spherical silicon carbide small-particle after falling prilling tower bottom in dropping process, with the sieve screening, obtain 80-240 purpose sic powder again;
The 5th step: green compact moulding
The 4th sic powder that obtain of step is put into the mould of green article, and the powder water ratio is 2-5%, with pressing machine powder is pressed into required green article then;
The 6th step: sintering
The green article that the 5th step made is put into the vacuum resistance furnace sintering, and sintering temperature is at 2200-2300 ℃, and sintering time is 12-18 hour, can obtain having high-resistance constant pressure sintering silicon carbide products.
The invention has the advantages that the constant pressure sintering silicon carbide products that adopts this production method to produce, its volume resistance value can be up to 10
8-10
10/ 0.01-0.2ohm-cm, and resistance is respectively consistent to distributing, and uses in IT and electrician trade and can satisfy its requirement fully, has widened the Application Areas of constant pressure sintering silicon carbide products.
Embodiment
The production method of high resistance constant pressure sintering silicon carbide products of the present invention, it comprises the steps:
The first step: purify
With granularity is that the carborundum powder of d50 〉=3.5 μ m adds water and mixes to stir in the container of stainless steel or liner urethanes and make slip, get nitric acid, hydrofluoric acid is mixed with mix acid liquor according to the ratio of weight part 1:1, add mix acid liquor according to 7% of carborundum powder weight, make itself and slip thorough mixing, water waters down then, and this process is 3 times repeatedly;
Second step: beat thin
Silicon carbide slip after the first step purification was put into grinding machine for grinding 300-400 hour, silicon-carbide particle is crushed to inferior micro powder grade, make d50≤0.5 μ m;
The 3rd step: preparation mist projection granulating slip
The second step gained slip is added water stir, the weight part proportioning that makes water and silicon carbide micro-powder is 50: 50, adds 8 parts polyvinyl alcohol, 2 parts polyoxyethylene glycol, 1 part norbide more therein and stirs that to make slip standby;
The 4th step: mist projection granulating integer
The slip that the 3rd step prepared is extracted out with slush pump, squeeze into the mist projection granulating top of tower by spray gun, the slip drop by hot air dries, promptly becomes spherical silicon carbide small-particle after falling prilling tower bottom in dropping process, with the sieve screening, obtain 80-240 purpose sic powder again;
The 5th step: green compact moulding
The 4th sic powder that obtain of step is put into the mould of green article, and the powder water ratio is 3%, with pressing machine powder is pressed into required green article then;
The 6th step: sintering
The green article that the 5th step made is put into the vacuum resistance furnace sintering, and sintering temperature is at 2250 ℃, and sintering time is 16 hours, can obtain the volume resistance value and reach 10
8-10
10The high resistance constant pressure sintering silicon carbide products of/0.01-0.2ohm-cm.
Claims (1)
1, a kind of production method of high resistance constant pressure sintering silicon carbide products, it is characterized in that: it comprises the steps:
The first step: purify
With granularity is that the carborundum powder of d50 〉=3.5 μ m adds water and mixes to stir in the container of stainless steel or liner urethanes and make slip, get nitric acid, hydrofluoric acid is mixed with mix acid liquor according to the ratio of weight part 1:1,5-10% according to carborundum powder weight adds mix acid liquor, make itself and slip thorough mixing, water waters down then, and this process is 2-3 time repeatedly;
Second step: beat thin
Silicon carbide slip after the first step purification was put into grinding machine for grinding 300-400 hour, silicon-carbide particle is crushed to inferior micro powder grade, make d50≤0.5 μ m;
The 3rd step: preparation mist projection granulating slip
The second step gained slip is added water to stir, the weight part proportioning that makes water and silicon carbide micro-powder is 52-48: 48-52, and the norbide that adds polyoxyethylene glycol, the 0.3-2 weight part of polyvinyl alcohol, the 0.5-4 weight part of 3-12 weight part more therein stirs that to make slip standby;
The 4th step: mist projection granulating integer
The slip that the 3rd step prepared is extracted out with slush pump, squeeze into the mist projection granulating top of tower by spray gun, the slip drop by hot air dries, promptly becomes spherical silicon carbide small-particle after falling prilling tower bottom in dropping process, with the sieve screening, obtain 80-240 purpose sic powder again;
The 5th step: green compact moulding
The 4th sic powder that obtain of step is put into the mould of green article, and the powder water ratio is 2-5%, with pressing machine powder is pressed into required green article then;
The 6th step: sintering
The green article that the 5th step made is put into the vacuum resistance furnace sintering, and sintering temperature is at 2200-2300 ℃, and sintering time is 12-18 hour, can obtain having high-resistance constant pressure sintering silicon carbide products.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100549112A CN100500612C (en) | 2007-08-08 | 2007-08-08 | Method for producing high resistance constant pressure sintering silicon carbide products |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100549112A CN100500612C (en) | 2007-08-08 | 2007-08-08 | Method for producing high resistance constant pressure sintering silicon carbide products |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101104560A CN101104560A (en) | 2008-01-16 |
| CN100500612C true CN100500612C (en) | 2009-06-17 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100549112A Active CN100500612C (en) | 2007-08-08 | 2007-08-08 | Method for producing high resistance constant pressure sintering silicon carbide products |
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| CN (1) | CN100500612C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NO335994B1 (en) | 2011-10-13 | 2015-04-13 | Saint Gobain Ceramic Mat As | Process for producing grains useful for the preparation of a silicon carbide-based sintered product, composite grains prepared by the process, and use of the grains. |
| CN111547725A (en) * | 2020-05-14 | 2020-08-18 | 湖南太子新材料科技有限公司 | Preparation method for extracting silicon carbide from polyurethane wrapped with silicon carbide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4004934A (en) * | 1973-10-24 | 1977-01-25 | General Electric Company | Sintered dense silicon carbide |
| US4410502A (en) * | 1980-11-13 | 1983-10-18 | Asahi-Dow Limited | Method for manufacture of silicon carbide |
| CN1915809A (en) * | 2006-09-07 | 2007-02-21 | 郑州华硕精密陶瓷有限公司 | Method of spraying granulation for preparing miropowder of silicon carbide in submicro level |
| CN1915632A (en) * | 2006-09-07 | 2007-02-21 | 郑州华硕精密陶瓷有限公司 | Pressure forming method for sintering green pressing products under normal pressure |
-
2007
- 2007-08-08 CN CNB2007100549112A patent/CN100500612C/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4004934A (en) * | 1973-10-24 | 1977-01-25 | General Electric Company | Sintered dense silicon carbide |
| US4410502A (en) * | 1980-11-13 | 1983-10-18 | Asahi-Dow Limited | Method for manufacture of silicon carbide |
| CN1915809A (en) * | 2006-09-07 | 2007-02-21 | 郑州华硕精密陶瓷有限公司 | Method of spraying granulation for preparing miropowder of silicon carbide in submicro level |
| CN1915632A (en) * | 2006-09-07 | 2007-02-21 | 郑州华硕精密陶瓷有限公司 | Pressure forming method for sintering green pressing products under normal pressure |
Non-Patent Citations (4)
| Title |
|---|
| 反应烧结SiC-B4C陶瓷材料的研究. 尹茜等.陶瓷，第2期. 2007 |
| 反应烧结SiC-B4C陶瓷材料的研究. 尹茜等.陶瓷，第2期. 2007 * |
| 碳化硅陶瓷的热等静压烧结. 佘继红等.硅酸盐学报，第25卷第4期. 1997 |
| 碳化硅陶瓷的热等静压烧结. 佘继红等.硅酸盐学报，第25卷第4期. 1997 * |
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| CN101104560A (en) | 2008-01-16 |
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