CN1137046C - Production process of submicron level silicon carbide - Google Patents
Production process of submicron level silicon carbide Download PDFInfo
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- CN1137046C CN1137046C CNB011246960A CN01124696A CN1137046C CN 1137046 C CN1137046 C CN 1137046C CN B011246960 A CNB011246960 A CN B011246960A CN 01124696 A CN01124696 A CN 01124696A CN 1137046 C CN1137046 C CN 1137046C
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- silicon carbide
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Abstract
The present invention relates to a method for producing submicron silicon carbide, which comprises: diluent silicon carbide slurry whose the granularity is from 100 to 1500 meshes is ground for 60 to 90 hours under the condition that silicon carbide grinding media exist. The method is characterized in that dispersing agents are added to the diluent silicon carbide slurry, and the silicon carbide grinding media are added according to the sizes of grain diameters. The method has the advantages of small equipment investment, simple production process, easy quality control, etc. The method enables the grain diameter of 85 to 99% of the silicon carbide powder to be less than 1 micrometre only through one-step grinding.
Description
Technical field
The present invention relates to a kind of production method of silicon carbide in submicro level.
Background technology
Silicon carbide is a kind of in several high hardness materials, and its Mohs' hardness is 9.2, is commonly called as powder emery.Silicon carbide is mainly used in grinding tool, Abrasive Industry in early days, in recent years, because many good characteristics that silicon carbide had, and be applied to fine ceramics goods field, but the requirement to its performance, granularity is very high, its mean particle size of general requirement is a submicron order, and size-grade distribution is had very high requirement, especially to less than 1 μ m quantity very high requirement being arranged also.
Now, the method of processing this submicron order powder is a lot, pulverize as airflow counter-collision, vibration mill is pulverized, the stirring abrasive dust is broken etc., each tool relative merits: it is that dry method is utilized high velocity air to drive silicon-carbide particle self to run foul of each other and pulverize that a. airflow counter-collision is pulverized, its advantage is that pollution is little, efficient is higher, be suitable for producing the various granularity powder products of several microns to thirties microns, though also can produce micron or contain one micron mixture of 10-20% with thin product, but its product distributed area is wide, need to increase classification operation and equipment, and very thin because of its granularity, manufacturing condition is difficult to control; At present, still incompetent accurately classification goes out 1 μ m (content is 60%) with interior production unit; B. vibration mill, stirring mill are to utilize medium to roll, clash into by comminuting matter and carry out grinding and processing, its advantage is that efficient is higher, but still need milling product is carried out classification, especially produce one micron product that accounts for 70-80% with interior particulate, also need above classification operation of secondary or the above pulverizing process of secondary, complex manufacturing; The powder particle of Chinese patent " a kind of autogenous attrition grinding method " (application number 87103890) disclosed a kind of at least 90% is decreased to the production method that granularity is the silicon carbide powder of 1 μ m, but its desired operation is a secondary, equipment has high input, complex technical process.
Summary of the invention
The objective of the invention is to overcome the defective of above-mentioned prior art, provide a kind of technological process simple, equipment drops into little, can a grinding and processing can reach the production method of 85-99% less than the submicron silicon carbide powder of 1 μ m.
Technical scheme of the present invention is:
A kind of production method of silicon carbide in submicro level, be included under the condition of silicon carbide grinding medium existence, with granularity is that 100-1500 purpose silicon carbide solvent or diluent slurry ground 60～90 hours, it is characterized in that: in above-mentioned silicon carbide solvent or diluent slurry, add dispersion agent, described dispersion agent is the composition of aniorfic surfactant and nonionic surface active agent, and its add-on is the 1-5% of weight of material; Described silicon carbide grinding medium is large, medium and small with 1 by its particle diameter: the weight proportion of 3-10: 20-30 adds, and its big spherical diameter is the 10-20 millimeter, and middle spherical diameter is the 5-10 millimeter, and little spherical diameter is the 1-2 millimeter;
The weight proportion of water and material is 5-10 in the described silicon carbide grout: 1;
The weight proportion of described aniorfic surfactant and nonionic surface active agent is 1: 0.5～5;
Described aniorfic surfactant is pyrophosphate salt, alkyl sulfonates, carboxylate salt or acrylate;
Described nonionic surface active agent is alkane Soxylat A 25-7 or ester class, sorbitan fatty acid class or sucrose fatty ester class;
Described silicon carbide grinding medium is Ceramic Balls or steel ball.
The submicron silicon carbide powder of producing with production technique of the present invention, after the purified processing, its purity is reached more than 98%, this purifying process adopts mixing acid such as HF, HCL to carry out cleanup acid treatment, metallic impurity ion of removing in the submicron silicon carbide powder or being introduced by grinding medium and free silica etc.
Realize working method of the present invention, its key point is to solve the scattering problem of powder; By general points of view, as long as pulverizing time sufficiently long, pulverized material just can reach required granularity, but in fact, when most materials are crushed to certain fineness, owing to be on the increase by the granule number of comminuting matter, specific surface area constantly increases thereupon, surface energy constantly increases, the probability that runs foul of each other between the particle increases, and after this collision acquires a certain degree, will produce agglomerating force between the particle: when material disperses in feed liquid when better, feed liquid is between a kind of particle constantly reunites, in the homeostasis process of constantly being broken again simultaneously; When material disperses then " flex point " can occur when general in feed liquid, promptly material is ground thicker and thicker.
The present invention is by adding dispersion agent---the composition of ionic surface active agent and nonionic surface active agent, make it to cooperatively interact, reduced by the surface energy of comminuting matter, it is reunited reduces, be equipped with suitable grinding medium mechanical fraction again, overcome the appearance of " flex point ", in other words " flex point " moved down into median size below 1 μ m, made by grinding and processing of comminuting matter to reach median size D
50≤ 0.65 μ m, specific surface area 〉=16m
2/ g; This method has that facility investment is little, and technology is simple, and quality is advantage such as control easily, after purified processing is expected in pulverizing of the present invention, its purity is reached more than 98%.
Embodiment
Embodiment 1:
With grinding particle size is 1000～1500 purpose material 80kg, water 600kg, (stirring rod is a multilayer to put into 900 liters of modified versions stirring mills, 30 ° of chiasma types) in, add cast iron hardened steel ball (particle diameter is that big ball 20kg, the particle diameter of 10-20mm is the middle ball 100kg of 5-10mm and the bead 500kg that particle diameter is 1-2mm) and dispersion agent: trisodium phosphate and Span be 800g (ratio of the two is 1: 1) altogether, pulverize and ground 60-70 hour, detecting its granularity is D
50=0.58 μ m, (Fe is produced in the neutralization of available hydrogen fluoric acid in purified processing
2O
3) after, detecting its granularity again is D
50=0.56 μ m, D
95=1.08 μ m, specific surface area (BET method)=16.9m
2/ g, its purity can reach 97.6%.
Embodiment 2
With grinding particle size is 600～1500 purpose material 100kg, and water 650kg puts into 900 liters of modified versions and stirs mill, adds Al
2O
3Ceramic Balls (its big ball 30kg, middle ball 90kg and bead 600kg) and dispersion agent: sodium alkyl benzene sulfonate and alkane Soxylat A 25-7 800g (ratio of the two is 1: 1.2), ground 80-90 hour, detecting its granularity is D
50=0.56 μ m, except that (purifying process is with embodiment 1) after the purification process, surveying its granularity again is D
50=0.515 μ m, D
95=0.989 μ m, specific surface area=17.1m
2/ g, its purity is 98.11%.
Embodiment 3
With grinding particle size is 1200～1500 purpose material 100kg, water 650kg, put into 900 liters of modified versions and stir mill, the oarse-grained 600kg of material self that adds 1-2mm, and dispersion agent: trisodium phosphate and sucrose ester be 800g (ratio of the two is 1: 1.2) altogether, ground 70-80 hour, detecting its granularity is D
50=0.64 μ m, after the purified processing (purifying process is with embodiment 1), detecting its granularity is D
50=0.65 μ m, D
95=1.44 μ m, specific surface area=15.6m
2/ g, its purity can reach 98.0%.
Claims (6)
1. the production method of a silicon carbide in submicro level, be included under the condition of silicon carbide grinding medium existence, with granularity is that 100-1500 purpose silicon carbide solvent or diluent slurry ground 60～90 hours, it is characterized in that: in above-mentioned silicon carbide solvent or diluent slurry, add dispersion agent, described dispersion agent is the composition of aniorfic surfactant and nonionic surface active agent, and its add-on is the 1-5% of weight of material; Described silicon carbide grinding medium is large, medium and small with 1 by its particle diameter: the weight proportion of 3-10: 20-30 adds, and its big spherical diameter is the 10-20 millimeter, and middle spherical diameter is the 5-10 millimeter, and little spherical diameter is the 1-2 millimeter.
2. by the production method of the described silicon carbide in submicro level of claim 1, it is characterized in that: the weight proportion of water and material is 5-10 in the described silicon carbide grout: 1.
3. by the production method of the described silicon carbide in submicro level of claim 1, it is characterized in that: the weight proportion of described aniorfic surfactant and nonionic surface active agent is 1: 0.5～5.
4. by the production method of claim 1 or 3 described silicon carbide in submicro level, it is characterized in that: described aniorfic surfactant is pyrophosphate salt, alkyl sulfonates, carboxylate salt or acrylate.
5. by the production method of claim 1 or 3 described silicon carbide in submicro level, it is characterized in that: described nonionic surface active agent is alkane Soxylat A 25-7 or ester class, sorbitan fatty acid class or sucrose fatty ester class.
6. by the production method of the described silicon carbide in submicro level of claim 1, it is characterized in that: described silicon carbide grinding medium is Ceramic Balls or steel ball.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011246960A CN1137046C (en) | 2001-08-07 | 2001-08-07 | Production process of submicron level silicon carbide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011246960A CN1137046C (en) | 2001-08-07 | 2001-08-07 | Production process of submicron level silicon carbide |
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| Publication Number | Publication Date |
|---|---|
| CN1344675A CN1344675A (en) | 2002-04-17 |
| CN1137046C true CN1137046C (en) | 2004-02-04 |
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|---|---|---|---|
| CNB011246960A Expired - Fee Related CN1137046C (en) | 2001-08-07 | 2001-08-07 | Production process of submicron level silicon carbide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100340347C (en) * | 2005-08-03 | 2007-10-03 | 连云港市研磨厂 | Technique for producing silicon carbide miropowder |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100374371C (en) * | 2006-09-07 | 2008-03-12 | 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 |
| CN101705076B (en) * | 2009-09-30 | 2013-05-08 | 汉寿金诚研磨材有限公司 | Method for producing green silicon carbide FEPA F P |
| CN101746758B (en) * | 2009-12-15 | 2012-02-01 | 昌乐鑫源碳化硅微粉有限公司 | Production method of ultrafine silicon carbide powder |
| CN102176519A (en) * | 2011-03-02 | 2011-09-07 | 湖南美特新材料科技有限公司 | Method for preparing submicron-level lithium carbonate, lithium carbonate powder and application of lithium carbonate powder |
| CN103072096A (en) * | 2011-10-26 | 2013-05-01 | 湖北天马研磨材料有限公司 | High-precision coated abrasive tool and production process method for same |
| CN103923605B (en) * | 2014-03-14 | 2015-12-02 | 唐山圣诺纳微科技有限公司 | A kind of making method of silicon carbide ball |
| CN104925811A (en) * | 2015-06-19 | 2015-09-23 | 山田研磨材料有限公司 | Method for manufacturing ceramic-grade silicon carbide micro-powder |
| CN106964435A (en) * | 2017-06-01 | 2017-07-21 | 黄山加佳荧光材料有限公司 | A kind of superfine grinding method of fluorescent pigment |
| CN107686360A (en) * | 2017-08-18 | 2018-02-13 | 山东青州微粉有限公司 | Silicon carbide inorganic agent |
| CN108314453B (en) * | 2018-03-28 | 2021-03-09 | 中国科学院宁波材料技术与工程研究所 | Method for improving dispersion stability of silicon carbide powder in water system |
| CN111868142B (en) * | 2018-12-28 | 2022-08-16 | 浙江三时纪新材科技有限公司 | Preparation method of spherical silicon resin powder or connected body thereof and spherical silicon resin powder or connected body thereof obtained by preparation method |
| CN113582699B (en) * | 2021-07-22 | 2023-03-17 | 武汉工程大学 | Low-viscosity high-solid-content ceramic slurry and preparation method thereof |
| CN113956049A (en) * | 2021-11-09 | 2022-01-21 | 北方民族大学 | Method for preparing high-density ceramic by pressureless sintering of beta-SiC powder synthesized by self-propagating combustion |
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2001
- 2001-08-07 CN CNB011246960A patent/CN1137046C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100340347C (en) * | 2005-08-03 | 2007-10-03 | 连云港市研磨厂 | Technique for producing silicon carbide miropowder |
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| CN1344675A (en) | 2002-04-17 |
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