CN104909369A - Ultra-fine metal silicon powder production method - Google Patents
Ultra-fine metal silicon powder production method Download PDFInfo
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- CN104909369A CN104909369A CN201510279645.8A CN201510279645A CN104909369A CN 104909369 A CN104909369 A CN 104909369A CN 201510279645 A CN201510279645 A CN 201510279645A CN 104909369 A CN104909369 A CN 104909369A
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Abstract
The present invention discloses an ultra-fine metal silicon powder production method, which comprises that a raw material metal silicon powder is subjected to acid washing, alkali washing and ingot casting treatment to obtain a semi-finished product with a purity of 99.9-99.999%, coarse crushing is performed, screening is performed through a 100-mesh sieve, washing is repeatedly performed 5-8 times with deionized water to achieve the purity of more than or equal to 99.995%, the material is crushed in a jet mill through the 1-3 time ultra-high-speed airflow of low temperature, high purity and high pressure gas, and the crushed particles enter a grading chamber, wherein the large particles are continuously crushed, the small particles enter a cyclone separator to carry out separation grading package with different finenesses, the final product purity is 99.99-99.999%, the product particle size is 1000-12500 mesh, and the yield is more than or equal to 99%. According to the present invention, the process is simple, no dust is discharged and no impurity enters during the crushing process so as not to cause secondary pollution, and the product has characteristics of high yield, fine particle size, uniform distribution, and regular morphology.
Description
Technical field
The invention belongs to silicon materials manufacture field, be specifically related to a kind of production method of superfine metal silica flour.
Background technology
Superfine metal silica flour is most important semiconductor material, is widely used in the aspects such as computer, micro-wave communication, optical-fibre communications, solar electrical energy generation.Scientist is the silicon epoch current designate, and Pure Silicon Metal has excellent physical chemistry and semiconductor property, is therefore applied very soon in the semiconductor device, and obtains develop rapidly.Tradition is prepared superfine metal silica flour and is easily produced impurity in process of production, is unfavorable for large-scale commercial production, often there is thin and impure, a pure and thinless difficult problem, and the technique also had is too complicated, productive expense is high.At present, the source dependence on import to a great extent of China's superfine metal silica flour, develops autonomous superfine metal silica flour production method and seems particularly important.
Summary of the invention
For making up the deficiencies in the prior art, the invention provides a kind of production method of superfine metal silica flour, the method technique is simple, and yield rate is high.
The present invention is achieved through the following technical solutions:
1. a production method for superfine metal silica flour, is characterized in that: comprise the following steps:
(1) by purity about 99%, the feed metal silica flour about fineness 200 order obtains the work in-process of purity 99.9%-99.999% after pickling, alkali cleaning, ingot casting process;
(2) cross 100 mesh sieves by after work in-process coarse reduction, repeatedly rinse 5-8 time to purity more than 99.995% with deionized water;
(3) clean fresh air forms low temperature high-purity pressure gas and enters Jet Mill after air compressor processed compressed, 1-3 times of ultra-high speed air-flow is formed through nozzle ejection, drive the material high-speed motion entered through micronizer mill feeding chamber, material is pulverized;
(5) particle after pulverizing arrives grading room with upstream, grading machine runs up, granularity is greater than 1000 object particles and is thrown to outer wall and drops to crushiing chamber and again pulverize, granularity is less than 1000 object particles and enters the separation that cyclopneumatic separator carries out different fineness and divide grade packaged, the finished product purity is 99.99%-99.999%, product granularity is 1000-12500 order, yield rate more than 99%;
(6) tail gas filters through cloth envelop collector, and remaining grit is caught collection by cloth bag, and clean tail gas is discharged through induced draft fan.
The production method of superfine metal silica flour of the present invention, in step (3), the process of clean fresh air is crossed and is called: clean fresh air compresses through air compressor, form the high pressure gas of 0.6-1.2MPa, high pressure gas enter gas-holder through stainless steel pipes and carry out oily water separation, then enter strainer and carry out secondary filter, form purer high pressure gas, then enter freeze drier and carry out lyophilize, enter strainer again and carry out high-accuracy filtration, final formation low temperature high-purity pressure gas.
Further, the dew-point temperature in described freeze drier is-40 DEG C.
Further, the feeding device of described micronizer mill adopts urethane to be aided with wearing composite material and makes, grading wheel blade and upper and lower end face urethane coated, nozzle adopts urethane to make, and tube wall inside adopts urethane to paste.
Compared with prior art, the invention has the beneficial effects as follows:
(1) first purify and pulverize, avoiding that ultrafine powder after pulverizing purifies cannot effectively solid-liquor separation, yield rate be low, a difficult problem for weak effect.
(2) feeding device, nozzle, grading wheel etc. are made with the position urethane that raw material directly contacts, and effectively prevent the secondary pollution that crushing process produces.
(3) production technique is simple, and the qualified product after crushing and classification directly enter feed bin becomes finished product, has reduced middle-chain, decreases the possibility of pollution, and yield rate is increased to more than 99% by conventional 80%, and product granularity is thin, is evenly distributed, pattern rule.
Embodiment
Below by specific embodiment, the present invention is further detailed explanation.
Embodiment
(1) feedstock purification
By the purity about 99% of buying, starting material about fineness 200 order are poured in closed container, the dilute acid soln being mixed with diluted hydrofluoric acid and dilute hydrochloric acid is adopted to carry out pickling, then alkali cleaning is carried out with diluted sodium hydroxide solution, the purification liquid heating adding preparation for different impurities fully stirs ingot casting, then pulverizing purifies rinses 7 times repeatedly with deionized water, and finally making raw material reach purity 99.995% becomes work in-process.
(2) crushing material
Clean fresh air compresses through air compressor, form the high pressure gas of 0.6-1.2MPa, high pressure gas enter gas-holder through stainless steel pipes and carry out oily water separation, then enter strainer and carry out secondary filter, form purer high pressure gas, then the freeze drier entering dew-point temperature-40 DEG C carries out lyophilize, enter strainer again and carry out high-accuracy filtration, final formation low temperature high-purity pressure gas, low temperature high-purity pressure gas enters Jet Mill, 1-3 times of ultra-high speed air-flow is formed through nozzle ejection, drive the material high-speed motion entered through micronizer mill feeding chamber, material is pulverized.
(3) stock grading
Particle after pulverizing arrives grading room with upstream, grading machine runs up, granularity is greater than 1000 object particles and is thrown to outer wall and drops to crushiing chamber and again pulverize, granularity is less than 1000 object particles and enters the separation that cyclopneumatic separator carries out different fineness and divide grade packaged, form the product of different size, the finished product purity is 99.998%, and product granularity is 2000-12500 order, yield rate more than 99.2%.Tail gas filters through cloth envelop collector, and remaining grit is caught by cloth bag and collected packaging formation product, and clean tail gas is discharged through induced draft fan.Raw material input is according to product requirement 5KG-100KG per hour, and output and input keep balancing.
The present invention first purifies and pulverizes, avoiding that ultrafine powder after pulverizing purifies cannot effectively solid-liquor separation, yield rate be low, a difficult problem for weak effect, purification process preparation purification solution, discharge pollutes, micronizer mill feeding device, nozzle, grading wheel etc. are aided with the made wear-resisting composite material of special material with the position urethane that raw material directly contacts and make, tube wall inside lining is with urethane, effectively prevent the secondary pollution that crushing process produces, product-collecting adopts fully automatic vacuum packaging, and yield rate is high, and product granularity is thin, be evenly distributed, pattern rule.
Claims (4)
1. a production method for superfine metal silica flour, is characterized in that: comprise the following steps:
(1) by purity about 99%, the feed metal silica flour about fineness 200 order obtains the work in-process of purity 99.9%-99.999% after pickling, alkali cleaning, ingot casting process;
(2) cross 100 mesh sieves by after work in-process coarse reduction, repeatedly rinse 5-8 time to purity more than 99.995% with deionized water;
(3) clean fresh air forms low temperature high-purity pressure gas and enters Jet Mill after air compressor processed compressed, 1-3 times of ultra-high speed air-flow is formed through nozzle ejection, drive the material high-speed motion entered through micronizer mill feeding chamber, material is pulverized;
(5) particle after pulverizing arrives grading room with upstream, grading machine runs up, granularity is greater than 1000 object particles and is thrown to outer wall and drops to crushiing chamber and again pulverize, granularity is less than 1000 object particles and enters the separation that cyclopneumatic separator carries out different fineness and divide grade packaged, the finished product purity is 99.99%-99.999%, product granularity is 1000-12500 order, yield rate more than 99%;
(6) tail gas filters through cloth envelop collector, and remaining grit is caught collection by cloth bag, and clean tail gas is discharged through induced draft fan.
2. the production method of a kind of superfine metal silica flour according to claim 1, it is characterized in that: in step (3), the process of clean fresh air is crossed and is called: clean fresh air compresses through air compressor, form the high pressure gas of 0.6-1.2MPa, high pressure gas enter gas-holder through stainless steel pipes and carry out oily water separation, then enter strainer and carry out secondary filter, form purer high pressure gas, then enter freeze drier and carry out lyophilize, enter strainer again and carry out high-accuracy filtration, final formation low temperature high-purity pressure gas.
3. the production method of a kind of superfine metal silica flour according to claim 2, is characterized in that: the dew-point temperature in described freeze drier is-40 DEG C.
4. the production method of a kind of superfine metal silica flour according to claim 1, it is characterized in that: the feeding device of micronizer mill adopts urethane to be aided with wearing composite material and makes, grading wheel blade and upper and lower end face urethane coated, nozzle adopts urethane to make, and tube wall inside adopts urethane to paste.
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| CN201510279645.8A CN104909369A (en) | 2015-05-28 | 2015-05-28 | Ultra-fine metal silicon powder production method |
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| CN201510279645.8A CN104909369A (en) | 2015-05-28 | 2015-05-28 | Ultra-fine metal silicon powder production method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110665615A (en) * | 2019-10-10 | 2020-01-10 | 青岛瓷兴新材料有限公司 | Preparation method of superfine silicon powder |
| CN111302397A (en) * | 2020-03-13 | 2020-06-19 | 中国科学院城市环境研究所 | Method and device for recovering waste denitration catalyst |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101219791A (en) * | 2008-01-29 | 2008-07-16 | 鄄城金威粉体科技有限公司 | Method for producing high purity ultra-fine silicon dioxide |
| CN102145898A (en) * | 2011-05-05 | 2011-08-10 | 张冬玲 | Production method of silicon dioxide ultrafine powder |
| CN102642835A (en) * | 2012-04-19 | 2012-08-22 | 镇江环太硅科技有限公司 | Method for recovering silicon material from waste materials in cutting crystalline silicon by diamond wire |
-
2015
- 2015-05-28 CN CN201510279645.8A patent/CN104909369A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101219791A (en) * | 2008-01-29 | 2008-07-16 | 鄄城金威粉体科技有限公司 | Method for producing high purity ultra-fine silicon dioxide |
| CN102145898A (en) * | 2011-05-05 | 2011-08-10 | 张冬玲 | Production method of silicon dioxide ultrafine powder |
| CN102642835A (en) * | 2012-04-19 | 2012-08-22 | 镇江环太硅科技有限公司 | Method for recovering silicon material from waste materials in cutting crystalline silicon by diamond wire |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110665615A (en) * | 2019-10-10 | 2020-01-10 | 青岛瓷兴新材料有限公司 | Preparation method of superfine silicon powder |
| CN111302397A (en) * | 2020-03-13 | 2020-06-19 | 中国科学院城市环境研究所 | Method and device for recovering waste denitration catalyst |
| CN111302397B (en) * | 2020-03-13 | 2022-06-24 | 中国科学院城市环境研究所 | Method and device for recovering waste denitration catalyst |
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Application publication date: 20150916 |