CN102923717A - Method of preparing electronic-grade spherical silicon micro-power through straws - Google Patents
Method of preparing electronic-grade spherical silicon micro-power through straws Download PDFInfo
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Abstract
The invention discloses a method of preparing electronic-grade spherical silicon micro-power through straws. According to the invention, the electronic-grade spherical silicon micro-power is prepared by carrying out pretreatment purification and thermolytic dissociation, and then controlling the size and the shape of particles through after-treatment with straws as a raw material. The method comprises the following steps of: after fully drying the straws, removing dust and impurities, crushing to straw powder of 20-40 meshes, adding the straw powder into 0.1-10% (wt.) of oxidized acidic aqueous solution according to a mass ratio of 1: 5, etching at 80-300 DEG C, and drying after washing; carrying out thermolytic dissociation at 600-900 DEG C under the oxygen or air atmosphere; adding a structure control agent, carrying out hydro-thermal treatment at 300 DEG C, washing and drying so as to obtain the electronic-grade spherical silicon micro-power. The electronic-grade spherical silicon micro-power, prepared by the method of the invention, has purity of 99.99%, no radioactive element and controllable grain size; and the method has the advantages of simple production process, low cost, wide source of feed and reproducibility.
Description
Technical field
The invention belongs to the materials chemistry field, relate to the preparation method of electron grade spherical silicon micropowder, be specifically related to a kind of method of utilizing straw to prepare electron grade spherical silicon micropowder.
Background technology
High-purity ultra-fine sphere silicon micro-powder claims again electron grade spherical silicon micropowder, owing to have the advantages such as high purity, high-k, high heat-resisting wet, high filler loading capacity, low-expansion coefficient, low alpha-ray and low-stress, become indispensable high quality raw material in extensive, the super large-scale integration, the while also is applied in fields such as optical-fibre communications, aerospace, sun power.General spherical shape silicon powder price is at 20,000～100,000 yuan/tons, and the price of nano-level sphere silicon powder is more up to 20～300,000/ton.
At present domestic high purity ball-shaped silicon micro powder for super large-scale integration is almost all by external import.Japan is comparatively successful aspect spheroidization research, also is the leading exporter of ball-shaped silicon micro powder.The common using plasma method of the preparation of ball-shaped silicon micro powder, high-temperature fusion gunite, gas flame method and liquid phase water solution.But because complex process, production cost is high, and these methods still rest on laboratory stage at home.
In a word, the production method of existing electron grade spherical silicon micropowder exists complex process, high in cost of production problem, can't produce market in the urgent need to low cost, electron grade spherical silicon micropowder can be mass-produced.
Summary of the invention
The object of the invention is to overcome the shortcoming of prior art, a kind of method of utilizing straw to prepare electron grade spherical silicon micropowder is provided, have the characteristics such as technique is simple, cost is low, raw material sources are wide, method of the present invention is take straw as raw material, by preparing cheaply electron grade spherical silicon micropowder after the physics and chemistry modification.
Straw is as the first agricultural crop straw of China, about 200,000,000 tons of annual production.As shown in table 1, straw rich cellulose, xylogen, polysaccharide, inorganic ash content, and the content of fat, protein is very low.
The chemical constitution information slip (wt%) of table 1 straw
As shown in table 2, contain the oxide compound of the elements such as a large amount of silicon-dioxide and a small amount of potassium, calcium, iron, magnesium in the ashes after the straw burning, this shows that straw can be used as the desirable feedstock of producing electron grade spherical silicon micropowder.
Composition in table 2 straw in the ash content (wt%)
The present invention is take straw as raw material, and after pre-treatment purifying and pyrolysis, the element beyond the silicon-dioxide all can be reduced to extremely low-level, and the size shape by aftertreatment control particle prepares electron grade spherical silicon micropowder again.
In order to achieve the above object, the present invention has adopted following technical scheme:
A kind of method of utilizing straw to prepare electron grade spherical silicon micropowder may further comprise the steps:
(1) pre-treatment: after the abundant drying of straw, remove dust impurity, then be ground into 20 orders～40 purpose rice straw powders, rice straw powder is added in the acid aqueous solution of oxidisability, 80～300 ℃ of etchings 30～60 minutes, dry after the washing;
(2) thermolysis: with step (1) products therefrom under oxygen or air atmosphere, in 600～900 ℃ of pyrolysis 120～300 minutes;
(3) aftertreatment: add constitution controller in step (2) products therefrom, in 60～300 ℃ of hydrothermal treatment consists 30～300 minutes, washing, drying obtained electron grade spherical silicon micropowder.
In the step (1), the acid solution of described oxidisability is the combination solution of a kind of composition in strong acid and hydrogen peroxide or the dioxide peroxide, and described strong acid is one or more in sulfuric acid, hydrochloric acid, nitric acid or the perchloric acid.
In the step (1), the mass concentration of each component is 0.1～10% in the acid solution of described oxidisability, and the mass ratio of the acid solution of described oxidisability and rice straw powder is (3～10): 1.
In the step (3), described constitution controller is one or more in ammoniacal liquor, thanomin, Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH, TBAH, methylamine, ethamine, quadrol, triethylene tetramine, tetraethylene pentamine, cetylamine, stearylamine, hydroxyethyl ethamine, palmityl trimethyl ammonium chloride, cetyl trimethylammonium bromide, cetylpyridinium chloride, polyacrylic acid, polymethyl acrylic acid or the polyvinylpyrrolidone.
The mass ratio of rice straw powder is (0.1～5) described in constitution controller described in the step (3) and the step (1): 100.
With respect to prior art, the present invention has following advantage:
(1) the electron grade spherical silicon micropowder purity of method of the present invention preparation reaches 99.99%, particle diameter is controlled;
(2) electron grade spherical silicon micropowder of method preparation of the present invention does not have the radioactivity alpha-ray to pollute substantially;
(3) method of the present invention has that production technique is simple, cost is low, raw material sources are wide, reproducible advantage.
Description of drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the ball-shaped silicon micro powder of the embodiment of the invention 1 preparation.
Fig. 2 is the scanning electron microscope (SEM) photograph of the ball-shaped silicon micro powder of the embodiment of the invention 2 preparations.
Fig. 3 is the scanning electron microscope (SEM) photograph of the ball-shaped silicon micro powder of the embodiment of the invention 3 preparations.
Fig. 4 is the scanning electron microscope (SEM) photograph of the ball-shaped silicon micro powder of the embodiment of the invention 4 preparations.
Fig. 5 is the scanning electron microscope (SEM) photograph of the ball-shaped silicon micro powder of the embodiment of the invention 5 preparations.
Fig. 6 is the scanning electron microscope (SEM) photograph of the ball-shaped silicon micro powder of the embodiment of the invention 6 preparations.
Fig. 7 is the scanning electron microscope (SEM) photograph of the ball-shaped silicon micro powder of the embodiment of the invention 7 preparations.
Fig. 8 is the scanning electron microscope (SEM) photograph of the ball-shaped silicon micro powder of the embodiment of the invention 8 preparations.
Fig. 9 is the scanning electron microscope (SEM) photograph of the ball-shaped silicon micro powder of the embodiment of the invention 9 preparations.
Figure 10 is the scanning electron microscope (SEM) photograph of the ball-shaped silicon micro powder of the embodiment of the invention 10 preparations.
Figure 11 is the scanning electron microscope (SEM) photograph of the ball-shaped silicon micro powder of the embodiment of the invention 11 preparations.
Figure 12 is the scanning electron microscope (SEM) photograph of the ball-shaped silicon micro powder of the embodiment of the invention 12 preparations.
Embodiment
The present invention is further illustrated below in conjunction with embodiment and accompanying drawing, but claimed scope of the present invention is not limited to this.
Embodiment 1
(1) pre-treatment: after the abundant drying of 1000g straw, remove dust impurity by vibratory screening apparatus again, then be ground into 20 order rice straw powders, the rice straw powder adding of 1000g is contained in the 5000g aqueous solution of 5% hydrochloric acid and 5% hydrogen peroxide, under 150 ℃, etching is 60 minutes in the teflon-lined autoclave, and is dry after the washing;
(2) thermolysis: with step (1) products therefrom under the oxygen atmosphere, in 700 ℃ of pyrolysis 120 minutes;
(3) aftertreatment: with step (2) products therefrom in reactor, add 5g ammoniacal liquor, 5g ethamine, 2g tetraethylene pentamine, 2g stearylamine, 2g palmityl trimethyl ammonium chloride, 2g polyvinylpyrrolidone, in 120 ℃ of hydrothermal treatment consists 120 minutes, washing, drying obtain electron grade spherical silicon micropowder.
Adopt 7500 type inductively coupled plasma atomic mass spectrometries (Agilent company, the U.S.) technical testing, its purity reaches 4N, and the content situation of impurity element sees Table 3.By electron microscopic observation, particle diameter is about 200nm, and electromicroscopic photograph as shown in Figure 1.
Embodiment 2
(1) pre-treatment: after the abundant drying of 1000g straw, remove dust impurity by vibratory screening apparatus again, then be ground into 40 order rice straw powders, the rice straw powder adding of 1000g is contained in the 5000g aqueous solution of 1% hydrochloric acid and 5% hydrogen peroxide, under 200 ℃, etching is 30 minutes in the teflon-lined autoclave, and is dry after the washing;
(2) thermolysis: with step (1) products therefrom under the oxygen atmosphere, in 700 ℃ of pyrolysis 200 minutes;
(3) aftertreatment: step (2) products therefrom in reactor, is added 40g ammoniacal liquor, 9g methylamine, 1g cetyl trimethyl chlorine brometo de amonio, and in 60 ℃ of hydrothermal treatment consists 300 minutes, washing, drying obtained electron grade spherical silicon micropowder.
Adopt 7500 type inductively coupled plasma atomic mass spectrometries (Agilent company, the U.S.) technical testing, its purity reaches 4N, and the content situation of impurity element sees Table 3.By electron microscopic observation, particle diameter is about 150nm, and electromicroscopic photograph as shown in Figure 2.
Embodiment 3
(1) pre-treatment: after the abundant drying of 1000g straw, remove dust impurity by vibratory screening apparatus again, then be ground into 30 order rice straw powders, the rice straw powder adding of 1000g is contained in the 5000g aqueous solution of 2% hydrochloric acid and 5% hydrogen peroxide, under 80 ℃, etching is 30 minutes in the teflon-lined autoclave, and is dry after the washing;
(2) thermolysis: with step (1) products therefrom under the oxygen atmosphere, in 700 ℃ of pyrolysis 200 minutes;
(3) aftertreatment: step (2) products therefrom in reactor, is added 20g ammoniacal liquor, 10g stearylamine, 5g polyvinylpyrrolidone, and in 200 ℃ of hydrothermal treatment consists 120 minutes, washing, drying obtained electron grade spherical silicon micropowder.
Adopt 7500 type inductively coupled plasma atomic mass spectrometries (Agilent company, the U.S.) technical testing, its purity reaches 3N, and the content situation of impurity element sees Table 3.By electron microscopic observation, particle diameter is about 30nm, and electromicroscopic photograph as shown in Figure 3.
Embodiment 4
(1) pre-treatment: after the abundant drying of 1000g straw, remove dust impurity by vibratory screening apparatus again, then be ground into 20 order rice straw powders, the rice straw powder adding of 1000g is contained in the 5000g aqueous solution of 0.1% hydrochloric acid and 5% hydrogen peroxide, under 300 ℃, etching is 30 minutes in the teflon-lined autoclave, and is dry after the washing;
(2) thermolysis: with step (1) products therefrom under the oxygen atmosphere, in 700 ℃ of pyrolysis 180 minutes;
(3) aftertreatment: step (2) products therefrom in reactor, is added 10g ammoniacal liquor, 10g cetylpyridinium chloride, 5g polyacrylic acid, and in 150 ℃ of hydrothermal treatment consists 180 minutes, washing, drying obtained electron grade spherical silicon micropowder.
Adopt 7500 type inductively coupled plasma atomic mass spectrometries (Agilent company, the U.S.) technical testing, its purity reaches 3N, and the content situation of impurity element sees Table 3.By electron microscopic observation, particle diameter is about 100nm, and electromicroscopic photograph as shown in Figure 4.
Embodiment 5
(1) pre-treatment: after the abundant drying of 1000g straw, remove dust impurity by vibratory screening apparatus again, then be ground into 30 order rice straw powders, the rice straw powder adding of 1000g is contained in the 5000g aqueous solution of 2% hydrochloric acid, 1% sulfuric acid and 5% hydrogen peroxide, under 200 ℃, etching is 30 minutes in the teflon-lined autoclave, and is dry after the washing;
(2) thermolysis: with step (1) products therefrom under the oxygen atmosphere, in 700 ℃ of pyrolysis 200 minutes;
(3) aftertreatment: with step (2) products therefrom in reactor, add 5g polyacrylic acid, 1g thanomin, 1g Tetramethylammonium hydroxide, 2g tetraethyl ammonium hydroxide, 1g TPAOH, 0.5g TBAH, in 90 ℃ of hydrothermal treatment consists 180 minutes, washing, drying obtain electron grade spherical silicon micropowder.
Adopt 7500 type inductively coupled plasma atomic mass spectrometries (Agilent company, the U.S.) technical testing, its purity reaches 3N, and the content situation of impurity element sees Table 3.By electron microscopic observation, particle diameter is about 10nm, and electromicroscopic photograph as shown in Figure 5.
Embodiment 6
(1) pre-treatment: after the abundant drying of 1000g straw, remove dust impurity by vibratory screening apparatus again, then be ground into 30 order rice straw powders, the rice straw powder adding of 1000g is contained in the 5000g aqueous solution of 10% hydrochloric acid, 5% sulfuric acid, 5% nitric acid and 5% hydrogen peroxide, under 300 ℃, etching is 30 minutes in the teflon-lined autoclave, and is dry after the washing;
(2) thermolysis: with step (1) products therefrom under the oxygen atmosphere, in 700 ℃ of pyrolysis 150 minutes;
(3) aftertreatment: with step (2) products therefrom in reactor, add 10g ammoniacal liquor, 1g diethanolamine, 1g trolamine, 2g tetraethyl ammonium hydroxide, 1g Tetramethylammonium hydroxide, 5g ethamine, 1g cetylamine, 2g polyvinylpyrrolidone, in 100 ℃ of hydrothermal treatment consists 180 minutes, washing, drying obtain electron grade spherical silicon micropowder.
Adopt 7500 type inductively coupled plasma atomic mass spectrometries (Agilent company, the U.S.) technical testing, its purity reaches 4N, and the content situation of impurity element sees Table 3.By electron microscopic observation, particle diameter is about 50nm, and electromicroscopic photograph as shown in Figure 6.Embodiment 7
(1) pre-treatment: after the abundant drying of 1000g straw, remove dust impurity by vibratory screening apparatus again, then be ground into 40 order rice straw powders, the rice straw powder adding of 1000g is contained in the 5000g aqueous solution of 1% hydrochloric acid, 1% perchloric acid, 1% nitric acid and 5% hydrogen peroxide, under 200 ℃, etching is 60 minutes in the teflon-lined autoclave, and is dry after the washing;
(2) thermolysis: with step (1) products therefrom under the oxygen atmosphere, in 700 ℃ of pyrolysis 200 minutes;
(3) aftertreatment: with step (2) products therefrom in reactor, add 5g thanomin, 1g Tetramethylammonium hydroxide, 2g tetraethyl ammonium hydroxide, 1g TPAOH, 0.5g TBAH, 10g polyvinylpyrrolidone, in 300 ℃ of hydrothermal treatment consists 30 minutes, washing, drying obtain electron grade spherical silicon micropowder.
Adopt 7500 type inductively coupled plasma atomic mass spectrometries (Agilent company, the U.S.) technical testing, its purity reaches 3N, and the content situation of impurity element sees Table 3.By electron microscopic observation, particle diameter is about 300nm, and electromicroscopic photograph as shown in Figure 7.
Embodiment 8
(1) pre-treatment: after the abundant drying of 1000g straw, remove dust impurity by vibratory screening apparatus again, then be ground into 20 order rice straw powders, the rice straw powder adding of 1000g is contained in the 5000g aqueous solution of 1% hydrochloric acid, 0.5% sulfuric acid, 1% nitric acid and 5% dioxide peroxide, under 200 ℃, etching is 60 minutes in the teflon-lined autoclave, and is dry after the washing;
(2) thermolysis: with step (1) products therefrom under the oxygen atmosphere, in 650 ℃ of pyrolysis 240 minutes;
(3) aftertreatment: with step (2) products therefrom in reactor, add 5g ammoniacal liquor, 3g thanomin, 5g Tetramethylammonium hydroxide, 0.5g TBAH, 10g polyvinylpyrrolidone, in 300 ℃ of hydrothermal treatment consists 60 minutes, washing, drying obtained electron grade spherical silicon micropowder.
Adopt 7500 type inductively coupled plasma atomic mass spectrometries (Agilent company, the U.S.) technical testing, its purity reaches 3N, and the content situation of impurity element sees Table 3.By electron microscopic observation, particle diameter is about 20nm, and electromicroscopic photograph as shown in Figure 8.
Embodiment 9
(1) pre-treatment: after the abundant drying of 1000g straw, remove dust impurity by vibratory screening apparatus again, then be ground into 30 order rice straw powders, the rice straw powder adding of 1000g is contained in the 5000g aqueous solution of 0.2% hydrochloric acid, 0.5% sulfuric acid, 0.1% nitric acid and 1% dioxide peroxide, under 200 ℃, etching is 60 minutes in the teflon-lined autoclave, and is dry after the washing;
(2) thermolysis: with step (1) products therefrom under air atmosphere, in 600 ℃ of pyrolysis 300 minutes;
(3) aftertreatment: with step (2) products therefrom in reactor, add 10g ammoniacal liquor, 5g thanomin, 5g Tetramethylammonium hydroxide, 1g methylamine, 3g polymethyl acrylic acid, 5g polyvinylpyrrolidone, in 150 ℃ of hydrothermal treatment consists 180 minutes, washing, drying obtain electron grade spherical silicon micropowder.
Adopt 7500 type inductively coupled plasma atomic mass spectrometries (Agilent company, the U.S.) technical testing, its purity reaches 2N, and the content situation of impurity element sees Table 3.By electron microscopic observation, particle diameter is about 10nm, and electromicroscopic photograph as shown in Figure 9.
Embodiment 10
(1) pre-treatment: after the abundant drying of 1000g straw, remove dust impurity by vibratory screening apparatus again, then be ground into 30 order rice straw powders, the rice straw powder adding of 1000g is contained in the 10000g aqueous solution of 1% hydrochloric acid, 1% sulfuric acid, 1% nitric acid, 4% hydrogen peroxide and 4% dioxide peroxide, under 220 ℃, etching is 60 minutes in the teflon-lined autoclave, and is dry after the washing;
(2) thermolysis: with step (1) products therefrom under the oxygen atmosphere, in 900 ℃ of pyrolysis 60 minutes;
(3) aftertreatment: step (2) products therefrom in reactor, is added 10g ammoniacal liquor, 1g trolamine and 1g Tetramethylammonium hydroxide, and in 300 ℃ of hydrothermal treatment consists 60 minutes, washing, drying obtained electron grade spherical silicon micropowder.
Adopt 7500 type inductively coupled plasma atomic mass spectrometries (Agilent company, the U.S.) technical testing, its purity reaches 3N, and the content situation of impurity element sees Table 3.By electron microscopic observation, particle diameter is about 300nm, and electromicroscopic photograph as shown in figure 10.
Embodiment 11
(1) pre-treatment: after the abundant drying of 1000g straw, remove dust impurity by vibratory screening apparatus again, then be ground into 20 order rice straw powders, the rice straw powder adding of 1000g is contained in the 3000g aqueous solution of 5% hydrochloric acid and 5% hydrogen peroxide, under 300 ℃, etching is 180 minutes in the teflon-lined autoclave, and is dry after the washing;
(2) thermolysis: with step (1) products therefrom under the oxygen atmosphere, in 800 ℃ of pyrolysis 120 minutes;
(3) aftertreatment: step (2) products therefrom in reactor, is added 10g ammoniacal liquor, 10g thanomin, 10g stearylamine, 10g Tetramethylammonium hydroxide, and in 60 ℃ of hydrothermal treatment consists 300 minutes, washing, drying obtained electron grade spherical silicon micropowder.
Adopt 7500 type inductively coupled plasma atomic mass spectrometries (Agilent company, the U.S.) technical testing, its purity reaches 4N, and the content situation of impurity element sees Table 3.By electron microscopic observation, particle diameter is about 100nm, and electromicroscopic photograph as shown in figure 11.
Embodiment 12
(1) pre-treatment: after the abundant drying of 1000g straw, remove dust impurity by vibratory screening apparatus again, then be ground into 20 order rice straw powders, the rice straw powder adding of 1000g is contained in the 6000g aqueous solution of 2% hydrochloric acid, 0.5% sulfuric acid, 1% nitric acid and 5% dioxide peroxide, under 250 ℃, etching is 120 minutes in the teflon-lined autoclave, and is dry after the washing;
(2) thermolysis: with step (1) products therefrom under the oxygen atmosphere, in 800 ℃ of pyrolysis 180 minutes;
(3) aftertreatment: step (2) products therefrom in reactor, is added 5g ammoniacal liquor, 5g diethanolamine, 5g Tetramethylammonium hydroxide, 1g TBAH, and in 300 ℃ of hydrothermal treatment consists 120 minutes, washing, drying obtained electron grade spherical silicon micropowder.
Adopt 7500 type inductively coupled plasma atomic mass spectrometries (Agilent company, the U.S.) technical testing, its purity reaches 3N, and the content situation of impurity element sees Table 3.By electron microscopic observation, particle diameter is about 160nm, and electromicroscopic photograph as shown in figure 12.
The composition of table 3 embodiment 1～12 gained silicon powder
As can be seen from Table 3, the electron grade spherical silicon micropowder purity of the present invention's preparation reaches 99.99%.
Can be found out that by Fig. 1～12 the electron grade spherical silicon micropowder particle diameter of the present invention's preparation is controlled, its particle size range is 10～300nm.
Claims (5)
1. a method of utilizing straw to prepare electron grade spherical silicon micropowder is characterized in that, may further comprise the steps:
(1) pre-treatment: after the abundant drying of straw, remove dust impurity, then be ground into 20 orders ~ 40 purpose rice straw powders, rice straw powder is added in the acid aqueous solution of oxidisability, in 80～300 ℃ of etchings 30～60 minutes, dry after the washing;
(2) thermolysis: with step (1) products therefrom under oxygen or air atmosphere, in 600～900 ℃ of pyrolysis 120～300 minutes;
(3) aftertreatment: add constitution controller in step (2) products therefrom, in 60～300 ℃ of hydrothermal treatment consists 30～300 minutes, washing, drying obtained electron grade spherical silicon micropowder.
2. method according to claim 1, it is characterized in that, in the step (1), the acid solution of described oxidisability is the combination solution of a kind of composition in strong acid and hydrogen peroxide or the dioxide peroxide, and described strong acid is one or more in sulfuric acid, hydrochloric acid, nitric acid or the perchloric acid.
3. method according to claim 2 is characterized in that, in the step (1), the mass concentration of each component is 0.1～10% in the acid solution of described oxidisability, and the mass ratio of the acid solution of described oxidisability and rice straw powder is (3 ~ 10): 1.
4. method according to claim 3, it is characterized in that, in the step (3), described constitution controller is one or more in ammoniacal liquor, thanomin, Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH, TBAH, methylamine, ethamine, quadrol, triethylene tetramine, tetraethylene pentamine, cetylamine, stearylamine, hydroxyethyl ethamine, palmityl trimethyl ammonium chloride, cetyl trimethylammonium bromide, cetylpyridinium chloride, polyacrylic acid, polymethyl acrylic acid or the polyvinylpyrrolidone.
5. method according to claim 4 is characterized in that, in the step (3), the mass ratio of rice straw powder is (0.1～5) described in described constitution controller and the step (1): 100.
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| CN103710023A (en) * | 2013-12-04 | 2014-04-09 | 华南理工大学 | Method for preparing porous photoluminescence material by utilization of rice husks |
| CN109384244A (en) * | 2018-12-29 | 2019-02-26 | 黄冈师范学院 | A kind of process using industrial silicon ash oxidation purification fine silica powder |
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| CN1962438A (en) * | 2006-11-16 | 2007-05-16 | 华南理工大学 | Method for preparing electron grade spherical silicon micropowder using rice hull |
| US20090148578A1 (en) * | 2005-08-31 | 2009-06-11 | Katsuyoshi Kondoh | Amorphous silicon powder and its production method |
| CN101528601A (en) * | 2006-10-27 | 2009-09-09 | 株式会社栗本铁工所 | Amorphous silica and process for production thereof |
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| US20090148578A1 (en) * | 2005-08-31 | 2009-06-11 | Katsuyoshi Kondoh | Amorphous silicon powder and its production method |
| CN101528601A (en) * | 2006-10-27 | 2009-09-09 | 株式会社栗本铁工所 | Amorphous silica and process for production thereof |
| CN1962438A (en) * | 2006-11-16 | 2007-05-16 | 华南理工大学 | Method for preparing electron grade spherical silicon micropowder using rice hull |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103710023A (en) * | 2013-12-04 | 2014-04-09 | 华南理工大学 | Method for preparing porous photoluminescence material by utilization of rice husks |
| CN109384244A (en) * | 2018-12-29 | 2019-02-26 | 黄冈师范学院 | A kind of process using industrial silicon ash oxidation purification fine silica powder |
| CN109384244B (en) * | 2018-12-29 | 2022-03-04 | 黄冈师范学院 | Process method for purifying silica micropowder by using industrial silica fume oxidation |
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Application publication date: 20130213 |