CN102275928A - Method for preparing high-purity polycrystalline silicon from diatom - Google Patents
Method for preparing high-purity polycrystalline silicon from diatom Download PDFInfo
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- CN102275928A CN102275928A CN2011102340926A CN201110234092A CN102275928A CN 102275928 A CN102275928 A CN 102275928A CN 2011102340926 A CN2011102340926 A CN 2011102340926A CN 201110234092 A CN201110234092 A CN 201110234092A CN 102275928 A CN102275928 A CN 102275928A
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Abstract
The invention discloses a method for preparing high-purity polycrystalline silicon from diatom, which comprises the following steps: 1) fully grinding 100 grams of diatom, placing the ground diatom into a furnace at a temperature of 400 to 1,200 DEG C, calcining for 0.5 to 8 hours in an air or oxygen atmosphere, and obtaining SiO2 powder; and (2) soaking the SiO2 powder in diluted hydrochloric acid solution at a concentration of 0.1 to 1.0 mol/L for 1 to 24 hours, filtering, cleaning, drying at 60 to 150 DEG C, fully mixing the dried product with 2 to 10 grams of metal reducer powder, placing the mixture in a furnace, calcining for 0.5 to 12 hours at 500 to 800 DEG C in the absence of the air or under the protection of an inert gas, cooling, soaking in diluted hydrochloric acid solution at a concentration of 0.1 to 1.0 mol/L for 1 to 24 hours, drying and obtaining polycrystalline silicon with a purity of over 99 percent. The method for preparing high-purity polycrystalline silicon from diatom, which is provided by the invention, has the advantages that: the raw material cost is low; a process flow is simple; and the economic value and application prospect are excellent.
Description
Technical field
The present invention relates to the preparation method of compound, relate in particular to a kind of method for preparing high purity polycrystalline silicon from diatom.
Background technology
Diatom (Diatom) is the unicellular plant plankton that a class has siliceous housing, be under the jurisdiction of Bacillariophyta (
Bacillariophyta), often become colony by a plurality of groups of cells.Diatom is the important marine phytoplankton of a class, and it is extremely extensive to distribute, and almost has the place of water that diatom is promptly arranged.Diatom is a primary productivity important in the ocean, is other halobiontic main bait.Diatom after death, its siliceous housing will sink under water, through very long geological age gradually enrichment of ore-forming form diatomite.When ocean environment was subjected to eutrophication pollution, some diatom formed red tide with overproduction, and fishery and ecotope are caused great effect.Have not yet to see research for the diatom development and use.
Owing to contain a large amount of siliceous housings in the diatom, its exploitation of carrying out polysilicon had great application prospect.The application of high-purity polycrystalline (Si) is very extensive, and polysilicon is the core material of information industry.In polysilicon, mix the group III A element of trace, form p type silicon semiconductor; Mixing the VA family element of trace, form n type and p N-type semiconductorN and combine, will be excellent solar cell, be a kind of up-and-coming material aspect develop energy.With polysilicon and ceramic mixed sintering, inherited the advantage separately of metal and pottery, remedied both birth defects again, be sintering metal, cosmonautic important materials.At present the preparation polysilicon mainly adopts following method: 1. SiO
2Si+the 2Cl of+2C=Si+2CO ↑ 2.
2=SiCl
4SiCl
4+ 2H
2=Si+4HCl.These two kinds of methods all need hot environment (more than 1200 degree), thereby have limited the exploitation and the application of polysilicon.
Because diatom will be dissociated through the structure of its housing after the pyrolysis, loosely organized, impurity is wherein easily removed.For adding thermal medium and reductive agent, prepare polysilicon from diatom by magnesium or aluminium powder, not only significantly reduced the synthesis temperature of polysilicon, the purity of gained polysilicon helps directly using or carrying out further processing treatment more than 99%.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of method for preparing high purity polycrystalline silicon from diatom is provided.
The step of method for preparing high purity polycrystalline silicon from diatom is as follows:
1) 100 g diatoms is fully pulverized, put into 400～1200
oUnder air or oxygen atmosphere, calcine 0.5～8 h in the C stove, obtain SiO
2Powder;
2) with SiO
2Powder soaks 1～24 h in the dilute hydrochloric acid solution of 0.1～1.0 mol/L, filter, and cleans 60～150
oStove is put in C oven dry back and 2～10 g metallic reducing agent powder thorough mixing, secluding air or under the protection of rare gas element 500～800
oC calcines 0.5～12 h; 1～24 h is soaked in cooling in the dilute hydrochloric acid solution of 0.1～1.0 mol/L, oven dry promptly gets purity and surpasses 99% polysilicon.
Described diatom is the single-cell sea plant plankton with siliceous housing; Described metallic reducing agent is one or both in simple substance magnesium powder or the aluminium powder; Described rare gas element is high pure nitrogen or high-purity argon gas.
What the present invention proposed prepares the method for high purity polycrystalline silicon from diatom, and material cost is cheap, and technical process is simple; Because diatom is through loosely organized after the pyrolysis, impurity is wherein easily removed, so the purity of gained polysilicon helps directly using or carrying out further processing treatment more than 99%; The method that the present invention proposes has extremely strong economic worth and application prospect.
Embodiment
The step of method for preparing high purity polycrystalline silicon from diatom is as follows:
1) 100 g diatoms is fully pulverized, put into 400～1200
oUnder air or oxygen atmosphere, calcine 0.5～8 h in the C stove, obtain SiO
2Powder;
2) with SiO
2Powder soaks 1～24 h in the dilute hydrochloric acid solution of 0.1～1.0 mol/L, filter, and cleans 60～150
oStove is put in C oven dry back and 2～10 g metallic reducing agent powder thorough mixing, secluding air or under the protection of rare gas element 500～800
oC calcines 0.5～12 h; 1～24 h is soaked in cooling in the dilute hydrochloric acid solution of 0.1～1.0 mol/L, oven dry promptly gets purity and surpasses 99% polysilicon.
Described diatom is the single-cell sea plant plankton with siliceous housing; Described metallic reducing agent is one or both in simple substance magnesium powder or the aluminium powder; Described rare gas element is high pure nitrogen or high-purity argon gas.
The reaction equation following (is example with the magnesium powder) that the present invention is concrete:
SiO
2?+?2Mg?→?Si?+?2MgO
Si+2Mg → Mg
2Si(association reaction)
Impurity such as the magnesium oxide that generates, magnesium silicide can soak by dilute hydrochloric acid equally to be removed.Promptly get purity after the oven dry and surpass 99% polysilicon.
Further specify the present invention below in conjunction with embodiment.
Embodiment 1:
1) 100 g diatoms is fully pulverized, put into 400
oCalcine 8 h in the C stove under air or oxygen atmosphere, obtaining main component is SiO
2Powder;
2) with gained SiO
2Powder soaks 24 h in the dilute hydrochloric acid solution of 0.1 mol/L, to remove impurity wherein; After the end with product 60
oStove is put in C oven dry back and 2 g metal magnesium powder thorough mixing, secluding air or under the protection of rare gas element 500
oC calcines 12 h; Take out the cooling back, soaks 24 h in the dilute hydrochloric acid solution of 0.1 mol/L, promptly gets purity and surpass 99% polysilicon.
Embodiment 2:
1) 100 g diatoms is fully pulverized, put into 1200
oCalcine 0.5 h in the C stove under air or oxygen atmosphere, obtaining main component is SiO
2Powder;
2) with gained SiO
2Powder soaks 1 h in the dilute hydrochloric acid solution of 1.0 mol/L, to remove impurity wherein; After the end with product 150
oStove is put in C oven dry back and 10 g metallic aluminium powder thorough mixing, secluding air or under the protection of rare gas element 800
oC calcines 0.5 h; Take out the cooling back, soaks 1 h in the dilute hydrochloric acid solution of 1.0 mol/L, promptly gets purity and surpass 99% polysilicon.
Embodiment 3:
1) 100 g diatoms is fully pulverized, put into 500
oCalcine 6 h in the C stove under air or oxygen atmosphere, obtaining main component is SiO
2Powder;
2) with gained SiO
2Powder soaks 18 h in the dilute hydrochloric acid solution of 0.2 mol/L, to remove impurity wherein; After the end with product 70
oStove is put in C oven dry back and 4 g metal magnesium powder thorough mixing, secluding air or under the protection of rare gas element 600
oC calcines 8 h; Take out the cooling back, soaks 18 h in the dilute hydrochloric acid solution of 0.2 mol/L, promptly gets purity and surpass 99% polysilicon.
Embodiment 4:
1) 100 g diatoms is fully pulverized, put into 600
oCalcine 4 h in the C stove under air or oxygen atmosphere, obtaining main component is SiO
2Powder;
2) with gained SiO
2Powder soaks 15 h in the dilute hydrochloric acid solution of 0.3 mol/L, to remove impurity wherein; After the end with product 90
oStove is put in C oven dry back and 6 g metallic aluminium powder thorough mixing, secluding air or under the protection of rare gas element 700
oC calcines 6 h; Take out the cooling back, soaks 15 h in the dilute hydrochloric acid solution of 0.3 mol/L, promptly gets purity and surpass 99% polysilicon.
Embodiment 5:
1) 100 g diatoms is fully pulverized, put into 700
oCalcine 3 h in the C stove under air or oxygen atmosphere, obtaining main component is SiO
2Powder;
2) with gained SiO
2Powder soaks 12 h in the dilute hydrochloric acid solution of 0.5 mol/L, to remove impurity wherein; After the end with product 100
oStove is put in C oven dry back and 8 g metal magnesium powder thorough mixing, secluding air or under the protection of rare gas element 650
oC calcines 9 h; Take out the cooling back, soaks 12 h in the dilute hydrochloric acid solution of 0.5 mol/L, promptly gets purity and surpass 99% polysilicon.
Embodiment 6: be raw material with the diatom
1) 100 g straws is fully pulverized, put into 1000
oCalcine 2 h in the C stove under air or oxygen atmosphere, obtaining main component is SiO
2Powder;
2) with gained SiO
2Powder soaks 5 h in the dilute hydrochloric acid solution of 0.8 mol/L, to remove impurity wherein; After the end with product 120
oStove is put in C oven dry back and 5 g metallic aluminium powder thorough mixing, secluding air or under the protection of rare gas element 750
oC calcines 3 h; Take out the cooling back, soaks 5 h in the dilute hydrochloric acid solution of 0.8 mol/L, promptly gets purity and surpass 99% polysilicon.
Claims (4)
1. one kind prepares the method for high purity polycrystalline silicon from diatom, it is characterized in that its step is as follows:
1) 100 g diatoms is fully pulverized, put into 400～1200
oUnder air or oxygen atmosphere, calcine 0.5～8 h in the C stove, obtain SiO
2Powder;
2) with SiO
2Powder soaks 1～24 h in the dilute hydrochloric acid solution of 0.1～1.0 mol/L, filter, and cleans 60～150
oStove is put in C oven dry back and 2～10 g metallic reducing agent powder thorough mixing, secluding air or under the protection of rare gas element 500～800
oC calcines 0.5～12 h; 1～24 h is soaked in cooling in the dilute hydrochloric acid solution of 0.1～1.0 mol/L, oven dry promptly gets purity and surpasses 99% polysilicon.
2. according to claim 1ly a kind ofly prepare the method for high purity polycrystalline silicon, it is characterized in that described diatom is the single-cell sea plant plankton with siliceous housing from diatom.
3. according to claim 1ly a kind ofly prepare the method for high purity polycrystalline silicon, it is characterized in that described metallic reducing agent is one or both in simple substance magnesium powder or the aluminium powder from diatom.
4. according to claim 1ly a kind ofly prepare the method for high purity polycrystalline silicon, it is characterized in that described rare gas element is high pure nitrogen or high-purity argon gas from diatom.
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102602945A (en) * | 2012-03-20 | 2012-07-25 | 上海交通大学 | Method for preparing porous silicon |
| CN107555436A (en) * | 2017-09-06 | 2018-01-09 | 中国科学院广州地球化学研究所 | The method and product of fibrous nano silicon materials are prepared using sepiolite as raw material |
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|---|---|---|---|---|
| CN101533907A (en) * | 2009-04-14 | 2009-09-16 | 北京科技大学 | Method for preparing silicon-based anode material of lithium-ion battery |
| CN101830473A (en) * | 2010-06-03 | 2010-09-15 | 张鹏 | Method for preparing silicon dioxide aerogel by taking diatoms as raw materials |
| CN102145890A (en) * | 2011-04-30 | 2011-08-10 | 南京大学 | Preparation method of hollow spherical silicon nanomaterial |
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2011
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101533907A (en) * | 2009-04-14 | 2009-09-16 | 北京科技大学 | Method for preparing silicon-based anode material of lithium-ion battery |
| CN101830473A (en) * | 2010-06-03 | 2010-09-15 | 张鹏 | Method for preparing silicon dioxide aerogel by taking diatoms as raw materials |
| CN102145890A (en) * | 2011-04-30 | 2011-08-10 | 南京大学 | Preparation method of hollow spherical silicon nanomaterial |
Non-Patent Citations (1)
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| ZHIHAO BAO等: "Chemical reduction of three-dimensional silica micro-assemblies into microporous silicon replicas", 《NATURE》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102602945A (en) * | 2012-03-20 | 2012-07-25 | 上海交通大学 | Method for preparing porous silicon |
| CN102602945B (en) * | 2012-03-20 | 2014-02-19 | 上海交通大学 | Method for preparing porous silicon |
| CN107555436A (en) * | 2017-09-06 | 2018-01-09 | 中国科学院广州地球化学研究所 | The method and product of fibrous nano silicon materials are prepared using sepiolite as raw material |
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Application publication date: 20111214 |