CN101880044A - Method for preparing solar grade silicon by disproportionation reaction - Google Patents
Method for preparing solar grade silicon by disproportionation reaction Download PDFInfo
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- CN101880044A CN101880044A CN2010102023438A CN201010202343A CN101880044A CN 101880044 A CN101880044 A CN 101880044A CN 2010102023438 A CN2010102023438 A CN 2010102023438A CN 201010202343 A CN201010202343 A CN 201010202343A CN 101880044 A CN101880044 A CN 101880044A
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Abstract
The invention relates to a method for preparing solar grade silicon by disproportionation reaction, which is characterized by comprising the following steps of: (1) crushing silicon dioxide and industrial silicon into fine powder respectively with a jet mill; (2) soaking the fine powder into concentrated nitric acid respectively; (3) filtering nitric acid off, flushing the fine powder with purified water, and heating and drying the fine powder in a vacuum chamber; (4), (5) mixing the dried fine powder of the silicon dioxide and the industrial silicon in a molar ratio of 1:1, and consolidating the mixture into blocks with a vacuum hot isostatic pressing device; (6) placing the mixed and consolidated blocks of the silicon dioxide and the industrial silicon after hot-pressing molding into a connection type vacuum high temperature disproportionation reactor to carry out the disproportionation reaction and prepare the solar grade silicon of which the purity reaches 6N. The solar grade silicon can also be prepared by mixing the two kinds of fine powder in a molar ratio of 1:1, and soaking the mixture with the nitric acid; then filtering, flushing, and drying the mixture, and hot-pressing the mixture into blocks; and finally feeding the mixture into the disproportionation reactor to carry out the disproportionation reaction. The method not only saves equipment investment, but also reduces production cost.
Description
Technical field
The invention belongs to the technical field of the purifying of silicon, be specifically related to a kind of method of utilizing the silicon monoxide disproportionation reaction to produce polycrystalline silicon used for solar battery.
Background technology
Polycrystalline silicon used for solar battery must be that content of impurities is lower than the HIGH-PURITY SILICON that 1ppmw, purity reach 6N (being 99.9999wt%), when making solar cell with its, can guarantee to reach needed photoelectric transformation efficiency; And tangible decay can not take place in the life-time service process.
For many years, the method that each major company of the world produces solar energy level silicon mainly is a Siemens Method, instant heating chemical vapor deposition (CVD) method.The technical process of this method is: the first step generates trichlorosilane or silicon tetrachloride with hydrochloric acid or chlorine with the industrial silicon reaction; Second step was used distillation method purify trichlorosilane or silicon tetrachloride; The 3rd step obtained HIGH-PURITY SILICON at indoor hydrogen reducing trichlorosilane of reduction or silicon tetrachloride.For China, main problem just goes out on the 3rd step reduction reaction, and the one, recovery rate is less than 20%; The 2nd, the not remaining hypertoxic trichlorosilane of complete reaction, silicon tetrachloride and inflammable, the explosive not easily separated and processing of hydrogen.At present, the newly-built how tame large polycrystalline silicon factory of China is all because fail to grasp the core technology of Siemens Method, and consequently environmental pollution is serious and be forced to stop production, and exhausts the people and drains the treasury, and but can not get the benefit of expecting.In recent years, because the promotion of world energy sources crisis and low-carbon economy development, various countries are to the equal pay attention to day by day of photovoltaic industry, thereby make the demand of solar energy level silicon increase sharply, and price is sharply soaring, and high always.The novel method of producing solar energy level silicon of seeking the photovoltaic industry development of more suitable China just seems very important under these circumstances!
Chinese patent ZL200710012825.5 has proposed " a kind of method for manufacturing polycrystalline silicon used for solar battery ", in this patent, we have adopted the means of silicon monoxide disproportionation reaction, acid dipping separation and vacuum melting, and successfully the method that combines with chemistry-physics has been produced the polysilicon of 6N level.Owing to discarded boron and two kinds of structural impurity of phosphorus (being lattice impurity) in the chlorination that Siemens Method adopted, the distillation means removal silicon, both reduced production cost; Eliminate environmental pollution again, had splendid social benefit and economic benefit.
Yet in the scale operation practice of implementing this patent, we find further to simplify its production process.Like this, guaranteeing under the product quality premise, can also save facility investment greatly and reduce production costs, obtaining better economic benefit.
Summary of the invention
The objective of the invention is on the basis of Chinese patent ZL200710012825.5, the new solar-grade polysilicon production technique of invention one cover, by simplifying production process, do not influencing under the product quality premise, in order to saving facility investment greatly and to reduce the production cost of polysilicon, thereby promote the sound development of China's photovoltaic industry.
The disproportionation reaction preparing process of solar energy level silicon proposed by the invention is characterized in that it is made up of following steps:
(1) silicon-dioxide and industrial silicon are become the micro mist of silicon-dioxide and industrial silicon with the airflow milling separated pulverizing, make its granularity reach 50～200 orders;
(2) silicon-dioxide after will pulverizing and industrial silicon micro mist place concentrated nitric acid to soak respectively and stirred 1～4 hour;
(3) behind the elimination nitric acid, handle silicon-dioxide later and industrial silicon micro mist with purified rinse water more than 1 hour through concentrated nitric acid with above-mentioned,, heating, drying in vacuum chamber again;
(4) with dried silicon dioxide and 1: 1 in molar ratio proportioning uniform mixing of industrial silicon micro mist;
(5) silicon-dioxide that mixes and industrial silicon micro mist are packed in the jacket, the hot pressing of reusable heat isopressing device is consolidated into piece;
(6) place connected vacuum high-temperature disproportionated reaction device to carry out disproportionation reaction the silicon-dioxide after hot-forming, industrial silicon mixing knot and produce the solar energy level silicon that purity reaches 6N.
In the above-mentioned steps (two), because silicon and silicon-dioxide is all water insoluble and nitric acid, and after boron and phosphorus soaks through concentrated nitric acid, then can separate out by following Reaction Separation:
B+3HNO
3(dense)=H
3BO
3+ 3NO
2
P+5HNO
3(dense)=H
3PO
4+ 5NO
2+ H
2O
Pressure in vacuum tank in the above-mentioned steps (three) is 10
-2Holder, bake out temperature are 150～250 ℃, are incubated 1～4 hour.
Pressure in the above-mentioned steps (five) in the jacket is 10
-2Holder, hip temperature is 700～1000 ℃, pressure is 50～120 MPas.
Above-mentioned steps (six) is to carry out in the connected vacuum high-temperature disproportionated reaction device that Chinese patent ZL201020111092.8 is provided, and its first Reaktionsofen pressure is 1 * 10
-4Holder, temperature is 1250～1300 ℃; The second Reaktionsofen pressure is 1 * 10
-5Holder, temperature is 1450～1500 ℃.
Above-mentioned steps of the present invention (two), (three) and (four), promptly the fine silica powder after pulverizing and industrial silicon micro mist respectively through concentrated nitric acid soak, filter, clean, oven dry and 1: 1 in molar ratio batch mixes evenly, carry out the fixed caked operation of hot isostatic pressing behind the jacket; Also can change over 1: 1 in molar ratio earlier with after fine silica powder and the industrial silicon micro mist batch mixes, soak, filter, clean, dry the back jacket through concentrated nitric acid again and carry out the fixed caked operation of hot isostatic pressing, but the order of connection of its each step and corresponding processing parameter are still constant.
This shows, technical scheme with Chinese patent 200710012825.5 is compared, the present invention has saved operations such as the melting of vacuum electron beam stove, plasma heating furnace melting and directional freeze in producing the production technique of solar energy level silicon, saved facility investment and production cost greatly.
Description of drawings
Fig. 1 soaks, filters, cleans, dries and be consolidated into the process flow sheet that piece carries out disproportionation reaction through hot isostatic pressing again after the batch mixes in 1: 1 in molar ratio through concentrated nitric acid respectively for the fine silica powder after will pulverizing and industrial silicon micro mist; Fig. 2 is after will pulverizing 1: 1 in molar ratio batch mixes of back fine silica powder and industrial silicon micro mist, soaks, filters, cleans, is consolidated into the process flow sheet that piece carries out disproportionation reaction through hot isostatic pressing again after the oven dry through concentrated nitric acid.
Embodiment
Below in conjunction with Figure of description and embodiment content of the present invention is further described and replenishes.
Embodiment 1 its technical process as shown in Figure 1
Step 1: adopt SiO
2Content reaches the chemical grade industrial silicon that the quartzy piece of 99.98% melting and purity reaches more than 99.68% and makes raw material, with airflow milling they is ground into 50～100 purpose micro mists respectively;
Step 2: quartzy micro mist of the melting after will pulverizing and chemical grade industrial silicon micro mist place concentrated nitric acid to soak respectively and stirred 1～3 hour;
Step 3: behind the elimination nitric acid, above-mentioned melting crystal micro mist and the chemical grade industrial silicon micro mist of handling later through concentrated nitric acid used purified rinse water respectively 4～6 hours,, be 1 * 10 at pressure again
-2Be heated to 150～200 ℃ of bakings in the vacuum chamber of holder, be incubated 3～4 hours;
Step 4, five: quartzy micro mist of the melting after will drying and 1: 1 in molar ratio proportioning batch mixing of chemical grade industrial silicon micro mist, in the jacket of packing into, the pressure in the jacket is 5 * 10
-2Holder is carried out hot isostatic pressing and is become piece under the condition of 700 ℃ of temperature, pressure 120 MPas, make its density reach 2.2～2.3 gram/cm
3
Step 6: in above-mentioned first Reaktionsofen that places the connected vacuum high-temperature disproportionated reaction device that Chinese patent ZL201020111092.8 provided through hip treatment hot isostatic pressing piece later, by the following reaction that in first Reaktionsofen, is taken place:
SiO
2+Si＝2SiO
With the following reaction that takes place in second Reaktionsofen:
2SiO＝Si+SiO
2
Produce solar-grade polysilicon.In the production process, the pressure in first Reaktionsofen is 1 * 10
-4Holder, temperature is 1250～1300 ℃; Pressure is 1 * 10 in second Reaktionsofen
-5Holder, temperature is 1450～1500 ℃.
Embodiment 2 its technical process as shown in Figure 2
Step 1: adopt SiO
2Content reaches the chemical grade industrial silicon that 99.98% high purity quartz piece and purity reaches more than 99.68% and makes raw material, with airflow milling they is ground into 100～200 purpose micro mists respectively;
Step 2: after above-mentioned two kinds of powder 1: 1 are in molar ratio mixed, place concentrated nitric acid to soak and stirred 1～3 hour;
Step 3: behind the elimination nitric acid, above-mentioned powder is used purified rinse water 4～6 hours,, be 2 * 10 at pressure again
-2Be heated to 150～200 ℃ of bakings in the vacuum chamber of holder, be incubated 3～4 hours;
Step 4, five: the powder after the above-mentioned oven dry is packed in the jacket, and pressure is 2 * 10 in the jacket
-2Holder is carried out hot isostatic pressing and is become knot under the condition of 1000 ℃ of temperature, pressure 50 MPas, make its density reach 2.2～2.3 gram/cm
3
Step 6: in above-mentioned first Reaktionsofen that places the connected vacuum high-temperature disproportionated reaction device that Chinese patent ZL201020111092.8 provided through hip treatment quartz, industrial silicon mixing knot later, by the following reaction that in first Reaktionsofen, takes place:
SiO
2+Si＝2SiO
With the following reaction that takes place in second Reaktionsofen:
2SiO＝Si+SiO
2
Produce solar-grade polysilicon.In the production process, the pressure in first Reaktionsofen is 1 * 10
-4Holder, temperature is 1250～1300 ℃; Pressure is 1 * 10 in second Reaktionsofen
-5Holder, temperature is 1450～1500 ℃.
Embodiment 3 its technical process as shown in Figure 1
Step 1: adopt SiO
2Content reaches the chemical grade industrial silicon that 99.98% high purity quartz piece and purity reaches more than 99.68% and makes raw material, with airflow milling they is ground into 100～150 purpose micro mists respectively;
Step 2: high purity quartz micro mist after will pulverizing and chemical grade industrial silicon micro mist place concentrated nitric acid to soak respectively and stirred 2～4 hours;
Step 3: behind the elimination nitric acid, used purified rinse water respectively 4～6 hours through concentrated nitric acid processing high purity quartz micro mist and chemical grade industrial silicon micro mist later with above-mentioned,, be 5 * 10 at pressure again
-2Be heated to 200～250 ℃ of bakings in the vacuum chamber of holder, be incubated 3～4 hours;
Step 4, five: high purity quartz micro mist after will drying and 1: 1 in molar ratio proportioning batch mixing of chemical grade industrial silicon micro mist, in the jacket of packing into, pressure is 1 * 10 in the jacket
-2Holder is carried out hot isostatic pressing and is become piece under the condition of 800 ℃ of temperature, pressure 100 MPas, make its density reach 2.3～2.4 gram/cm
3
Step 6: in above-mentioned first Reaktionsofen that places the connected vacuum high-temperature disproportionated reaction device that Chinese patent ZL201020111092.8 provided through hip treatment quartz, industrial silicon mixing knot later, by the following reaction in first Reaktionsofen:
SiO
2+Si＝2SiO
With the following reaction in second Reaktionsofen:
2SiO＝Si+SiO
2
Produce solar-grade polysilicon.In the production process, the pressure in first Reaktionsofen is 1 * 10
-4Holder, temperature is 1250～1300 ℃; Pressure is 1 * 10 in second Reaktionsofen
-5Holder, temperature is 1450～1500 ℃.
Embodiment 4 its technical process as shown in Figure 2
Step 1: adopt SiO
2Content reaches the chemical grade industrial silicon that the quartzy piece of 99.98% melting and purity reaches more than 99.68% and makes raw material, with airflow milling they is ground into 100～200 purpose micro mists respectively;
Step 2: after above-mentioned two kinds of powder 1: 1 are in molar ratio mixed, place concentrated nitric acid to soak and stirred 1～3 hour;
Step 3: behind the elimination nitric acid, above-mentioned powder is used purified rinse water 5～8 hours,, be 2 * 10 at pressure again
-2Be heated to 200～250 ℃ of bakings in the vacuum chamber of holder, be incubated 1～3 hour;
Step 4, five: the powder after the above-mentioned oven dry is packed in the jacket, and the pressure in the jacket is 5 * 10
-2Holder is carried out hot isostatic pressing and is become knot under the condition of 900 ℃ of temperature, pressure 80 MPas, make its density reach 2.1～2.2 gram/cm
3
Step 6: in above-mentioned first Reaktionsofen that places the connected vacuum high-temperature disproportionated reaction device that Chinese patent ZL201020111092.78 provided through hip treatment crystal, industrial silicon mixing knot later, by the following reaction in first Reaktionsofen:
SiO
2+Si＝2SiO
With the following reaction in second Reaktionsofen:
2SiO＝Si+SiO
2
Produce solar-grade polysilicon.In the production process, the pressure in first Reaktionsofen is 1 * 10
-4Holder, temperature is 1250～1300 ℃; Pressure is 1 * 10 in second Reaktionsofen
-5Holder, temperature is 1450～1500 ℃.
Embodiment 5 its technical process as shown in Figure 1
Step 1: adopt SiO
2Content reaches the chemical grade industrial silicon that 99.98% high purity quartz piece and purity reaches more than 99.68% and makes raw material, with airflow milling they is ground into 100～150 purpose micro mists respectively;
Step 2: high purity quartz micro mist after will pulverizing and chemical grade industrial silicon micro mist place concentrated nitric acid to soak respectively and stirred 2～4 hours;
Step 3: behind the elimination nitric acid, used purified rinse water respectively 4～6 hours through concentrated nitric acid processing high purity quartz micro mist and chemical grade industrial silicon micro mist later with above-mentioned,, be 1 * 10 at pressure again
-2Be heated to 200～250 ℃ of bakings in the vacuum chamber of holder, be incubated 1～3 hour;
Step 4, five: high purity quartz micro mist after will drying and 1: 1 in molar ratio proportioning batch mixing of chemical grade industrial silicon micro mist, in the jacket of packing into, the pressure in the jacket is 2 * 10
-2Holder is carried out hot isostatic pressing and is become piece under the condition of 800 ℃ of temperature, pressure 100 MPas, make its density reach 2.3～2.4 gram/cm
3
Step 6: in above-mentioned first Reaktionsofen that places the connected vacuum high-temperature disproportionated reaction device that Chinese patent ZL201020111092.8 provided through hip treatment quartz, industrial silicon mixing knot later, by the following reaction in first Reaktionsofen:
SiO
2+Si＝2SiO
With the following reaction in second Reaktionsofen:
2SiO＝Si+SiO
2
Produce solar-grade polysilicon.In the production process, the pressure in first Reaktionsofen is 1 * 10
-4Holder, temperature is 1250～1300 ℃; Pressure is 1 * 10 in second Reaktionsofen
-5Holder, temperature is 1450～1500 ℃.
Embodiment 6 its technical process as shown in Figure 2
Step 1: adopt SiO
2Content reaches the chemical grade industrial silicon that the quartzy piece of 99.98% melting and purity reaches more than 99.68% and makes raw material, with airflow milling they is ground into 100～200 purpose micro mists respectively;
Step 2: after above-mentioned two kinds of powder 1: 1 are in molar ratio mixed, place concentrated nitric acid to soak and stirred 2～4 hours;
Step 3: behind the elimination nitric acid, above-mentioned powder is used purified rinse water 5～8 hours,, be 2 * 10 at pressure again
-2Be heated to 200～250 ℃ of bakings in the vacuum chamber of holder, be incubated 3～4 hours;
Step 4, five: the powder after the above-mentioned oven dry is packed in the jacket, and the pressure in the jacket is 1 * 10
-2Holder is carried out hot isostatic pressing and is become knot under the condition of 900 ℃ of temperature, pressure 100 MPas, make its density reach 2.2～2.3 gram/cm
3
Step 6: in above-mentioned first Reaktionsofen that places the connected vacuum high-temperature disproportionated reaction device that Chinese patent ZL201020111092.78 provided through hip treatment fusion crystal, industrial silicon mixing knot later, by the following reaction in first Reaktionsofen:
SiO
2+Si＝2SiO
With the following reaction in second Reaktionsofen:
2SiO＝Si+SiO
2
Produce solar-grade polysilicon.In the production process, the pressure in first Reaktionsofen is 1 * 10
-4Holder, temperature is 1250～1300 ℃; Pressure is 1 * 10 in second Reaktionsofen
-5Holder, temperature is 1450～1500 ℃.
The present invention ties up on the basis of Chinese patent 200710012825.5, by the significant improvement of after the further commerical test above-mentioned patent having been done.The contriver finds in test: as long as in process of production, with raw material process abundant pulverizing back and through nitric acid treatment, just can make two kinds of lattice impurities of boron and phosphorus remove most, by the silicon monoxide disproportionation reaction it is separated fully with silicon it again, thus, even if saved removal of impurities operations such as original vacuum high-temperature smelting and directional freeze, can obtain the polycrystalline silicon used for solar battery material that purity reaches the 6N level equally.And adopt the vacuum heat and other static pressuring processes to make fine silica powder become knot with industrial silicon micro mist mixture, and carry out the disproportionation reaction operation again, not only can prevent powder splashing in the disproportionation reaction stove effectively, but also can improve the production efficiency of dismutation furnace.Above-mentioned these great technological improvements have brought huge economic benefit for the production of solar-grade polysilicon, have great application value.
Claims (8)
1. the disproportionation reaction preparing process of a solar energy level silicon is characterized in that it is made up of following steps:
(1) silicon-dioxide and industrial silicon are become the micro mist of silicon-dioxide and industrial silicon with the airflow milling separated pulverizing, make its granularity reach 50～200 orders;
(2) silicon-dioxide after will pulverizing and industrial silicon micro mist place concentrated nitric acid to soak respectively and stirred 1～4 hour;
(3) behind the elimination nitric acid, handle silicon-dioxide later and industrial silicon micro mist with purified rinse water more than 1 hour through concentrated nitric acid with above-mentioned,, heating, drying in vacuum chamber again;
(4) with dried silicon dioxide and 1: 1 in molar ratio proportioning uniform mixing of industrial silicon micro mist;
(5) silicon-dioxide that mixes and industrial silicon micro mist are packed in the jacket, be consolidated into piece with heat isostatic apparatus hot pressing;
(6) place connected vacuum high-temperature disproportionated reaction device to carry out disproportionation reaction the silicon-dioxide after hot-forming, industrial silicon mixing knot and produce the solar energy level silicon that purity reaches 6N.
2. by the disproportionation reaction preparing process of the described solar energy level silicon of claim 1, it is characterized in that the pressure in vacuum tank in the said step (three) is 10
-2Holder, bake out temperature are 150～250 ℃, are incubated 1～4 hour.
3. by the disproportionation reaction preparing process of the described solar energy level silicon of claim 1, it is characterized in that the pressure in the jacket is 10 in the said step (five)
-2Holder, hip temperature is 700～1000 ℃, pressure is 50～120 MPas.
4. by the disproportionation reaction preparing process of the described solar energy level silicon of claim 1, it is characterized in that its first Reaktionsofen pressure of connected vacuum high-temperature disproportionated reaction device in the said step (six) is 1 * 10
-4Holder, temperature is 1250～1300 ℃; The second Reaktionsofen pressure is 1 * 10
-5Holder, temperature is 1450～1500 ℃.
5. the disproportionation reaction preparing process of a solar energy level silicon is characterized in that it is made up of following steps:
(1) silicon-dioxide and industrial silicon are become the micro mist of silicon-dioxide and industrial silicon with the airflow milling separated pulverizing, make its granularity reach 50～200 orders;
(2) uniform mixing in addition after 1: 1 in molar ratio batching of silicon-dioxide after will pulverizing and industrial silicon micro mist;
(3) silicon-dioxide after will mixing and industrial silicon micro mist place concentrated nitric acid to soak and stirred 1～4 hour;
(4) behind the elimination nitric acid, handle silicon-dioxide later and industrial silicon mixture with purified rinse water more than 1 hour through concentrated nitric acid with above-mentioned,, heating, drying in vacuum chamber again;
(5) dried silicon dioxide and industrial silicon mixture are packed in the jacket, be hot pressed into knot with heat isostatic apparatus;
(6) place connected vacuum high-temperature disproportionated reaction device to carry out disproportionation reaction the silicon-dioxide after hot-forming, industrial silicon mixing knot and produce the solar energy level silicon that purity reaches 6N.
6. by the disproportionation reaction preparing process of the described solar energy level silicon of claim 5, it is characterized in that the pressure in vacuum tank in the said step (four) is 10
-2Holder, bake out temperature is 150～250 ℃, is incubated 1～4 hour.
7. by the disproportionation reaction preparing process of the described solar energy level silicon of claim 5, it is characterized in that the pressure in the jacket is 10 in the said step (five)
-2Holder, hip temperature is 700～1000 ℃, pressure is 50～120 MPas.
8. by the disproportionation reaction preparing process of the described solar energy level silicon of claim 5, it is characterized in that its first Reaktionsofen pressure of connected vacuum high-temperature disproportionated reaction device in the said step (six) is 1 * 10
-4Holder, temperature is 1250～1300 ℃; The second Reaktionsofen pressure is 1 * 10
-5Holder, temperature is 1450～1500 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530949A (en) * | 2012-03-02 | 2012-07-04 | 李绍光 | Electromagnetic suspension liquid-solid separation method and device |
| WO2016086502A1 (en) * | 2014-12-02 | 2016-06-09 | 李绍光 | Method for preparing solar grade silicon using silica |
| CN109175375A (en) * | 2018-08-07 | 2019-01-11 | 东营鲁知信息科技有限公司 | A kind of hot isostatic pressing acid-hatching of young eggs jacket removal device |
-
2010
- 2010-06-18 CN CN2010102023438A patent/CN101880044A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530949A (en) * | 2012-03-02 | 2012-07-04 | 李绍光 | Electromagnetic suspension liquid-solid separation method and device |
| WO2016086502A1 (en) * | 2014-12-02 | 2016-06-09 | 李绍光 | Method for preparing solar grade silicon using silica |
| CN105712349A (en) * | 2014-12-02 | 2016-06-29 | 李绍光 | Method for preparing solar-grade silicon by using silicon dioxide |
| CN109175375A (en) * | 2018-08-07 | 2019-01-11 | 东营鲁知信息科技有限公司 | A kind of hot isostatic pressing acid-hatching of young eggs jacket removal device |
| CN109175375B (en) * | 2018-08-07 | 2021-05-25 | 青岛绿谷知识产权有限公司 | Acid leaching method canning remove device for hot isostatic pressing |
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Application publication date: 20101110 |