CN115385339A - Preparation method of ultrapure silicon for solar photovoltaic industry - Google Patents
Preparation method of ultrapure silicon for solar photovoltaic industry Download PDFInfo
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- CN115385339A CN115385339A CN202111169413.9A CN202111169413A CN115385339A CN 115385339 A CN115385339 A CN 115385339A CN 202111169413 A CN202111169413 A CN 202111169413A CN 115385339 A CN115385339 A CN 115385339A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/023—Preparation by reduction of silica or free silica-containing material
- C01B33/025—Preparation by reduction of silica or free silica-containing material with carbon or a solid carbonaceous material, i.e. carbo-thermal process
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/037—Purification
- C01B33/039—Purification by conversion of the silicon into a compound, optional purification of the compound, and reconversion into silicon
Abstract
The invention discloses a preparation method of ultrapure silicon for solar photovoltaic industry, which comprises the following steps: s1, selecting materials, namely selecting 10-20 parts of quartz stone ore in a quartz stone pit, and detecting and selecting the quartz stone ore with the silicon dioxide content of more than 90%; s2, putting the raw materials in the step S1 into a special cleaning container, and continuously overturning, cleaning and drying the raw materials by using a high-pressure water gun; s3, putting the cleaned raw materials in the S2 into a crusher to be crushed to obtain 10-20 parts of quartz powder materials; s4, putting the raw materials in the step S3 into a quartz calcining furnace, removing air in the furnace by using nitrogen, and calcining for 3-6 hours at 950-1050 ℃; the preparation method is adopted to produce the ultra-pure silicon material, the ultra-pure silicon material is used to produce the solar photovoltaic product, the development requirements of the domestic solar photovoltaic industry and other high and new technology industries are met, and the passive situation that the ultra-pure silicon material required by the solar photovoltaic industry depends on import is broken.
Description
Technical Field
The invention relates to the technical field of preparation of ultrapure silicon, in particular to a preparation method of ultrapure silicon for solar photovoltaic industry.
Background
The ultra-pure silicon material for the solar photovoltaic industry is an upstream material in the high and new technical fields of semiconductor electronic technology, optical fiber communication, special light sources, aerospace, national defense and military industry and the like, the industry supported by the ultra-pure silicon material reaches trillion dollars, the ultra-pure silicon material for producing solar photovoltaic products always depends on import, and the rapid development and the technical promotion of the related high and new technical industry in China are seriously restricted. At present, the domestic ultra-pure silicon material for the solar photovoltaic industry is not produced in batches, and if the ultra-pure silicon material cannot meet the advanced level of the world, the further development and technical promotion of the high and new technology industry in China are bound to be restrained. With the rapid development of computer market and network information technology market, the CPU collection degree is getting larger and larger, and the operation speed is getting faster and faster. Therefore, the requirements on computer technology and network technology are higher and higher, the micro-electronics industry based on high technology is developed rapidly, and the hardware support of large-scale and ultra-large-scale integrated circuits cannot be kept for PIII and PIV processors and broadband large-capacity transmission networks. In addition to the rapid development of the microelectronic industry, the requirements of large-scale and ultra-large-scale integrated circuits on packaging materials are higher and higher, and the filler silicon micropowder is required to be ultrafine and also required to have high purity and low content of radioactive elements. The high-purity superfine silicon powder has high purity (SiO 2 is more than or equal to 99.98 percent), fine particle size (0.5-5 um) of powder, large specific surface area, high dielectric property, high heat resistance, high moisture resistance, high filling amount, low expansion, low stress, low impurity, low friction coefficient and other excellent performances, and becomes an indispensable excellent material in substrates and electronic packaging materials of large-scale and ultra-large-scale integrated circuits.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method of ultrapure silicon for the solar photovoltaic industry, which has the advantage of high purity, solves the defects of the domestic preparation technology of the ultrapure silicon and replaces the problem of dependence on import.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of ultrapure silicon for solar photovoltaic industry comprises the following steps:
s1, selecting materials, namely selecting 10-20 parts of quartz stone ore in a quartz stone pit, and detecting and selecting the quartz stone ore with the silicon dioxide content of more than 90%;
s2, putting the raw materials in the step S1 into a special cleaning container, and continuously overturning, cleaning and drying the raw materials by using a high-pressure water gun;
s3, putting the cleaned raw materials in the step S2 into a crusher to be crushed, and obtaining 10-20 parts of quartz powder materials;
s4, putting the raw materials in the step S3 into a quartz calcining furnace, removing air in the furnace by using nitrogen, and calcining for 3-6 hours at 950-1050 ℃; quickly putting the calcined lump material into a cold water pool with circulating cooling water for water quenching; taking out the water-quenched material, manually selecting to remove impurities, and airing for later use;
s5, putting 10-20 parts of quartz powder in the step S4 into a crucible of a high-frequency induction furnace, adding 5-10 parts of reducing agent, and performing continuous turnover reaction at a high temperature of 800-1000 ℃ to obtain crude silicon;
s6, putting the crude silicon obtained in the step S5 into the reaction kettle again, injecting 5-10 parts of a reactant, fully stirring to enable the crude silicon and the reactant to fully react to generate silicon tetrachloride gas, injecting 5-10 parts of hydrogen into the reaction kettle, heating at the high temperature of 1000-1500 ℃ to enable the hydrogen to fully react to generate pure silicon and hydrogen chloride gas;
and S7, collecting the generated pure silicon by using a special tool, and recycling the generated hydrogen chloride gas.
Preferably, the ore dressing in S1 is manually distinguished, and then the content of the quartz ore is detected through an assay.
Preferably, the tail end of the cleaning device in the S2 is matched with a high-temperature dryer, so that moisture is eliminated, and improvement of pure silicon preparation is facilitated.
Preferably, the reducing agent in S5 is coke, and the carbon monoxide gas is generated by the reduction reaction, and the carbon monoxide collecting device is provided outside the crucible.
Preferably, the reactant in S6 is chlorine.
Preferably, the pressure of the reaction kettle in the S5 is 300-500kPa during operation.
Preferably, the processing sequence in S6 is such that the crude silicon and the reactant are, in order, fully reacted before the hydrogen gas is injected and reacted with the reaction product.
Preferably, the hydrogen chloride in S7 can be reacted to produce a hydrochloric acid solution.
(III) advantageous effects
Compared with the prior art, the invention provides a preparation method of ultrapure silicon for the solar photovoltaic industry, which has the following beneficial effects:
1. according to the preparation method of the ultrapure silicon for the solar photovoltaic industry, the high-pressure water gun is used for washing, overturning and drying to remove impurities, so that the influence of the impurities on the preparation of the ultrapure silicon can be improved.
2. According to the preparation method of the ultra-pure silicon for the solar photovoltaic industry, the high-frequency induction furnace is used as the reaction kettle, so that the reduction efficiency and the reduction speed of the quartz stone powder can be improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The first embodiment is as follows:
a preparation method of ultra-pure silicon for the solar photovoltaic industry comprises the following steps:
s1, selecting materials, namely selecting 10 parts of quartz stone ore in a quartz stone pit, and detecting the quartz stone ore with the silicon dioxide content of more than 90%;
s2, placing the raw materials in the step S1 into a special cleaning container, and continuously overturning, cleaning and drying the raw materials by using a high-pressure water gun;
s3, putting the cleaned raw materials in the S2 into a crusher to be crushed to obtain 10 parts of quartz powder materials;
s4, loading the raw materials in the step S3 into a quartz calcining furnace, removing air in the furnace by using nitrogen, and calcining for 3 hours at 950 ℃; quickly putting the calcined lump material into a cold water pool with circulating cooling water for water quenching; taking out the water-quenched material, manually selecting to remove impurities, and airing for later use;
s5, putting 10 parts of quartz stone powder in the step S4 into a crucible of a high-frequency induction furnace, adding 5 parts of reducing agent, and continuously performing turnover reaction at high temperature of 800 ℃ to obtain crude silicon;
s6, putting the crude silicon obtained in the step S5 into the reaction kettle again, injecting 5 parts of reactant, fully stirring to enable the crude silicon and the reactant to fully react to generate silicon tetrachloride gas, injecting 5 parts of hydrogen into the reaction kettle, heating at a high temperature of 1000 ℃ to enable the crude silicon and the reactant to fully react to generate pure silicon and hydrogen chloride gas;
and S7, collecting the generated pure silicon by using a special tool, and recycling the generated hydrogen chloride gas.
Example two:
a preparation method of ultrapure silicon for solar photovoltaic industry comprises the following steps:
s1, selecting materials, namely selecting 11 parts of quartz stone ore in a quartz stone pit, and detecting the quartz stone ore with the silicon dioxide content of more than 90%;
s2, putting the raw materials in the step S1 into a special cleaning container, and continuously overturning, cleaning and drying the raw materials by using a high-pressure water gun;
s3, putting the cleaned raw materials in the S2 into a crusher to be crushed to obtain 11 parts of quartz powder materials;
s4, loading the raw materials in the S3 into a quartz calcining furnace, removing air in the furnace by using nitrogen, and calcining for 3.5 hours at 975 ℃; quickly putting the calcined lump material into a cold water pool with circulating cooling water for water quenching; taking out the water-quenched material, manually selecting to remove impurities, and airing for later use;
s5, putting 11 parts of quartz stone powder in the step S4 into a crucible of a high-frequency induction furnace, adding 6 parts of reducing agent, and continuously performing turnover reaction at a high temperature of 820 ℃ to obtain crude silicon;
s6, putting the crude silicon obtained in the step S5 into the reaction kettle again, injecting 6 parts of reactant, fully stirring to enable the crude silicon and the reactant to fully react to generate silicon tetrachloride gas, injecting 6 parts of hydrogen into the reaction kettle, heating at a high temperature of 1150 ℃ to enable the crude silicon and the reactant to fully react to generate pure silicon and hydrogen chloride gas;
and S7, collecting the generated pure silicon by using a special tool, and recycling the generated hydrogen chloride gas.
Example three:
a preparation method of ultrapure silicon for solar photovoltaic industry comprises the following steps:
s1, selecting materials, namely selecting 13 parts of quartz ore in a quartz ore pit, and detecting the quartz ore with the silicon dioxide content of more than 90%;
s2, placing the raw materials in the step S1 into a special cleaning container, and continuously overturning, cleaning and drying the raw materials by using a high-pressure water gun;
s3, putting the cleaned raw materials in the step S2 into a crusher to be crushed to obtain 13 parts of quartz powder materials;
s4, loading the raw materials in the S3 into a quartz calcining furnace, removing air in the furnace by using nitrogen, and calcining for 3.8 hours at 980 ℃; then quickly putting the calcined lump material into a cold water pool with circulating cooling water for water quenching; taking out the water-quenched material, manually selecting to remove impurities, and airing for later use;
s5, putting 11 parts of quartz stone powder in the step S4 into a crucible of a high-frequency induction furnace, adding 6.5 parts of reducing agent, and continuously performing turnover reaction at a high temperature of 850 ℃ to obtain crude silicon;
s6, putting the crude silicon obtained in the S5 into the reaction kettle again, injecting 6.5 parts of a reactant, fully stirring to enable the crude silicon and the reactant to fully react to generate silicon tetrachloride gas, injecting 6.5 parts of hydrogen into the reaction kettle, heating at a high temperature of 1175 ℃ to fully react to generate pure silicon and hydrogen chloride gas;
and S7, collecting the generated pure silicon by using a special tool, and recycling the generated hydrogen chloride gas.
Experimental example four:
a preparation method of ultrapure silicon for solar photovoltaic industry comprises the following steps:
s1, selecting materials, namely selecting 14 parts of quartz ores in a quartz pit, and detecting the quartz ores with the silicon dioxide content of more than 90%;
s2, putting the raw materials in the step S1 into a special cleaning container, and continuously overturning, cleaning and drying the raw materials by using a high-pressure water gun;
s3, putting the cleaned raw materials in the step S2 into a crusher to be crushed to obtain 14 parts of quartz powder materials;
s4, the raw materials in the S3 are loaded into a quartz calcining furnace, air in the furnace is removed by nitrogen, and calcining is carried out for 4 hours at 990C; quickly putting the calcined lump material into a cold water pool with circulating cooling water for water quenching; taking out the water-quenched material, manually selecting to remove impurities, and airing for later use;
s5, putting 14 parts of quartz stone powder in the step S4 into a crucible of a high-frequency induction furnace, adding 7 parts of reducing agent, and continuously performing turnover reaction at high temperature of 890 ℃ to obtain crude silicon;
s6, putting the crude silicon obtained in the step S5 into the reaction kettle again, injecting 7 parts of reactant, fully stirring to enable the crude silicon and the reactant to fully react to generate silicon tetrachloride gas, injecting 7 parts of hydrogen into the reaction kettle, heating at a high temperature of 1200 ℃ to enable the crude silicon and the reactant to fully react to generate pure silicon and hydrogen chloride gas;
and S7, collecting the generated pure silicon by using a special tool, and recycling the generated hydrogen chloride gas.
Experimental example five:
a preparation method of ultrapure silicon for solar photovoltaic industry comprises the following steps:
s1, selecting materials, namely selecting 15 parts of quartz stone ore in a quartz stone pit, and detecting the quartz stone ore with the silicon dioxide content of more than 90%;
s2, putting the raw materials in the step S1 into a special cleaning container, and continuously overturning, cleaning and drying the raw materials by using a high-pressure water gun;
s3, putting the cleaned raw materials in the S2 into a crusher to be crushed to obtain 15 parts of quartz powder materials;
s4, loading the raw materials in the S3 into a quartz calcining furnace, removing air in the furnace by using nitrogen, and calcining for 4.5 hours at 1000 ℃; quickly putting the calcined lump material into a cold water pool with circulating cooling water for water quenching; taking out the water-quenched material, manually selecting to remove impurities, and airing for later use;
s5, putting 15 parts of quartz stone powder in the step S4 into a crucible of a high-frequency induction furnace, adding 8 parts of reducing agent, and continuously performing turnover reaction at a high temperature of 920 ℃ to obtain crude silicon;
s6, putting the crude silicon obtained in the step S5 into the reaction kettle again, injecting 8 parts of reactant, fully stirring to enable the crude silicon and the reactant to fully react to generate silicon tetrachloride gas, injecting 8 parts of hydrogen into the reaction kettle, heating at 1250 ℃ to enable the crude silicon and the reactant to fully react to generate pure silicon and hydrogen chloride gas;
and S7, collecting the generated pure silicon by using a special tool, and recycling the generated hydrogen chloride gas.
Experimental example six:
a preparation method of ultra-pure silicon for the solar photovoltaic industry comprises the following steps:
s1, selecting materials, namely selecting 16 parts of quartz ores in a quartz pit, and detecting the quartz ores with the silicon dioxide content of more than 90%;
s2, putting the raw materials in the step S1 into a special cleaning container, and continuously overturning, cleaning and drying the raw materials by using a high-pressure water gun;
s3, putting the cleaned raw materials in the step S2 into a crusher to be crushed to obtain 16 parts of quartz powder materials;
s4, loading the raw materials in the S3 into a quartz calcining furnace, removing air in the furnace by using nitrogen, and calcining for 5 hours at 1020 ℃; quickly putting the calcined lump material into a cold water pool with circulating cooling water for water quenching; taking out the water-quenched material, manually selecting to remove impurities, and airing for later use;
s5, placing 16 parts of quartz stone powder in the step S4 into a crucible of a high-frequency induction furnace, adding 8.5 parts of reducing agent, and continuously performing turnover reaction at high temperature of 950 ℃ to obtain crude silicon;
s6, putting the crude silicon obtained in the S5 into the reaction kettle again, injecting 8.5 parts of a reactant, fully stirring to enable the crude silicon and the reactant to fully react to generate silicon tetrachloride gas, injecting 8.5 parts of hydrogen into the reaction kettle, heating at a high temperature of 1300 ℃ to enable the reaction kettle to fully react to generate pure silicon and hydrogen chloride gas;
and S7, collecting the generated pure silicon by using a special tool, and recycling the generated hydrogen chloride gas.
Seventh Experimental example:
a preparation method of ultra-pure silicon for the solar photovoltaic industry comprises the following steps:
s1, selecting materials, namely selecting 18 parts of quartz ore in a quartz ore pit, and detecting the quartz ore with the silicon dioxide content of more than 90%;
s2, putting the raw materials in the step S1 into a special cleaning container, and continuously overturning, cleaning and drying the raw materials by using a high-pressure water gun;
s3, putting the cleaned raw materials in the S2 into a crusher to be crushed to obtain 18 parts of quartz powder materials;
s4, the raw materials in the S3 are loaded into a quartz calcining furnace, air in the furnace is removed by nitrogen, and calcining is carried out for 5.5 hours at 1040C; quickly putting the calcined lump material into a cold water pool with circulating cooling water for water quenching; taking out the water-quenched material, manually selecting to remove impurities, and airing for later use;
s5, putting 18 parts of quartz stone powder in the step S4 into a crucible of a high-frequency induction furnace, adding 9 parts of reducing agent, and continuously performing turnover reaction at a high temperature of 980 ℃ to obtain crude silicon;
s6, putting the crude silicon obtained in the step S5 into the reaction kettle again, injecting 9 parts of reactant, fully stirring to enable the crude silicon and the reactant to fully react to generate silicon tetrachloride gas, injecting 9 parts of hydrogen into the reaction kettle, heating at a high temperature of 1400 ℃ to enable the crude silicon and the reactant to fully react to generate pure silicon and hydrogen chloride gas;
and S7, collecting the generated pure silicon by using a special tool, and recycling the generated hydrogen chloride gas.
Seventh Experimental example:
a preparation method of ultrapure silicon for solar photovoltaic industry comprises the following steps:
s1, selecting materials, namely selecting 20 parts of quartz ore in a quartz ore pit, and detecting the quartz ore with the silicon dioxide content of more than 90%;
s2, placing the raw materials in the step S1 into a special cleaning container, and continuously overturning, cleaning and drying the raw materials by using a high-pressure water gun;
s3, putting the cleaned raw materials in the step S2 into a crusher to be crushed, and obtaining 20 parts of quartz powder materials;
s4, loading the raw materials in the step S3 into a quartz calcining furnace, removing air in the furnace by using nitrogen, and calcining for 6 hours at 1050 ℃; then quickly putting the calcined lump material into a cold water pool with circulating cooling water for water quenching; taking out the water-quenched material, manually selecting to remove impurities, and airing for later use;
s5, putting 20 parts of quartz powder in the step S4 into a crucible of a high-frequency induction furnace, adding 10 parts of reducing agent, and continuously performing turnover reaction at high temperature of 1000 ℃ to obtain crude silicon;
s6, putting the crude silicon obtained in the S5 into the reaction kettle again, injecting 10 parts of a reactant, fully stirring to enable the crude silicon and the reactant to fully react to generate silicon tetrachloride gas, injecting 10 parts of hydrogen into the reaction kettle, heating at a high temperature of 1500 ℃ to fully react to generate pure silicon and hydrogen chloride gas;
and S7, collecting the generated pure silicon by using a special tool, and recycling the generated hydrogen chloride gas.
The beneficial effects of the invention are: wash through the high-pressure squirt, the upset is dried, gets rid of impurity, can improve the influence of impurity to the ultrapure silicon of preparation, is reation kettle through the high-frequency induction furnace, can improve the speed to the reduction efficiency and the reduction of quartz powder, and the silicon purity that makes the preparation through the reaction is higher.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A preparation method of ultrapure silicon for solar photovoltaic industry is characterized by comprising the following steps:
s1, selecting materials, namely selecting 10-20 parts of quartz stone ore in a quartz stone pit, and detecting and selecting the quartz stone ore with the silicon dioxide content of more than 90%;
s2, putting the raw materials in the step S1 into a special cleaning container, and continuously overturning, cleaning and drying the raw materials by using a high-pressure water gun;
s3, putting the cleaned raw materials in the step S2 into a crusher to be crushed, and obtaining 10-20 parts of quartz powder materials;
s4, putting the raw materials in the step S3 into a quartz calcining furnace, removing air in the furnace by using nitrogen, and calcining for 3-6 hours at 950-1050 ℃; quickly putting the calcined lump material into a cold water pool with circulating cooling water for water quenching; taking out the water-quenched material, manually selecting to remove impurities, and airing for later use;
s5, putting 10-20 parts of quartz powder in the step S4 into a crucible of a high-frequency induction furnace, adding 5-10 parts of reducing agent, and performing continuous turnover reaction at a high temperature of 800-1000 ℃ to obtain crude silicon;
s6, putting the crude silicon obtained in the step S5 into the reaction kettle again, injecting 5-10 parts of a reactant, fully stirring to enable the crude silicon and the reactant to fully react to generate silicon tetrachloride gas, injecting 5-10 parts of hydrogen into the reaction kettle, heating at the high temperature of 1000-1500 ℃ to enable the hydrogen to fully react to generate pure silicon and hydrogen chloride gas;
and S7, collecting the generated pure silicon by using a special tool, and recycling the generated hydrogen chloride gas.
2. The method according to claim 1, wherein the beneficiation in S1 is performed by manual discrimination and then the content of the quartz ore is detected by assay.
3. The method according to claim 1, wherein a high temperature dryer is provided at the end of the cleaning device in step S2 to remove moisture, which is helpful for improving purity of silicon.
4. The method of claim 1, wherein the reducing agent in S5 is coke, and the reduction reaction produces carbon monoxide gas, and the carbon monoxide collection device is disposed outside the crucible.
5. The method of claim 1, wherein the reactant in S6 is chlorine.
6. The method of claim 1, wherein the pressure in the reactor of S5 is 300-500kPa.
7. The method of claim 1, wherein the step of S6 comprises reacting the crude silicon with the reactant to react with the reactant, and injecting hydrogen gas to react with the reactant.
8. The method of claim 1, wherein the hydrogen chloride in S7 is reacted to produce hydrochloric acid solution.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH365709A (en) * | 1956-12-22 | 1962-11-30 | Texas Instruments Inc | Process for the production of high purity silicon from silicon tetrachloride |
| US20100233063A1 (en) * | 2009-03-13 | 2010-09-16 | Radiant Technology Co. | Method for manufacturing high-purity silicon material |
| CN102225766A (en) * | 2011-03-29 | 2011-10-26 | 东海县圣达石英制品有限公司 | Preparation method for ultra pure silicon material used in solar energy photovoltaic industry |
-
2021
- 2021-10-08 CN CN202111169413.9A patent/CN115385339A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH365709A (en) * | 1956-12-22 | 1962-11-30 | Texas Instruments Inc | Process for the production of high purity silicon from silicon tetrachloride |
| US20100233063A1 (en) * | 2009-03-13 | 2010-09-16 | Radiant Technology Co. | Method for manufacturing high-purity silicon material |
| CN102225766A (en) * | 2011-03-29 | 2011-10-26 | 东海县圣达石英制品有限公司 | Preparation method for ultra pure silicon material used in solar energy photovoltaic industry |
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