CN110605176A - Method for breaking polycrystalline silicon material through water explosion - Google Patents

Method for breaking polycrystalline silicon material through water explosion Download PDF

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Publication number
CN110605176A
CN110605176A CN201911012499.7A CN201911012499A CN110605176A CN 110605176 A CN110605176 A CN 110605176A CN 201911012499 A CN201911012499 A CN 201911012499A CN 110605176 A CN110605176 A CN 110605176A
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silicon
silicon material
polycrystalline silicon
water
size
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CN201911012499.7A
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Chinese (zh)
Inventor
李建军
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XI'AN HUAJING ELECTRONIC TECHNOLOGY Co Ltd
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XI'AN HUAJING ELECTRONIC TECHNOLOGY Co Ltd
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Priority to CN201911012499.7A priority Critical patent/CN110605176A/en
Publication of CN110605176A publication Critical patent/CN110605176A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00Other disintegrating devices or methods
    • B02C19/18Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
    • B02C19/186Use of cold or heat for disintegrating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C21/00Disintegrating plant with or without drying of the material

Abstract

The invention discloses a method for breaking a polycrystalline silicon material by water explosion, which comprises the following specific processes: placing the raw silicon polycrystalline silicon bar in a high vacuum melting furnace, vacuumizing, introducing argon, heating, keeping the temperature, cooling along with the furnace, cooling the cooled charging frame loaded with the raw silicon polycrystalline silicon bar by flowing water to obtain the raw silicon polycrystalline silicon bar with cracks on the surface, crushing the raw silicon polycrystalline silicon bar by collision, sorting to obtain a silicon material crude product with the size of 10-100 mm, and cleaning and drying to obtain the silicon material. According to the invention, the charging basket is used for loading the raw silicon polycrystalline silicon bar for heating and heat preservation, then water explosion is carried out in the water tank, and then the silicon material is prepared by crushing and colliding.

Description

Method for breaking polycrystalline silicon material through water explosion
Technical Field
The invention belongs to the technical field of polycrystalline silicon ingot preparation, and particularly relates to a method for crushing a polycrystalline silicon material through water explosion.
Background
With the increasing productivity in the field of solar power generation, the cost of the single crystal technology is gradually reduced, and particularly continuous crystal pulling of secondary added materials becomes the basic requirement of the photovoltaic industry. Therefore, the demand of small blocks in the whole industry is extremely large, and in addition, the product produced by the improved Siemens method which is a production process of the small blocks is a bar or a large block, the small crushed aggregates produced in the whole primary polycrystalline silicon production process are extremely few, and the market demand can not be met.
The method can crush the silicon material to the size required by the market, but has the disadvantages of low yield, low efficiency, large dust in the production process, high pollution, high silicon material loss, high production cost, high manual input cost, more edges and corners generated on the surface of crushed materials, insufficient roundness and more surface powder influencing the crystallinity of single crystals.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for breaking a polycrystalline silicon material by water explosion aiming at the defects of the prior art. According to the method, a charging basket is used for loading the raw silicon polycrystalline silicon bar for heating and heat preservation, then water explosion is carried out in a water tank, and then the silicon material is prepared through collision and crushing.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for breaking polycrystalline silicon material by water explosion is characterized by comprising the following steps:
step one, placing a primary silicon polycrystalline silicon bar vertically upwards in a material loading frame, then placing the bar in a high-vacuum smelting furnace, starting a mechanical pump and a plug board valve, and vacuumizing the high-vacuum smelting furnace within 25-30 min until the vacuum degree is not more than 0.2 mbar; the air leakage rate of the high vacuum smelting furnace after vacuum pumping is lower than 0.015 mbar;
step two, introducing argon into the high vacuum melting furnace vacuumized in the step one, heating the raw silicon polycrystalline silicon bar, enabling the heating power to reach 70% -75% within 20 min-30 min, when the heating temperature is raised to 700 ℃, switching the high vacuum melting furnace from a power mode to a temperature control mode for 1.5h, continuously preserving the heat for 2.5 h-3.5 h, and then cooling the high vacuum melting furnace to 500 ℃ -550 ℃ along with the furnace within 1.5 h-2 h under the condition of continuously introducing argon;
taking out the charging frame which is cooled to 500-550 ℃ in the step two and is loaded with the primary silicon polycrystalline silicon bar, putting the charging frame into a water tank within 30s for flowing water cooling for 2.5min, taking out the charging frame, spraying water to remove surface powder, and draining to obtain the primary silicon polycrystalline silicon bar with cracks on the surface;
step four, the primary silicon polycrystalline silicon bars with cracks on the surfaces, which are obtained in the step three, are crushed in a colliding mode, then the primary silicon polycrystalline silicon bars are sorted to obtain silicon material crude products with the size of 10 mm-100 mm, the sorted silicon material crude products with the size larger than the size are sequentially placed in a high-vacuum smelting furnace and a vacuumizing process in the step one, a heating, heat preservation and cooling process in the step two, a cooling and spraying draining process in the step three and a colliding, crushing and sorting process in the step four until the silicon material crude products with the size of 10 mm-100 mm are obtained;
and step five, carrying out ultrasonic cleaning on the silicon material crude product with the size of 10-100 mm obtained in the step four, then placing the silicon material crude product on a tetrafluoro material plate, and sending the silicon material crude product into a drying oven for drying to obtain the silicon material with the size of 10-100 mm.
The method comprises the steps of heating and insulating a primary silicon polycrystalline silicon bar, cooling to 500-550 ℃, performing water explosion treatment, performing collision crushing treatment, and sequentially performing sorting, cleaning and drying to obtain a silicon material with the size of 10-100 mm. The invention loads the raw silicon polycrystalline silicon bar by the charging basket for heating and heat preservation, improves the raw material processing amount and the yield of the silicon material, avoids the surface oxidation problem of the raw silicon polycrystalline silicon bar in the conventional high-temperature heating process by introducing argon for protection and controlling the temperature parameter of the heating and heat preservation in the heating and heat preservation process, is favorable for improving the purity of the silicon material, then puts the heated raw silicon polycrystalline silicon bar into the water tank for flowing water cooling, avoids the heated raw silicon polycrystalline silicon bar from being exposed in the air for a long time by controlling the process parameter of the process, avoids the introduction of oxygen atoms to harm the quality of the silicon material, simultaneously avoids the air from taking away partial heat to influence the subsequent water explosion effect, shortens the cooling time, improves the water explosion efficiency, and avoids the bar surface from being exposed in the air for a long time to be oxidized by utilizing the wettability of the water, the method has the advantages of reducing pollution, improving the quality of the silicon material, reducing dust pollution, improving the conversion rate of the silicon material, reducing material loss, along with high yield and high efficiency, and removing a surface loose layer and residual amorphous silicon by adopting collision crushing and subsequent ultrasonic cleaning treatment to obtain the silicon material with less dust, round surface and uniform size, greatly improving the purity of the silicon material and promoting the crystallization property of the silicon material for pulling single crystals.
The method for crushing the polycrystalline silicon material by water explosion is characterized in that the material of the material loading frame in the step one is 304 heat-resistant stainless steel. The heat-resistant temperature of the 304 heat-resistant stainless steel is 1300 ℃, which is far higher than the temperature of the primary silicon polycrystalline silicon bar fed into the high-vacuum melting furnace for heating and heat preservation, so that the requirement of large loading is met, the primary silicon polycrystalline silicon bar is prevented from being polluted by introducing high-temperature impurities, and the charging amount is large and the yield is high.
The method for crushing the polycrystalline silicon material by water explosion is characterized in that in the step one, the conductivity type of the primary silicon polycrystalline silicon rod is N type, the resistivity of the base phosphorus is more than 400 omega-cm, the service life of a minority carrier is more than 500 mu s, and the content of carbon atoms is not more than 2.0 multiplied by 1016atoms/cm3Oxygen atom content of not more than 0.2X 1017atoms/cm3The base metal impurity was 50 ppbw. The performance parameters of the raw silicon polycrystalline silicon rod material reach the standard, the impurity content is low, the silicon material obtained from the raw material is used for preparing the single crystal silicon rod, the impurity content is low, and the service life is long.
The method for crushing the polycrystalline silicon material by water explosion is characterized in that the flowing water is cooled by circulating flowing industrial pure water in the third step. In the water explosion process, water in the water tank is heated from top to bottom, industrial pure water which flows circularly is adopted for cooling, cold water is fed from the lower part of the water tank, cooled hot water is rapidly discharged from the upper part of the water tank, heat is rapidly taken away, the difference between the internal temperature and the external temperature of the primary silicon polycrystalline silicon bar in the material loading frame is further increased, more cracks are generated, and the subsequent collision and crushing are facilitated to generate silicon materials with smooth and uniform surfaces; in addition, continuous water explosion production is realized by adopting the circularly flowing industrial pure water, the water explosion efficiency is improved, the silicon material yield is improved, and the water temperature of the circularly flowing industrial pure water is preferably below 30 ℃.
The method for crushing the polycrystalline silicon material by water explosion is characterized in that the grade of the silicon material crude product with the size of 10 mm-100 mm in the fourth step is as follows: the size of the first-stage silicon material crude product is more than or equal to 10mm and less than 20mm, the size of the second-stage silicon material crude product is more than or equal to 20mm and less than 40mm, the size of the third-stage silicon material crude product is more than or equal to 40mm and less than 70mm, and the size of the fourth-stage silicon material crude product is more than or equal to 70mm and less than or equal to 100 mm. Silicon materials with different size grades are obtained through the silicon material crude products with the divided sizes, so that the requirements for preparing different single crystal silicon rods are met, and the applicability of the method is expanded.
The method for crushing the polycrystalline silicon material by water explosion is characterized in that in the fifth step, the ultrasonic cleaning power is 6kW, the frequency is 50Hz, and the time is 2 min. The ultrasonic cleaning process adopting the parameters is beneficial to further removing the loose layer on the surface of the crude silicon material and the residual amorphous silicon, greatly improves the purity of the silicon material and promotes the single crystal crystallization of the silicon material.
The method for crushing the polycrystalline silicon material by water explosion is characterized in that the drying temperature in the fifth step is 145 ℃, and the time is 0.5 h. The drying temperature ensures that the surface of the dried silicon material has no water stain, and simultaneously avoids the silicon material from being heated to excessively soften the PTFE material plate.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the charging basket is used for loading the raw silicon polycrystalline silicon bar for heating and heat preservation, then water explosion is carried out in the water tank, and then the silicon material is prepared by crushing and colliding.
2. The invention carries out low-temperature heating and heat preservation by introducing nitrogen protection, thereby avoiding the pollution of impurities such as oxygen, carbon and the like, ensuring the purity of the silicon material, simultaneously reducing the process difficulty and further realizing the large-scale production of the silicon material.
3. The charging frame adopted by the invention has simple structure, is economic, has low cost and is suitable for large-scale production.
4. The invention adopts the flowing recyclable industrial-grade pure water as the water special for the water explosion material, thereby not only effectively controlling the production cost, but also ensuring the purity of the silicon material.
5. The silicon material prepared by the method has uniform size and round and smooth surface, and can be used for producing silicon materials with different size grades according to use requirements, so that the application range of the silicon material is expanded.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
Fig. 1 is a schematic structural diagram of a charging frame adopted by the invention.
Fig. 2 is a schematic structural view of a sink employed in the present invention.
Description of the reference numerals
1-hanging ring; 2, lining; 3-a frame;
4-inner groove; 5, a shell; 6, a water inlet pipeline;
7-a drainage pipeline.
Detailed Description
As shown in figure 1, the charging frame adopted by the invention consists of a frame 3 and a lining 2 arranged in the frame 3, wherein a hanging ring 1 is arranged on the outer wall of the frame 3; the hanging ring 1, the lining 2 and the frame 3 are all made of 304 heat-resistant stainless steel preferably.
As shown in figure 2, the water tank of the invention comprises a shell 5 and an inner tank 4 arranged in the shell 5, wherein a water inlet pipeline 6 is arranged at the bottom of the inner tank 4, a water drainage pipeline 7 is arranged at the upper part of the inner tank 4 and at the same side of the water inlet pipeline 6, the arrangement directions of the water inlet pipeline 6 and the water drainage pipeline 7 are vertical, and the preferable material of the inner tank 4 is a tetrafluoro plate.
Example 1
The embodiment comprises the following steps:
step one, in a dust-free workshop, a loader wears dust-free clothes,wearing a mask and cleaning gloves, vertically and upwards placing 700kg of raw silicon polycrystalline silicon bars in a 304 heat-resistant stainless steel charging frame along the axial direction, keeping the whole process lightly taking and placing the bars in a high-vacuum smelting furnace, starting a mechanical pump and a plug board valve, and vacuumizing the high-vacuum smelting furnace within 25min until the vacuum degree is 0.2 mbar; the air leakage rate of the high-vacuum smelting furnace after vacuum pumping is lower than 0.015mbar, namely the vacuum degree difference value of the high-vacuum smelting furnace in the leakage detection time of 5min is lower than 0.015 mbar; the conductivity type of the primary silicon polycrystalline silicon bar is N type, the resistivity of the base phosphorus is larger than 400 omega cm, the service life of a minority carrier is larger than 500 mu s, and the content of carbon atoms is not more than 2.0 multiplied by 1016atoms/cm3Oxygen atom content of not more than 0.2X 1017atoms/cm3The matrix metal impurity was 50 ppbw;
step two, introducing argon into the high vacuum smelting furnace vacuumized in the step one, heating the raw silicon polycrystalline silicon bar, enabling the heating power to reach 70% within 20min, switching the high vacuum smelting furnace from a power mode to a temperature control mode for 1.5h when the heating temperature rises to 700 ℃, continuously preserving heat for 2.5h, and then cooling to 500 ℃ along with the furnace within 1.5h under the condition of continuously introducing argon;
taking out the loading frame loaded with the raw silicon polycrystalline silicon bars cooled to 500 ℃ in the step two by using an electric forklift, hoisting the loading frame into the water tank by using a crane within 30s, starting a circulating water pump of the water tank to perform water circulation, simultaneously placing the loading frame loaded with the raw silicon polycrystalline silicon bars into the water tank, cooling the loading frame by using circulating flowing water for 2.5min, taking out the loading frame into the water tank for 30s, taking out the loading frame, performing water spraying on the loading frame from top to bottom and from inside to outside to remove surface powder generated by water explosion treatment, hoisting the loading frame out of the water tank, and draining to obtain the raw silicon polycrystalline silicon bars with cracks on the surface;
step four, the primary silicon polycrystalline silicon bars with cracks on the surfaces, which are obtained in the step three, are crushed in a colliding mode, then the primary silicon polycrystalline silicon bars are sorted to obtain silicon material crude products with the size of 10 mm-100 mm, the sorted silicon material crude products with the size larger than the size are sequentially placed in a high-vacuum smelting furnace and a vacuumizing process in the step one, a heating, heat preservation and cooling process in the step two, a cooling and spraying draining process in the step three and a colliding, crushing and sorting process in the step four until the silicon material crude products with the size of 10 mm-100 mm are obtained; in the crude silicon material obtained by crushing the primary silicon polycrystalline silicon bar, the mass percentage of the crude silicon material with the size of less than 10mm is 3%, the mass percentage of the crude silicon material with the size of 10 mm-100 mm is 97%, and the mass percentage of the crude silicon material with the size of more than 100mm is 2%; the grade of the crude silicon material with the size of 10 mm-100 mm is as follows: the size of the first-stage silicon material crude product is more than or equal to 10mm and less than 20mm, the size of the second-stage silicon material crude product is more than or equal to 20mm and less than 40mm, the size of the third-stage silicon material crude product is more than or equal to 40mm and less than 70mm, and the size of the fourth-stage silicon material crude product is more than or equal to 70mm and not more than 100mm
And step five, ultrasonically cleaning the silicon material crude product with the size of 10 mm-100 mm obtained in the step four for 2min under the conditions that the power is 6kW and the frequency is 50Hz, removing surface fine powder generated by crushing and sorting, then placing the silicon material crude product on a PTFE material plate, and sending the silicon material crude product into a drying oven to dry for 0.5h under the temperature of 145 ℃ to obtain the silicon material with the size of 10 mm-100 mm.
Placing the silicon material obtained in the embodiment in a dust-free chamber, standing until the room temperature of the dust-free chamber is the same, then packaging by using a clean plastic bag, wherein the packaging specification is 10 kg/bag, and packaging by using an inner layer seal and an outer layer seal, wherein each bag is prevented from being provided with a material information card, and information such as the type, name, particle size and weight of the silicon material is recorded; and (4) independently recovering the silicon material falling on the bottom surface in the packaging process and repeating the ultrasonic cleaning and drying process in the fifth step.
The differences between the embodiments 2 to 13 of the present invention and the embodiment 1 include: the vacuum pumping time and the vacuum degree in the first step, the heating time and the heating power in the second step, the temperature after heating, the heat preservation time, the cooling time in the third step, the tapping temperature, the silicon material water feeding time, the heating power and the mass percentage of the crude silicon material products with different size ranges obtained after the primary silicon polycrystalline silicon rod material is crushed, and different process parameters of the embodiments 2 to 13 are shown in the following table 1.
TABLE 1
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.

Claims (7)

1. A method for breaking polycrystalline silicon material by water explosion is characterized by comprising the following steps:
step one, placing a primary silicon polycrystalline silicon bar vertically upwards in a material loading frame, then placing the bar in a high-vacuum smelting furnace, starting a mechanical pump and a plug board valve, and vacuumizing the high-vacuum smelting furnace within 25-30 min until the vacuum degree is not more than 0.2 mbar; the air leakage rate of the high vacuum smelting furnace after vacuum pumping is lower than 0.015 mbar;
step two, introducing argon into the high vacuum melting furnace vacuumized in the step one, heating the raw silicon polycrystalline silicon bar, enabling the heating power to reach 70% -75% within 20 min-30 min, when the heating temperature is raised to 700 ℃, switching the high vacuum melting furnace from a power mode to a temperature control mode for 1.5h, continuously preserving the heat for 2.5 h-3.5 h, and then cooling the high vacuum melting furnace to 500 ℃ -550 ℃ along with the furnace within 1.5 h-2 h under the condition of continuously introducing argon;
taking out the charging frame which is cooled to 500-550 ℃ in the step two and is loaded with the primary silicon polycrystalline silicon bar, putting the charging frame into a water tank within 30s for flowing water cooling for 2.5min, taking out the charging frame, spraying water to remove surface powder, and draining to obtain the primary silicon polycrystalline silicon bar with cracks on the surface;
step four, the primary silicon polycrystalline silicon bars with cracks on the surfaces, which are obtained in the step three, are crushed in a colliding mode, then the primary silicon polycrystalline silicon bars are sorted to obtain silicon material crude products with the size of 10 mm-100 mm, the sorted silicon material crude products with the size larger than the size are sequentially placed in a high-vacuum smelting furnace and a vacuumizing process in the step one, a heating, heat preservation and cooling process in the step two, a cooling and spraying draining process in the step three and a colliding, crushing and sorting process in the step four until the silicon material crude products with the size of 10 mm-100 mm are obtained;
and step five, carrying out ultrasonic cleaning on the silicon material crude product with the size of 10-100 mm obtained in the step four, then placing the silicon material crude product on a tetrafluoro material plate, and sending the silicon material crude product into a drying oven for drying to obtain the silicon material with the size of 10-100 mm.
2. The method for water blasting breaking of polysilicon according to claim 1, wherein the material of the charging frame in the first step is 304 heat-resistant stainless steel.
3. The method of claim 1, wherein in step one, the raw polysilicon rod has an N-type conductivity, a resistivity of greater than 400 Ω -cm, a minority carrier lifetime of greater than 500 μ s, and a carbon atom content of no more than 2.0 x 1016atoms/cm3Oxygen atom content of not more than 0.2X 1017atoms/cm3The base metal impurity was 50 ppbw.
4. The method for water blasting breaking of polysilicon according to claim 1, wherein the flowing water is cooled by circulating industrial grade pure water in step three.
5. The method for crushing the polycrystalline silicon material through water explosion according to claim 1, wherein the grade of the crude silicon material with the size of 10 mm-100 mm in the fourth step is as follows: the size of the first-stage silicon material crude product is more than or equal to 10mm and less than 20mm, the size of the second-stage silicon material crude product is more than or equal to 20mm and less than 40mm, the size of the third-stage silicon material crude product is more than or equal to 40mm and less than 70mm, and the size of the fourth-stage silicon material crude product is more than or equal to 70mm and less than or equal to 100 mm.
6. The method for water blasting breaking of polycrystalline silicon material according to claim 1, wherein the ultrasonic cleaning in the fifth step is performed at 6kW, 50Hz and 2 min.
7. The method for water blasting breaking of polysilicon according to claim 1, wherein the drying temperature in step five is 145 ℃ and the drying time is 0.5 h.
CN201911012499.7A 2019-10-23 2019-10-23 Method for breaking polycrystalline silicon material through water explosion Pending CN110605176A (en)

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CN114534886A (en) * 2022-02-14 2022-05-27 江苏鑫华半导体科技股份有限公司 Electronic grade polycrystalline silicon thermal crushing heating device, heating method and crushing device

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CN114534886A (en) * 2022-02-14 2022-05-27 江苏鑫华半导体科技股份有限公司 Electronic grade polycrystalline silicon thermal crushing heating device, heating method and crushing device

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Application publication date: 20191224