CN115354387A - Method for improving crystallization rate in ingot purification of monocrystalline crucible bottom waste - Google Patents
Method for improving crystallization rate in ingot purification of monocrystalline crucible bottom waste Download PDFInfo
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- CN115354387A CN115354387A CN202210955098.0A CN202210955098A CN115354387A CN 115354387 A CN115354387 A CN 115354387A CN 202210955098 A CN202210955098 A CN 202210955098A CN 115354387 A CN115354387 A CN 115354387A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for improving the crystallization rate in the ingot casting purification of single crystal crucible bottom waste, which comprises the following steps of setting the flow of argon gas at 200 to 220slpm and blowing for 3 to 5min after charging is finished; secondly, extracting slag in each section, controlling the temperature of the extracted slag, closing the bottom heating power before adding the last cylinder material, and setting the main heating power at 65-75kw; in addition, if impurities appear in the temperature adjusting process, the shouldering process or the equal-diameter process, the impurities are respectively treated in different modes; and finally, independently adjusting the process in the broken line interval, if the broken line interval is less than or equal to 400mm, and the drawing is less than or equal to 2 times, rotating the temperature-adjusting crucible for 8 turns, setting the furnace pressure to be 15torr, setting the argon flow to be l00slpm, and if the drawing is more than 2 times, and no effective output exists, hanging the polycrystal for 300mm, and drawing again. The method has the advantages of effectively recycling the single crystal waste, improving the crystallization rate of the waste, improving the utilization rate of raw materials, saving cost and improving economic benefit.
Description
Technical Field
The invention relates to the technical field of photovoltaic manufacturing, in particular to a method for improving the crystallization rate in ingot purification of single crystal crucible bottom waste.
Background
In the process of single crystal growth, except for available single crystals, other low-quality waste materials such as crucible materials or crucible bed charge materials and the like can be produced, the part of the raw materials is limited by self impurity deposition and cannot be normally recycled to a single crystal process, the raw materials are generally used for low-price external marketing or scrapping treatment, and the raw materials after ingot casting purification have the abnormalities such as difficult crystallization, low yield and the like.
In addition, along with the continuous upgrading and expansion of the thermal field, the output proportion of waste materials is increased, the crucible bed charge produced by purifying raw materials is accumulated continuously, and the consumption cost is increased.
Disclosure of Invention
The invention aims to solve the problems of high yield, difficult crystallization after purification and serious waste of the existing crucible bottom waste, and provides a method for improving the crystallization rate in ingot purification of single crystal crucible bottom waste, which effectively recycles the single crystal waste, improves the crystallization rate of the waste, improves the utilization rate of raw materials, saves cost and improves economic benefit.
In order to achieve the purpose, the invention adopts the following technical scheme:
the utility model provides a method for improving the crystallization rate in purification of single crystal crucible end waste material ingot casting, includes that single crystal waste material collects the back, through polycrystal ingot casting procedure, heating, melting, growing brilliant, produce available polycrystal after annealing and the cooling, get rid of top skin and flaw-piece again, the production is carried out to the single crystal process to surplus raw materials retrieval and utilization, and the polycrystal that the single crystal waste ingot casting produced is after dropping into the single crystal furnace, through the melt, draw the brilliant, put the shoulder, change the shoulder, the isometric and effective single crystal of process output of ending, wherein:
(1) After feeding is finished, namely after the polycrystal generated by the single crystal waste ingot casting is put into a single crystal furnace, setting the flow rate of argon gas to be 200-220slpm, and blowing for 3-5min;
(2) Extracting slag at each stage, and extracting slag and controlling temperature: closing the bottom adding power before adding the last cylinder material, and setting the main adding power to be 65-75kw;
(3) Impurities are treated in different cases: if impurities appear in the temperature adjusting process, the shouldering process or the equal-diameter process, the impurities are respectively treated in different modes;
(4) And (3) independent process adjustment of the breaking line region: if the broken line interval is less than or equal to 400mm and the drawing is less than or equal to 2 times, the temperature-adjusting crucible rotates for 8 turns, the furnace pressure is set to be 15torr, the argon flow is given to l00slpm, if the drawing is more than 2 times, no effective output exists, the polycrystal is lifted by 300mm, and the polycrystal is drawn again.
Further, in the step (3), if impurities appear in the temperature adjusting process, once crystallization is performed to extract slag, namely, the power is reduced, so that the liquid level of the molten silicon in the crucible is affected by the temperature to form a layer of crystalline surface, and the layer of crystalline surface can adhere to infusible impurities on the surface of the molten silicon, so that slag-eating broken lines of crystals in the process of constant diameter are prevented from being caused by the impurities.
Further, in the step (3), if impurities appear in the shouldering process, the shouldering is soaked and adhered, namely, during the growth of the single crystal, remelting is needed due to wire breakage, when the single crystal is remelted to the shoulder part, the power is reduced, the shape of the shoulder part is kept, the infusible impurities floating on the surface of the molten silicon are adhered, and then the shoulder part and the impurities are extracted together.
Furthermore, in the step (3), if impurities appear in the equal-diameter process, the equal-diameter wire is broken, secondary crystallization slag extraction is performed, namely, in the normal drawing process of the monocrystalline silicon, four ridges at the surface end of the crystal are broken due to external interference factors, a dislocation polycrystalline part is formed, the part cannot be used as a monocrystalline product, and the step of crystallizing slag extraction is repeated after the equal-diameter wire is broken.
Further, in the step (3), the power in the crystallization extraction slag is reduced to 8-10kw.
According to the technical scheme, on the basis of the existing polycrystalline ingot casting, the single crystal crystallization process is improved, the crystallization rate is improved, the utilization rate of raw materials is improved, single crystal waste is effectively recycled, the environment is protected, the cost is saved, and the economic benefit is improved.
Detailed Description
Example 1
In order to make the present invention more clearly understood, the method for improving the crystallization rate in the purification of the single crystal crucible bottom waste ingot according to the present invention will be further described, and the specific examples described herein are only for illustrating the present invention and are not intended to limit the present invention.
After the single crystal waste is collected, usable polycrystal is produced through a polycrystal ingot casting process, heating, melting, crystal growing, annealing and cooling, then top skin and side skin are removed, the rest raw materials are recycled to a single crystal process for production, the polycrystal produced by the single crystal waste ingot casting is put into a single crystal furnace, and effective single crystal is produced through the processes of melting, seeding, shouldering, shoulder rotating, diameter equalizing and ending, in the process, the invention provides a method for improving the crystal yield in the purification of the single crystal crucible bottom waste ingot casting, which is characterized by comprising the following steps:
(1) After feeding is finished, namely after the polycrystal generated by the single crystal waste ingot casting is put into a single crystal furnace, setting the flow rate of argon gas to be 200-220slpm, and blowing for 3-5min;
(2) Extracting slag at each stage, and extracting slag and controlling temperature: namely, the production of the single crystal is carried out in sections, slag extraction treatment is carried out in each section, the bottom power is closed before the last barrel material is added, and the main power is set to be 65-75kw;
(3) Impurities are treated in different cases:
a. if impurities appear in the temperature regulation process, carrying out primary crystallization and slag extraction, namely reducing the power to 8-10kw to enable the liquid level of the silicon melt in the crucible to be influenced by the temperature to form a layer of crystalline surface, wherein the crystalline surface of the layer can adhere to infusible impurities on the surface of the silicon melt, so that slag-eating broken lines of crystals in the process of constant diameter are prevented from being caused by the impurities;
b. if impurities appear in the shouldering process, the shouldering and slag adhering are carried out, namely, during the growth process of the single crystal, the meltback is carried out due to wire breakage, when the meltback reaches the shoulder of the single crystal, the power is reduced, the shape of the shoulder is kept, the infusible impurities floating on the surface of the molten silicon are adhered, and then the shoulder and the impurities are extracted together;
c. if impurities appear in the process of equal diameter, equal diameter wire breakage and secondary crystallization slag extraction are carried out, namely, in the normal drawing process of the monocrystalline silicon, the four ridge lines at the surface end of the monocrystalline silicon are broken due to external interference factors such as temperature, drawing speed, impurities or mechanical oscillation, and dislocation polycrystalline parts are formed, and the dislocation polycrystalline parts cannot be used as monocrystalline products, and the step of crystallization slag extraction is repeated after equal diameter wire breakage;
(4) Independent process adjustment between breaking line areas: if the broken line interval is less than or equal to 400mm and the drawing is less than or equal to 2 times, the temperature-adjusting crucible rotates for 8 turns, the furnace pressure is set to be 15torr, the argon flow is given to l00slpm, if the drawing is more than 2 times, no effective output exists, the polycrystal is lifted by 300mm, and the polycrystal is drawn again.
The invention improves the single crystal crystallization process, improves the crystallization rate, improves the utilization rate of raw materials, and effectively recycles the single crystal waste material, before the method is used, the crystallization rate of the raw crucible bottom waste material is 60 percent, the yield is 40 percent, after the method is used, the crystallization rate of the ingot casting purification recycled material can reach 80 percent, and the yield can reach 64 percent.
In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.
Claims (5)
1. The utility model provides a method for improving the crystal forming rate in purification of single crystal crucible bottom waste material ingot casting, includes that single crystal waste material collects the back, through polycrystal ingot casting process, heating, melting, growing brilliant, produce available polycrystal after annealing and cooling, get rid of top skin and flaw-piece again, the production is carried out to single crystal process to surplus raw materials retrieval and utilization, the polycrystal that single crystal waste material ingot casting produced is after throwing into the single crystal furnace, through the melt, draw the brilliant, put shoulder, constant diameter and the effective single crystal of process output of ending, its characterized in that includes:
(1) After feeding is finished, namely after the polycrystal generated by the single crystal waste ingot casting is put into a single crystal furnace, setting the flow rate of argon gas to be 200-220slpm, and blowing for 3-5min;
(2) Extracting slag in each section, and extracting slag and controlling temperature: closing the bottom adding power before adding the last cylinder material, and setting the main adding power to be 65-75kw;
(3) Impurities are treated in different cases: if impurities appear in the temperature adjusting process, the shouldering process or the equal-diameter process, the impurities are respectively treated in different modes;
(4) Independent process adjustment between breaking line areas: if the broken line interval is less than or equal to 400mm and the drawing is less than or equal to 2 times, the temperature-adjusting crucible rotates for 8 turns, the furnace pressure is set to be 15torr, the argon flow is given to l00slpm, if the drawing is more than 2 times, no effective output exists, the polycrystal is lifted by 300mm, and the polycrystal is drawn again.
2. The method for improving the crystallization rate in the purification of the single crystal crucible bottom waste ingot according to claim 1, characterized in that:
in the step (3), if impurities appear in the temperature adjusting process, once crystallization is carried out to extract slag, namely, the power is reduced, so that the liquid level of the molten silicon in the crucible is influenced by the temperature to form a layer of crystalline surface, and the layer of crystalline surface can adhere to infusible impurities on the surface of the molten silicon, thereby preventing the impurities from causing slag-eating broken lines of crystals in the process of constant diameter.
3. The method for improving the crystallization rate in the purification of the single crystal crucible bottom waste ingot according to claim 1 or 2, characterized in that:
in the step (3), if impurities appear in the shouldering process, the shouldering is soaked and adhered, namely, during the growth of the single crystal, meltback is needed due to wire breakage, when the single crystal is remelted to the shoulder part, the power is reduced, the shape of the shoulder part is maintained, infusible impurities floating on the surface of the molten silicon are adhered, and then the shoulder part and the impurities are extracted together.
4. The method for improving the crystallization rate in the ingot purification of the single crystal crucible bottom waste according to claim 1 or 2, characterized in that:
in the step (3), if impurities appear in the process of equal diameter, the equal diameter is broken, secondary crystallization is carried out, and slag is extracted, namely, in the normal drawing process of the monocrystalline silicon, four ridge lines at the surface end of the crystal are broken due to external interference factors, a dislocation polycrystalline part is formed, the part cannot be used as a monocrystalline product, and the step of crystallization and slag extraction is repeated after the equal diameter is broken.
5. The method for improving the crystallization rate in the purification of the single crystal crucible bottom waste ingot according to claim 4, characterized in that:
in the step (3), the power in the crystallization extraction slag is reduced to 8-10kw.
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| CN202210955098.0A CN115354387A (en) | 2022-08-10 | 2022-08-10 | Method for improving crystallization rate in ingot purification of monocrystalline crucible bottom waste |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08208369A (en) * | 1995-02-02 | 1996-08-13 | Sumitomo Metal Ind Ltd | Method for growing single crystal |
| CN102212872A (en) * | 2011-05-20 | 2011-10-12 | 浙江星宇能源科技有限公司 | Shoulder-lifting edulcoration method in monocrystal production process |
| CN102242397A (en) * | 2011-07-15 | 2011-11-16 | 西安华晶电子技术股份有限公司 | Process for producing Czochralski silicon single crystal |
| CN105887190A (en) * | 2016-04-20 | 2016-08-24 | 佳科太阳能硅(龙岩)有限公司 | Method for purifying and recovering gallium-doped ingot top materials |
| CN110685010A (en) * | 2019-10-30 | 2020-01-14 | 晶科能源有限公司 | Efficient polycrystalline silicon ingot casting method |
| CN110983427A (en) * | 2019-12-27 | 2020-04-10 | 内蒙古中环光伏材料有限公司 | Repeated segment taking and re-casting process for large-diameter single crystal silicon rod |
| CN111020192A (en) * | 2019-10-30 | 2020-04-17 | 福达合金材料股份有限公司 | Method for purifying and recycling AgCd alloy from AgCd waste |
| CN112301426A (en) * | 2019-08-02 | 2021-02-02 | 宁夏隆基硅材料有限公司 | Method for manufacturing silicon single crystal rod |
-
2022
- 2022-08-10 CN CN202210955098.0A patent/CN115354387A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08208369A (en) * | 1995-02-02 | 1996-08-13 | Sumitomo Metal Ind Ltd | Method for growing single crystal |
| CN102212872A (en) * | 2011-05-20 | 2011-10-12 | 浙江星宇能源科技有限公司 | Shoulder-lifting edulcoration method in monocrystal production process |
| CN102242397A (en) * | 2011-07-15 | 2011-11-16 | 西安华晶电子技术股份有限公司 | Process for producing Czochralski silicon single crystal |
| CN105887190A (en) * | 2016-04-20 | 2016-08-24 | 佳科太阳能硅(龙岩)有限公司 | Method for purifying and recovering gallium-doped ingot top materials |
| CN112301426A (en) * | 2019-08-02 | 2021-02-02 | 宁夏隆基硅材料有限公司 | Method for manufacturing silicon single crystal rod |
| CN110685010A (en) * | 2019-10-30 | 2020-01-14 | 晶科能源有限公司 | Efficient polycrystalline silicon ingot casting method |
| CN111020192A (en) * | 2019-10-30 | 2020-04-17 | 福达合金材料股份有限公司 | Method for purifying and recycling AgCd alloy from AgCd waste |
| CN110983427A (en) * | 2019-12-27 | 2020-04-10 | 内蒙古中环光伏材料有限公司 | Repeated segment taking and re-casting process for large-diameter single crystal silicon rod |
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