CN115478322B - Charging method for re-returning ultrathin silicon wafer to furnace - Google Patents
Charging method for re-returning ultrathin silicon wafer to furnace Download PDFInfo
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- CN115478322B CN115478322B CN202211169762.5A CN202211169762A CN115478322B CN 115478322 B CN115478322 B CN 115478322B CN 202211169762 A CN202211169762 A CN 202211169762A CN 115478322 B CN115478322 B CN 115478322B
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 71
- 239000010703 silicon Substances 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 25
- 235000012431 wafers Nutrition 0.000 claims abstract description 53
- 239000000463 material Substances 0.000 claims abstract description 52
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052786 argon Inorganic materials 0.000 claims abstract description 20
- 239000013078 crystal Substances 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 230000002159 abnormal effect Effects 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 9
- 239000002210 silicon-based material Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- 238000000137 annealing Methods 0.000 claims 6
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000000903 blocking effect Effects 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract description 2
- 230000008018 melting Effects 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 description 7
- 238000010309 melting process Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 4
- 238000007664 blowing Methods 0.000 description 2
- 230000005856 abnormality Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
-
- 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
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
- C30B35/007—Apparatus for preparing, pre-treating the source material to be used for crystal growth
Abstract
The invention discloses a charging method for re-returning an ultrathin silicon wafer to a furnace, which comprises the steps of stirring 10-20 kg of crushed ultrathin silicon wafers and 40-50 kg of conventional re-charging materials in a tetrafluoro box, uniformly mixing and then adding the materials into a charging barrel; then adding 10-20 kg of conventional re-feeding materials above the mixture; repeating the steps, sequentially adding the 1 st, the 2 nd, the 3 th and the … … (n-1) barrels, and adding conventional re-feeding materials into the nth barrel, so that the sum of all the feeding materials in the 1 st to n th barrels is equal to the total feeding material to be filled; the argon flow in the feeding is increased to 130-150 slpm, the dry pump frequency is adjusted to 100%, the feeding interval time is shortened to 35-50 min, the single crystal furnace melting power is set to be 80-90 kw of the bottom heater, and the main heater is 100-110 kw. The invention has the advantages that the ultra-thin silicon can be recycled, the blocking of the ultra-thin silicon chip in the feeding process is avoided, and the feeding efficiency, the quality of the silicon rod and the yield are improved.
Description
Technical Field
The invention relates to the technical field of ultrathin silicon wafer production, in particular to a charging method for returning ultrathin silicon wafers to a furnace.
Background
When silicon wafer, battery piece and photovoltaic module enterprises expand production by a wide margin, the increase of the productivity of the silicon material is relatively slow, the structural supply and demand of the upstream and downstream are unbalanced, the price of the silicon material is greatly increased, and the cost of the silicon material of a company is greatly increased, so that the cost of the silicon material of the company is a necessary trend, the recycling of the waste ultrathin silicon wafer is reasonably used, the cost of the silicon material of the company is reduced, the profit margin is increased, and the competitiveness of the company is improved.
At present, an ultrathin silicon wafer is crushed into a sheet shape, the fluidity is poor, the ultrathin silicon wafer is easy to adhere in a high-temperature feeding process, a material clamping phenomenon of a charging barrel is caused, and the feeding efficiency is influenced. Meanwhile, the ultrathin silicon wafer has large specific surface area, tiny impurities in the air are easy to adsorb during crushing, and the tiny impurities are attached to the inner surface of the single crystal furnace after the charging is finished, so that the growth of the single crystal silicon rod is adversely affected, and the yield of the single crystal silicon rod is influenced.
Disclosure of Invention
The invention aims to solve the problems that the existing ultra-thin silicon wafer feeding is easy to adhere, the efficiency is low and the quality of a crystal bar is affected by the adhesion of impurities, and provides a feeding method for re-returning ultra-thin silicon wafers, which can realize the re-returning of ultra-thin silicon wafers, avoid the blocking of the ultra-thin silicon wafers in the feeding process, reduce the influence on the growth of a single crystal furnace and the single crystal silicon bar during the feeding of the ultra-thin silicon wafers, and improve the feeding efficiency and the yield of the silicon bar.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the charging method for re-returning the ultrathin silicon wafer comprises the following specific steps of:
(1) Mixing: firstly, stirring 10-20 kg of crushed ultrathin silicon wafers and 40-50 kg of conventional re-feeding materials in a tetrafluoro box to fully mix the crushed ultrathin silicon wafers and the conventional re-feeding materials, and adding the crushed ultrathin silicon wafers and the conventional re-feeding materials into a charging barrel after uniformly mixing;
(2) Pressing: after adding the ultrathin silicon wafer mixture, adding 10-20 kg of conventional re-feeding material above the mixture to press the ultrathin silicon wafer by the upper lump material, and performing material melting at the bottom of the silicon liquid to reduce abnormal accidents and broken wires;
(3) And (2) charging: repeating the steps (1) and (2), sequentially adding the 1 st, 2 nd, 3 th and … … (n-1) barrels, and adding conventional re-feeding materials into the nth barrel, so that the sum of all the feeding materials in the 1 st to n th barrels is equal to the total feeding material to be filled;
(4) Argon flow and dry pump frequency adjustment: in the feeding process, the argon flow is increased from 80-100 slpm to 130-150 slpm, the dry pump frequency is adjusted from 60% to 100%, the high-flow argon can enhance the blowing capacity, the high-flow argon has stronger suction force, the high-flow argon can effectively take away tiny impurities adsorbed on the surface of an ultrathin silicon wafer, and the impurities can be restrained from being adsorbed on the inner surface of a single crystal furnace, so that the growth of a subsequent silicon single crystal is facilitated;
(5) And (3) controlling feeding interval time: the feeding interval time of two adjacent barrels of ultrathin silicon wafers is shortened from 45-60 min to 35-50 min for feeding;
(6) Heater power adjustment: the normalizing power of the single crystal furnace is set to 80-90 kw of the bottom heater and 100-110 kw of the main heater.
Further, in the step (1), the diameter of the ultrathin silicon wafer is 3-20 mm, and the feeding amounts of the ultrathin silicon wafer and the conventional re-feeding are 20kg and 50kg respectively.
Further, in the step (2), the conventional re-feeding amount of the secondary addition is 10kg.
Further, in the steps (4) - (6), the bottom heater is 85kw, the main heater is 105kw, the argon flow is 130slpm, and the dry pump frequency is adjusted to 100%.
In the step (5), in order to prevent the crucible from being damaged due to too high temperature, the feeding interval time is shortened, and the feeding is controlled to be 30-45 min.
Further, in the step (6), if the material waiting or abnormal conditions are met, in order to prevent the silicon liquid in the furnace from boiling, the bottom heating power is reduced to 60-70 kw, the main heating power is reduced to 80-100 kw, the material is fed after the material is kept for 20-30 min, and the heating power is recovered to be normal after the ultra-thin silicon wafer is added.
Further, in the step (6), when an abnormal condition is met, the power of the bottom heater is reduced to 70kw, the main power is increased to 95kw, the silicon liquid is kept stable after 24 minutes, an ultrathin silicon wafer is added at the moment, the power of the bottom heater is recovered to 85kw after the silicon material is added, the main power is recovered to 105kw, the argon flow is 130slpm, the opening of a dry pump is 100%, and the furnace pressure is 9.4torr.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) According to the invention, the crushed ultrathin silicon wafer is mixed with the conventional re-feeding material, and the ultrathin silicon wafer after mixing drives the ultrathin silicon wafer to fall along with the falling of large lump materials in the feeding process, so that the re-furnace application of the ultrathin silicon wafer is realized;
(2) According to the invention, the lump materials are added on the mixture, so that an ultrathin silicon wafer can be effectively pressed, the material is melted at the bottom of the silicon liquid, and abnormal accidents and broken wires are reduced;
(3) The high-flow argon can enhance the blowing capacity, and the higher opening degree of the dry pump has stronger suction force, so that the high-flow argon can effectively take away tiny impurities adsorbed on the surface of an ultrathin silicon wafer, inhibit the impurities from being adsorbed on the inner surface of a single crystal furnace, and facilitate the growth of subsequent silicon single crystals;
(4) The method shortens the feeding interval time, controls the temperature in the single crystal furnace and prevents abnormal accidents such as crucible bulge and the like;
(5) According to the invention, the heating power is adjusted, so that the temperature of the silicon liquid in the furnace can be quickly reduced, and the abnormality caused by crucible damage due to overhigh temperature can be prevented.
Drawings
Fig. 1 is a schematic diagram showing the distribution of the charging mode of the present invention.
Detailed Description
Example 1
In order that the invention may become more readily apparent, a method for charging an ultra-thin silicon wafer back to the furnace according to the present invention will be further described with reference to the accompanying drawings, wherein the specific embodiments described herein are for illustrative purposes only and are not limiting.
Taking 36 inch thermal field as an example, the granular silicon is added with 450kg of material, and the specific steps are as follows:
1) After the crystal bar is normally ended, on-site production personnel report the material to inform a loading room of 450kg of secondary feeding quantity.
2) The operator of the loading room loads according to the ultra-thin silicon wafer feeding technology in sequence:
a. weighing 20kg of fragment materials and 50kg of conventional re-feeding materials by using an electronic scale;
b. stirring in a tetrafluoro box to fully mix the materials;
c. adding uniformly mixed raw materials into a charging barrel, and adding 10kg of conventional re-charging materials above the charging barrel after the charging is finished;
d. repeatedly adding 1, 2, 3, 4 and 5 barrels according to the steps, wherein the barrel loading amount is 80kg;
e. adding 50kg of conventional re-feeding materials into a 6 th barrel;
f. and after the loading is completed, loading personnel send the materials to the site.
3) And (3) feeding by on-site production personnel after taking out the crystal bars:
a. adding a 1 st barrel: the power of the bottom heater is 85kw, the main power is 105kw, the argon flow is 130slpm, the opening of the dry pump is 100%, the furnace pressure is 8.9torr, and the material melting process is not abnormal;
b. adding a 2 nd barrel material: the feeding interval time is 38min, the bottom heater power is 85kw, the main feeding power is 105kw, the argon flow is 130slpm, the opening of a dry pump is 100%, the furnace pressure is 8.7torr, and the material melting process is not abnormal;
c. adding a 3 rd barrel: the feeding interval time is 41min, the bottom heater power is 85kw, the main feeding power is 105kw, the argon flow is 130slpm, the opening of a dry pump is 100%, the furnace pressure is 8.6torr, and the material melting process is not abnormal;
d. adding a 4 th barrel material: the feeding interval time is 45min, the bottom heater power is 85kw, the main feeding power is 105kw, the argon flow is 130slpm, the opening of a dry pump is 100%, the furnace pressure is 9.1torr, and the material melting process is not abnormal;
e. adding a 5 th barrel material: and (5) boiling the silicon liquid in the furnace after the material is prepared. The power of the bottom heater is reduced to 70kw, the main power is added to 95kw, the silicon liquid is kept stable after 24min, and the silicon material is added at the moment. The power of the bottom heater is recovered to 85kw after the silicon material is added, the main power is recovered to 105kw, the argon flow is 130slpm, the opening of a dry pump is 100%, the furnace pressure is 9.4torr, and the material melting process is not abnormal in the state;
f. adding a 6 th barrel material: the feeding interval time is 50min, the bottom heater power is 85kw, the main feeding power is 105kw, the argon flow is changed to 80slpm, the opening of a dry pump is 60%, and the furnace pressure is 13.2torr.
4) After the feeding is finished, normal temperature adjustment and guiding and discharging are carried out.
The method can realize the re-furnace use of the ultrathin silicon, reduce the cost of companies, increase profit margin, improve economic benefit and improve the quality and yield of the monocrystalline silicon rod.
In addition to the embodiments described above, other embodiments of the invention are possible. All technical schemes formed by equivalent substitution or equivalent transformation fall within the protection scope of the invention.
Claims (7)
1. The charging method for re-returning the ultrathin silicon wafer comprises the following specific steps of adjusting the charging mode of the ultrathin silicon wafer and adjusting the charging process, and is characterized by comprising the following steps of:
(1) Mixing: firstly, stirring 10-20 kg of crushed ultrathin silicon wafers and 40-50 kg of conventional re-feeding materials in a tetrafluoro box to fully mix the crushed ultrathin silicon wafers and the conventional re-feeding materials, and adding the crushed ultrathin silicon wafers and the conventional re-feeding materials into a charging barrel after uniformly mixing;
(2) Pressing: adding 10-20 kg of conventional re-feeding materials above the ultra-thin silicon wafer mixture after adding the ultra-thin silicon wafer mixture;
(3) And (2) charging: repeating the steps (1) and (2), sequentially adding the 1 st, 2 nd, 3 th and … … (n-1) barrels, and adding conventional re-feeding materials into the nth barrel, so that the sum of all the feeding materials in the 1 st to n th barrels is equal to the total feeding material to be filled;
(4) Argon flow and dry pump frequency adjustment: in the feeding process, the argon flow is increased from 80-100 slpm to 130-150 slpm, and the dry pump frequency is adjusted from 60% to 100%;
(5) And (3) controlling feeding interval time: the feeding interval time of two adjacent barrels of ultrathin silicon wafers is shortened from 45-60 min to 35-50 min for feeding;
(6) Heater power adjustment: the normalizing power of the single crystal furnace is set to 80-90 kw of the bottom heater and 100-110 kw of the main heater.
2. The charging method for re-annealing ultra-thin silicon wafers according to claim 1, wherein the charging method comprises the following steps:
in the step (1), the diameter of the ultrathin silicon wafer is 3-20 mm, and the feeding amounts of the ultrathin silicon wafer and the conventional re-feeding are 20kg and 50kg respectively.
3. The charging method for re-annealing ultra-thin silicon wafers according to claim 1 or 2, characterized in that:
in the step (2), the conventional re-feeding material for secondary feeding is 10kg.
4. The charging method for re-annealing ultra-thin silicon wafers according to claim 1 or 2, characterized in that:
in the steps (4) - (6), the bottom heater is 85kw, the main heater is 105kw, the argon flow is 130slpm, and the dry pump frequency is adjusted to 100%.
5. The charging method for re-annealing ultra-thin silicon wafers according to claim 1 or 2, characterized in that:
in the step (5), in order to prevent the crucible from being damaged due to the too high temperature, the feeding interval time is shortened, and the feeding is performed in a manner of controlling the feeding interval time to be 30-45 min.
6. The charging method for re-annealing ultra-thin silicon wafers according to claim 1 or 2, characterized in that:
in the step (6), if the material waiting or abnormal conditions are met, in order to prevent the silicon liquid in the furnace from boiling, the bottom heating power is reduced to 60-70 kw, the main heating power is reduced to 80-100 kw, the material is fed after the material is kept for 20-30 min, and the heating power is recovered to be normal after the ultra-thin silicon wafer is added.
7. The charging method for re-annealing ultra-thin silicon wafers according to claim 6, wherein the charging method comprises the following steps:
in the step (6), when an abnormal condition is met, the power of the bottom heater is reduced to 70kw, the main power is increased to 95kw, the silicon liquid is kept stable after 24 minutes, an ultrathin silicon wafer is added at the moment, the power of the bottom heater is recovered to 85kw after the silicon material is added, the main power is recovered to 105kw, the argon flow is 130slpm, the opening of a dry pump is 100%, and the furnace pressure is 9.4torr.
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| CN202211169762.5A CN115478322B (en) | 2022-09-26 | 2022-09-26 | Charging method for re-returning ultrathin silicon wafer to furnace |
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| CN115478322B true CN115478322B (en) | 2023-11-21 |
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| JP4498457B1 (en) * | 2009-06-15 | 2010-07-07 | 佑吉 堀岡 | Crystal growth method |
| CN103014838A (en) * | 2012-12-27 | 2013-04-03 | 常州大学 | Czochralski preparation method of ultrathin monocrystalline silicon wafer |
| CN106315589A (en) * | 2015-06-23 | 2017-01-11 | 姚伟 | Method for processing recycling waste silicon material |
| CN106350866A (en) * | 2016-08-25 | 2017-01-25 | 常州大学 | Equipment and method for preparing ultrathin black silicon wafer |
| CN107815735A (en) * | 2016-09-14 | 2018-03-20 | 上海新昇半导体科技有限公司 | A kind of polysilicon secondary charging device and method |
| CN109537047A (en) * | 2019-01-03 | 2019-03-29 | 内蒙古中环光伏材料有限公司 | A kind of silicon material matching method improving monocrystalline quality |
| CN111807371A (en) * | 2020-07-21 | 2020-10-23 | 昆明理工大学 | Method for recycling silicon wafer cutting waste |
| CN113430639A (en) * | 2021-06-25 | 2021-09-24 | 江苏协鑫硅材料科技发展有限公司 | Feeding method of silicon material |
-
2022
- 2022-09-26 CN CN202211169762.5A patent/CN115478322B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4498457B1 (en) * | 2009-06-15 | 2010-07-07 | 佑吉 堀岡 | Crystal growth method |
| CN103014838A (en) * | 2012-12-27 | 2013-04-03 | 常州大学 | Czochralski preparation method of ultrathin monocrystalline silicon wafer |
| CN106315589A (en) * | 2015-06-23 | 2017-01-11 | 姚伟 | Method for processing recycling waste silicon material |
| CN106350866A (en) * | 2016-08-25 | 2017-01-25 | 常州大学 | Equipment and method for preparing ultrathin black silicon wafer |
| CN107815735A (en) * | 2016-09-14 | 2018-03-20 | 上海新昇半导体科技有限公司 | A kind of polysilicon secondary charging device and method |
| CN109537047A (en) * | 2019-01-03 | 2019-03-29 | 内蒙古中环光伏材料有限公司 | A kind of silicon material matching method improving monocrystalline quality |
| CN111807371A (en) * | 2020-07-21 | 2020-10-23 | 昆明理工大学 | Method for recycling silicon wafer cutting waste |
| CN113430639A (en) * | 2021-06-25 | 2021-09-24 | 江苏协鑫硅材料科技发展有限公司 | Feeding method of silicon material |
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