CN108754603A - A kind of production method of ingot casting - Google Patents

A kind of production method of ingot casting Download PDF

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Publication number
CN108754603A
CN108754603A CN201810643061.8A CN201810643061A CN108754603A CN 108754603 A CN108754603 A CN 108754603A CN 201810643061 A CN201810643061 A CN 201810643061A CN 108754603 A CN108754603 A CN 108754603A
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CN
China
Prior art keywords
ingot
ingot casting
production method
stove
gas
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Pending
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CN201810643061.8A
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Chinese (zh)
Inventor
冷金标
龙昭钦
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Zhejiang Jinko Solar Co Ltd
Jinko Solar Co Ltd
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Zhejiang Jinko Solar Co Ltd
Jinko Solar Co Ltd
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Priority to CN201810643061.8A priority Critical patent/CN108754603A/en
Publication of CN108754603A publication Critical patent/CN108754603A/en
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B28/00Production of homogeneous polycrystalline material with defined structure
    • C30B28/04Production of homogeneous polycrystalline material with defined structure from liquids
    • C30B28/06Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B33/00After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/02Heat treatment

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Silicon Compounds (AREA)

Abstract

This application discloses a kind of production methods of ingot casting, including heating process, melting process, long crystalline substance process, annealing operation, cooling process and process of coming out of the stove, the cooling process is the flowing stopped between ingot furnace internal gas and the outer gas of stove, it keeps being pressure constant state of the pressure in 400mbar to 800mbar inside ingot furnace, the heat of ingot casting itself is conducted via the ingot furnace internal gas to fluid pipeline, and heat is brought to outside stove via the liquid that circulates in the fluid pipeline, the production method of above-mentioned ingot casting, the stress of silicon ingot can be reduced, Crack prevention generates, reduce dislocation density, improve minority carrier life time, also it is avoided that impurity diffusion is entered, improve utilization rate of silicon ingot and photoelectric conversion efficiency, reduce production cost.

Description

A kind of production method of ingot casting
Technical field
The invention belongs to photovoltaic apparatus manufacturing technology fields, more particularly to a kind of production method of ingot casting.
Background technology
The basic material of silica-based solar cell is polysilicon chip and monocrystalline silicon piece at present, and polysilicon chip is former with polysilicon Material is fabricated through ingot casting and slice.The common process of polycrystalline silicon ingot casting is:Heating → fusing → long crystalline substance → annealing → cooling → come out of the stove.
In order to obtain excellent silicon ingot, handle well it is long it is brilliant after silicon ingot annealing and cooling process it is particularly significant, currently, silicon ingot Annealing and cooling process be to be carried out in the environment for being passed through argon gas.Polycrystalline cast ingot annealing operation under normal circumstances, is logical It crosses argon gas flowing atmosphere and takes away heat, it is the flowing in argon gas that achieving the purpose that, which reduces silicon ingot thermal stress and defect, cooling process, In atmosphere, achieve the purpose that cool.In this conventional method, since the argon gas for cooling being passed through is quickly to flow It moves and passes through polycrystalline ingot furnace, residence time is shorter in ingot furnace, the thermal Finite taken away, due to ingot furnace furnace wall Cooling water is connected in hollow structure, the cooling water in furnace wall can manual control flow velocity, to take away certain heat.Above-mentioned In traditional ingot casting annealing and cooling procedure, since the heat that the cooling water of furnace wall flowing is taken away is less, argon gas flows atmosphere mould Formula take away heat mode account for it is leading.
Since in above-mentioned conventional anneal and the type of cooling, temperature decline is too fast, and the stress of silicon ingot can be caused to increase, caused hidden Crackle brings high density dislocation, and then is impacted to silicon ingot minority carrier life time, the final utilization rate for influencing silicon ingot and silicon chip Photoelectric conversion efficiency, and impurity is easy to diffuse into and generates implant damage in silicon ingot, leads to the growth of secondary defect, reduces silicon ingot Utilization rate, improve production cost.
Invention content
To solve the above problems, the present invention provides a kind of production method of ingot casting, the stress of silicon ingot can be reduced, is avoided Crackle generates, and reduces dislocation density, improves minority carrier life time, is also avoided that impurity diffusion is entered, and improves utilization rate of silicon ingot and photoelectricity Transfer efficiency reduces production cost.
A kind of production method of ingot casting provided by the invention, including heating process, melting process, long brilliant process, lehr attendant Sequence, cooling process and process of coming out of the stove, the cooling process are the flowing stopped between ingot furnace internal gas and the outer gas of stove, It keeps inside ingot furnace being pressure constant state of the pressure in 400mbar to 800mbar, the heat of ingot casting itself is via the ingot casting Furnace interior gas conduction brings heat to outside stove to fluid pipeline, and via the liquid that circulates in the fluid pipeline.
Preferably, in the production method of above-mentioned ingot casting, the annealing operation be in vacuum environment to the ingot casting into Row annealing.
Preferably, in the production method of above-mentioned ingot casting, the pressure of the pressure constant state is 600mbar.
Preferably, in the production method of above-mentioned ingot casting, the ingot furnace internal gas is argon gas.
Preferably, in the production method of above-mentioned ingot casting, the liquid that circulates is deionized water.
Preferably, in the production method of above-mentioned ingot casting, the fluid pipeline is set to inside the furnace wall of the ingot furnace.
Preferably, in the production method of above-mentioned ingot casting, the cooling process duration range is 12 hours to 20 Hour.
Preferably, in the production method of above-mentioned ingot casting, the annealing operation duration range is 12 hours to 16 Hour.
Preferably, in the production method of above-mentioned ingot casting, the temperature range that the annealing operation uses for 1100 DEG C extremely 1370℃。
By foregoing description it is found that the production method of above-mentioned ingot casting provided by the invention, since the cooling process is to stop The only flowing between ingot furnace internal gas and the outer gas of stove keeps being pressure inside ingot furnace in 400mbar to 800mbar Pressure constant state, the heat of ingot casting itself conducts via the ingot furnace internal gas to fluid pipeline, and via the liquid The liquid that circulates in pipeline brings heat to outside stove, and the contact between this internal gas and ingot casting itself is more abundant, this The rate that kind internal gas takes away heat more mitigates, therefore the cooling rate at each position of ingot casting is more uniform, so as to The stress of silicon ingot is reduced, Crack prevention generates, and reduces dislocation density, improves minority carrier life time, is also avoided that impurity diffusion is entered, and is carried High utilization rate of silicon ingot and photoelectric conversion efficiency reduce production cost.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis The attached drawing of offer obtains other attached drawings.
Fig. 1 is the schematic diagram of the production method of the first ingot casting provided by the embodiments of the present application.
Specific implementation mode
Core of the invention thought is to provide a kind of production method of ingot casting, can reduce the stress of silicon ingot, avoid splitting Line generates, and reduces dislocation density, improves minority carrier life time, is also avoided that impurity diffusion is entered, and improves utilization rate of silicon ingot and turns with photoelectricity Efficiency is changed, production cost is reduced.
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
As shown in FIG. 1, FIG. 1 is the embodiment of the present application offers for the production method of the first ingot casting provided by the embodiments of the present application The first ingot casting production method schematic diagram, including:
S1:Heating process;
Specifically, can be by temperature rise to 1175 DEG C, heat-insulation cage is closed during being somebody's turn to do, and furnace pressure range is 200 to 600mbar, duration 3-7h.
S2:Melting process;
Specifically, the process of this to be P be converted into T, for temperature within the scope of 1175 to 1550 DEG C, which melts silicon material Change, solid phase silicon is fused into liquid phase, furnace pressure is 400 to 800mbar, charge flow rate 55 to 75L/min, the duration be 14 to 18h。
S3:Long crystalline substance process;
Specifically, long crystalline substance is crystal growing process, driving force is mainly used as by vertical temperature gradient, temperature range is 1380 to 1410 DEG C, the ranging from 6.0cm to 22cm of heat-insulated cage location, the duration is 35 to 40h.
S4:Annealing operation;
Specifically, this annealing operation is the process of a cooling, it is main to eliminate because temperature reduces the stress generated.
S5:Cooling process, the cooling process are the flowing stopped between ingot furnace internal gas and the outer gas of stove, are kept It is pressure constant state of the pressure in 400mbar to 800mbar inside ingot furnace, this pressure range is conducive to ingot melting and long The thermal convection current in brilliant stage and the discharge of impurity, the impurity referred here to mainly include oxygen impurities and carbon impurity, ingot casting itself Heat is conducted via the ingot furnace internal gas to fluid pipeline, and will via the liquid that circulates in the fluid pipeline Heat is brought to outside stove;
It should be noted that technique provided herein it is targeted can be polycrystal silicon ingot, can also be class monocrystal silicon Or other kinds of silicon ingot, it being not intended to limit herein, this type of cooling proposed here is properly termed as a kind of pressurize cooling technique, Namely enter after cooling stage, ingot furnace neither air inlet also holds one's breath, and a pressure constant state is kept into, until pourer Skill flow terminates, and during carrying out this technique, the heat of ingot casting itself is constantly dispersed into surrounding gas, is caused The temperature of gas and the temperature of ingot casting itself are consistent in furnace body, and this process is just as the stove in a closed room is by entire room Between air themperature be all increased to same temperature, at this point, in furnace body gas generate expansion, be evenly distributed in furnace body Interior, since gas distribution area is wide, the medium as heat transfer can be transmitted to more heats fluid pipeline, and utilize liquid Liquid is circulated in pipeline, it will be able to heat be brought to outside stove, and static gas phase for flowing in the prior art Gas for, the gas distribution around ingot casting itself is more uniform, and this makes it possible to realize each position of ingot casting itself more Uniform cooling, moreover, cooling rate can be controlled better, about the position of fluid pipeline used here, this Place does not limit, if the heat taken away in gas that can be more efficient, and the class of liquids in this fluid pipeline It does not limit, can be deionized water, can also be organic liquid, as long as can efficiently flow to take away furnace gas conduction The heat to come over carries out temperature with high efficiency to ingot casting itself.
S6:It comes out of the stove process.
By foregoing description it is found that the production method of above-mentioned ingot casting provided by the embodiments of the present application, due to the bosher Sequence is the flowing stopped between the outer gas of ingot furnace internal gas and stove, keep be pressure inside ingot furnace 400mbar extremely The heat of pressure constant state in 800mbar, ingot casting itself is conducted via the ingot furnace internal gas to fluid pipeline, and via The liquid that circulates in the fluid pipeline brings heat to outside stove, and the contact between this internal gas and ingot casting itself is more Fully, this internal gas is taken away the rate of heat and is more mitigated, therefore the cooling rate at each position of ingot casting is more uniform, from And the stress of silicon ingot can be reduced, Crack prevention generates, and reduces dislocation density, improves minority carrier life time, is also avoided that impurity diffusion Enter, improves utilization rate of silicon ingot and photoelectric conversion efficiency, and using this scheme without being passed through gas, therefore make and cast per stove The gas usage amount of ingot can reduce 35kg to 45kg, further decrease production cost.
The production method of second of ingot casting provided by the embodiments of the present application is the production method in the first above-mentioned ingot casting On the basis of, further include following technical characteristic:
The annealing operation is to anneal to the ingot casting in vacuum environment.
Temperature Distribution is more uniform in this way, and ingot furnace thermal field convection current is also relatively uniform
The production method of the third ingot casting provided by the embodiments of the present application is the production method in the first above-mentioned ingot casting On the basis of, further include following technical characteristic:
The pressure of the pressure constant state is 600mbar.
Test proves that the pressure of 600mbar can be more efficient heat dissipation, and heat dissipation uniformity is also more preferable, specifically, Can annealing and cooling technique be set according to table 1 using when this pressure:
Table 1 is annealed and cooling technique controls procedure parameter table
Wherein, MODE is stage set-up mode in certain process, and TIME is the duration set for each step, and T/P is Temp-controled mode/power control mode, INLET/OUTLET are input (air inlet)/output (outlet), and PREASURE is pressure Pattern, INSULATION are heat-insulation cage positions, and Gas is gas mode, and Vacuum is vacuum mode, and A1, A2 ... A5, which refer to, to move back Five stages of fire, C1, C2 ... C5 refer to five cooling stages.
As it can be seen that in this embodiment, the cooling procedure under the annealing process and gas mode under vacuum state is used, In this case, ingot casting cooling temperature rate is more uniform, and the thermal stress of ingot casting is discharged, better medium is provided, can To reduce the dislocation value of entire silicon ingot, the photoelectric conversion efficiency for the battery subsequently produced is improved, specifically, efficiency can be put forward High 0.02% to 0.05%.
The production method of 4th kind of ingot casting provided by the embodiments of the present application, be it is above-mentioned the first to the third ingot casting system Make it is any in method on the basis of, further include following technical characteristic:
The ingot furnace internal gas is argon gas.
It should be noted that the gas is selected as argon gas by this preferred embodiment, cost is relatively low and technical maturity, removes certainly Except argon gas, other kinds of inert gas, such as helium or neon etc. can also be selected according to actual needs, herein simultaneously It does not limit, as long as not reacting with ingot casting.
The production method of 5th kind of ingot casting provided by the embodiments of the present application, be it is above-mentioned the first to the third ingot casting system Make it is any in method on the basis of, further include following technical characteristic:
The liquid that circulates is deionized water.
It should be noted that this deionized water, which is that one kind is most common, circulates liquid, cost is relatively low, but this Only it is one of preferred embodiment, other kinds of liquid can also be selected according to actual needs, be not intended to limit herein, as long as energy It is enough effectively to take away furnace heat.
The production method of 6th kind of ingot casting provided by the embodiments of the present application is the production method in above-mentioned 5th kind of ingot casting On the basis of, further include following technical characteristic:
The fluid pipeline is set to inside the furnace wall of the ingot furnace.
It should be noted that existing fluid pipeline is arranged inside furnace wall, design so compacter, but this is only one Fluid pipeline can also actually be arranged in furnace inner space, be not intended to limit herein by kind preferred embodiment according to actual needs.
The production method of 7th kind of ingot casting provided by the embodiments of the present application, be it is above-mentioned the first to the third ingot casting system Make it is any in method on the basis of, further include following technical characteristic:
The cooling process duration range is 12 hours to 20 hours.
The production method of 8th kind of ingot casting provided by the embodiments of the present application, is the production method in above-mentioned second of ingot casting On the basis of, further include following technical characteristic:
The annealing operation duration range is 12 hours to 16 hours.
The production method of 9th kind of ingot casting provided by the embodiments of the present application is the production method in above-mentioned 8th kind of ingot casting On the basis of, further include following technical characteristic:
The temperature range that the annealing operation uses is 1100 DEG C to 1370 DEG C.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, as defined herein General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one The widest range caused.

Claims (9)

1. a kind of production method of ingot casting, including heating process, melting process, long brilliant process, annealing operation, cooling process and It comes out of the stove process, which is characterized in that the cooling process is the flowing stopped between ingot furnace internal gas and the outer gas of stove, is kept It is pressure constant state of the pressure in 400mbar to 800mbar inside ingot furnace, the heat of ingot casting itself is via in the ingot furnace Portion's gas conduction brings heat to outside stove to fluid pipeline, and via the liquid that circulates in the fluid pipeline.
2. the production method of ingot casting according to claim 1, which is characterized in that the annealing operation is in vacuum environment It anneals to the ingot casting.
3. the production method of ingot casting according to claim 1, which is characterized in that the pressure of the pressure constant state is 600mbar。
4. according to the production method of claim 1-3 any one of them ingot castings, which is characterized in that the ingot furnace internal gas For argon gas.
5. according to the production method of claim 1-3 any one of them ingot castings, which is characterized in that the liquid that circulates is Deionized water.
6. the production method of ingot casting according to claim 5, which is characterized in that the fluid pipeline is set to the ingot casting Inside the furnace wall of stove.
7. according to the production method of claim 1-3 any one of them ingot castings, which is characterized in that the cooling process is lasting Time range is 12 hours to 20 hours.
8. the production method of ingot casting according to claim 2, which is characterized in that the annealing operation duration range It is 12 hours to 16 hours.
9. the production method of ingot casting according to claim 8, which is characterized in that the temperature range that the annealing operation uses It is 1100 DEG C to 1370 DEG C.
CN201810643061.8A 2018-06-21 2018-06-21 A kind of production method of ingot casting Pending CN108754603A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113073392A (en) * 2021-03-31 2021-07-06 哈尔滨科友半导体产业装备与技术研究院有限公司 Treatment method for reducing thermal stress of crystal

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102296368A (en) * 2011-09-02 2011-12-28 江西赛维Ldk太阳能高科技有限公司 Method for reducing thermal stress of crystal
CN102691110A (en) * 2012-06-13 2012-09-26 天津英利新能源有限公司 Annealing process for ingot furnace
CN102978709A (en) * 2012-11-16 2013-03-20 晶科能源有限公司 Efficient cooling technical method of polycrystal ingot casting
CN103343391A (en) * 2013-07-16 2013-10-09 江西旭阳雷迪高科技股份有限公司 Polysilicon cast ingot annealing and cooling technology

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102296368A (en) * 2011-09-02 2011-12-28 江西赛维Ldk太阳能高科技有限公司 Method for reducing thermal stress of crystal
CN102691110A (en) * 2012-06-13 2012-09-26 天津英利新能源有限公司 Annealing process for ingot furnace
CN102978709A (en) * 2012-11-16 2013-03-20 晶科能源有限公司 Efficient cooling technical method of polycrystal ingot casting
CN103343391A (en) * 2013-07-16 2013-10-09 江西旭阳雷迪高科技股份有限公司 Polysilicon cast ingot annealing and cooling technology

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113073392A (en) * 2021-03-31 2021-07-06 哈尔滨科友半导体产业装备与技术研究院有限公司 Treatment method for reducing thermal stress of crystal

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