CN108301038A - A kind of drawing method of pulling silicon single crystal stove and growing single-crystal silicon - Google Patents

A kind of drawing method of pulling silicon single crystal stove and growing single-crystal silicon Download PDF

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Publication number
CN108301038A
CN108301038A CN201710028070.1A CN201710028070A CN108301038A CN 108301038 A CN108301038 A CN 108301038A CN 201710028070 A CN201710028070 A CN 201710028070A CN 108301038 A CN108301038 A CN 108301038A
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China
Prior art keywords
silicon
crucible
pulling
sub
single crystal
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CN201710028070.1A
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Inventor
夏高强
范协诚
银波
王文
胡颖
罗飞飞
宋高杰
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Xinjiang Zhixin Technology Co Ltd
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Xinjiang Zhixin Technology Co Ltd
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Priority to CN201710028070.1A priority Critical patent/CN108301038A/en
Publication of CN108301038A publication Critical patent/CN108301038A/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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • 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

Abstract

The invention discloses a kind of drawing method of pulling silicon single crystal stove and growing single-crystal silicon, a kind of pulling silicon single crystal stove, including:Furnace chamber, tubular reactor for heating, crucible, pulling silicon single crystal mechanism, the heater for being heated to crucible are provided in furnace chamber, gas silicon source pyrolysis in tubular reactor generates silica flour, silica flour or silica flour are melted into molten silicon and enter in crucible, pulling silicon single crystal mechanism is set to above crucible, and pulling silicon single crystal mechanism is for lifting seed crystal by the molten silicon pulling growth monocrystalline silicon in crucible.Present invention omits the production stages of solid silicon material, energy consumption can be reduced, production can also be saved and handle the huge investment needed for solid silicon material, pollution problem can be introduced to avoid solid silicon material, to ensure the purity of the monocrystalline silicon generated, relative to the continuous feeding of solid silicon material, gas silicon source thermal decomposition supplement melting silicon material more can be realized easily, and the speed for supplementing melting silicon material can accomplish to be accurately controlled.

Description

A kind of drawing method of pulling silicon single crystal stove and growing single-crystal silicon
Technical field
The invention belongs to crystalline silicon growing technology fields, and in particular to a kind of drawing of pulling silicon single crystal stove and growing single-crystal silicon Method processed.
Background technology
Crystalline silicon is the important raw and processed materials of silicon based semiconductor and solar-energy photo-voltaic cell.Crystalline silicon growing method is main at present There are two types of:A kind of method is that solid silicon material is placed in ingot furnace to carry out ingot casting, and the product produced is polysilicon, after slice It is mainly used for the manufacture of solar-energy photo-voltaic cell piece;Another method is that solid silicon material is placed in single crystal growing furnace, is used after fusing The method of lifting grows silicon single crystal rod, and the monocrystalline silicon piece used in semiconductor and solar-energy photo-voltaic cell can be by silicon single crystal rod Manufacture.In addition to above two method, also zone-melting process, this method equally use solid silicon material, are mainly used for growing high-purity Monocrystalline silicon.
Solid silicon material is produced using the methods of Siemens Method, fluidized bed process, free-space Method at present.These methods with Gas silicon source such as trichlorosilane, silane be raw material, will gas silicon source carry out chemical vapor deposition or thermal decomposition after be made silicon rod or The solids silicon material such as silicon particle.
In existing technology, the crystalline silicon from gas silicon source to semiconductor and used in photovoltaic cell need to pass through solid silicon material This intermediate steps.The chemical vapor deposition of gas silicon source or thermal decomposition generally carry out at high temperature, and solid silicon material is utilized to give birth to Production crystalline silicon is generally heated to the fusion temperature of silicon or more from room temperature, therefore considers from energy point of view, from the gas of high temperature The solid silicon material of silicon source to room temperature arrives the high temperature silicon liquid of melting to produce crystalline silicon be uneconomic again.In addition, solid silicon material Production process is inherently complex, and needs special equipment, and such as patent CN200580017512, EP2019084A2, institute is public The free-space Method opened, the fine silica powder generated after the thermal decomposition of gas silicon source is needed can be more as being suitable for by specially treated Brilliant ingot casting or the solid silicon material of crystal growth.
Invention content
The technical problem to be solved by the present invention is to aiming at the above shortcomings existing in the prior art, provide a kind of monocrystalline silicon The drawing method of lifting furnace and growing single-crystal silicon uses gas silicon source for the pulling silicon single crystal stove of raw material growing single-crystal silicon and side The production stage of solid silicon material is omitted in method, on the one hand can reduce energy consumption, on the other hand can save production and processing solid Huge investment needed for silicon material.
Technical solution is to provide a kind of pulling silicon single crystal stove used by solving present invention problem, including:Furnace chamber, institute State be provided in furnace chamber tubular reactor for heating, crucible, pulling silicon single crystal mechanism, for being heated to the crucible Heater, gas silicon source pyrolysis in the tubular reactor generates silica flour, and the silica flour or the silica flour are molten Melt and entered in the crucible as molten silicon, the pulling silicon single crystal mechanism is set to above the crucible, the monocrystalline silicon Shift mechanism is for lifting seed crystal by the molten silicon pulling growth monocrystalline silicon in the crucible.
Preferably, the crucible includes the first sub- crucible and the second sub- crucible, and the first sub- crucible is set to described In second sub- crucible, the opening of the first sub- crucible and the second sub- crucible is arranged in the same direction, the first sub- crucible and institute The second sub- crucible bottom connection is stated, the silica flour or the silica flour are melted into molten silicon and enter one of them sub- crucible Interior, the pulling silicon single crystal mechanism is for lifting seed crystal by the molten silicon pulling growth monocrystalline silicon in another sub- crucible.
Preferably, the silica flour or the silica flour are melted into molten silicon and enter in the described second sub- crucible, institute Pulling silicon single crystal mechanism is stated for lifting seed crystal by the molten silicon pulling growth monocrystalline silicon in the described first sub- crucible.
Preferably, the silica flour or the silica flour are melted into the opening of the sub- crucible of one of molten silicon entrance Height of the height at end less than the open end of another sub- crucible.
Preferably, the outlet of the tubular reactor is located in the molten silicon in the crucible.
Preferably, the tubular reactor is made of one kind in quartz, carbon material, silicon carbide, silicon nitride;
The inside coating of the crucible and/or the tubular reactor is SiC or Si3N4
The present invention also provides a kind of drawing methods using above-mentioned pulling silicon single crystal stove growing single-crystal silicon, including following step Suddenly:
(1) by heat gas silicon source in the tubular reactor in furnace chamber, pyrolysis generates silica flour;
(2) silica flour or silica flour heating are melted into molten silicon and enter in the crucible;
(3) seed crystal is lifted by the molten silicon pulling growth monocrystalline silicon in crucible by pulling silicon single crystal mechanism.
Preferably, the step (3) is discontinuous by the molten silicon in crucible by pulling silicon single crystal mechanism lifting seed crystal Pulling growth monocrystalline silicon.Specifically, can first thermally decompose gas silicon source, then vacuumize, then with inert atmosphere in furnace chamber into Row gas displacement, then carry out pulling growth monocrystalline silicon in inert atmosphere.
Preferably, further include being pre-placed solid silicon material in step (i) crucible before the step (2), lead to It crosses the heater heating and the solid silicon material is melt into molten silicon.
Preferably, the temperature heated in the step (1) is 500~1000 DEG C.
Preferably, the gas silicon source is one kind in monosilane, dichlorosilane, trichlorosilane;Preferably, institute It is monosilane to state gas silicon source.
Preferably, the grain size of the silica flour is 50nm~50 μm.
The present embodiment has following remarkable result:
(1) use gas silicon source that the production stage of solid silicon material is omitted for the device and method of raw material growing single-crystal silicon, On the one hand energy consumption about 2kWh/kg can be reduced, on the other hand can save production and handles the huge investment needed for solid silicon material; The process for preparing monocrystalline silicon compared with the existing technology needs first to prepare the silicon material of high temperature, then is cooled to solid silicon material, reheats At molten silicon, then drawn monocrystalline silicon, the method in the present invention, directly by gas silicon source decompose the high temperature silica flour generated be heated into it is molten Melt silicon and carry out drawn monocrystalline silicon, to save energy consumption;
(2) in such a way that gas silicon source thermally decomposes direct crystal pulling, silicon rod in the prior art can be avoided or silicon particle turns The process that fortune, packaging etc. are easily introduced surface contamination, to ensure the purity of the monocrystalline silicon generated.
(3) gas silicon source thermal decomposition constantly can supplement molten silicon into pulling silicon single crystal stove, relative to solid silicon material Continuous feeding, gas silicon source thermal decomposition supplement melting silicon material more can easily realize, and supplement melting silicon material speed Degree can be accomplished to be accurately controlled.
Description of the drawings
Fig. 1 is the structural schematic diagram of the drawing device of the growing single-crystal silicon in the embodiment of the present invention 1;
Fig. 2 is the structural schematic diagram of the drawing device of the growing single-crystal silicon in the embodiment of the present invention 2.
In figure:1- furnace chambers;2- tubular reactors;21- tube bodies;211- tube body entrances;212- tube bodies export;22- heating members; 3- crucibles;The first sub- crucibles of 31-;The second sub- crucibles of 32-;4- pulling silicon single crystals mechanism;41- lifting pieces;42- heat shieldings.
Specific implementation mode
To make those skilled in the art more fully understand technical scheme of the present invention, below in conjunction with the accompanying drawings and specific embodiment party Present invention is further described in detail for formula.
Embodiment 1
As shown in Figure 1, the present embodiment provides a kind of pulling silicon single crystal stoves, including:Furnace chamber 1, be provided in furnace chamber 1 for plus Tubular reactor 2, crucible 3, pulling silicon single crystal mechanism 4, the heater for being heated to crucible 3 of heat, gas silicon source exist Pyrolysis generates silica flour in tubular reactor 2, and silica flour or silica flour are melted into molten silicon and enter in crucible 3, monocrystalline Silicon shift mechanism 4 is set to 3 top of crucible, and pulling silicon single crystal mechanism 4 is used to lift seed crystal and the molten silicon in crucible 3 is drawn life Long monocrystalline silicon.
Specifically, the tubular reactor 2 in the present embodiment includes tube body 21 and the heating for being heated to tube body 21 Part 22, tube body 21 include tube body entrance 211 and tube body outlet 212, gas silicon source by tube body entrance 211 be passed into tube body 21 by Heat and the reaction in tube body 21, by 212 discharge of tube body outlet.The mode of heating of the heating member 22 of tubular reactor 2 may be used Resistance heating can also use sensing heating.
Preferably, the tubular reactor 2 in the present embodiment is by a kind of system in quartz, carbon material, silicon carbide, silicon nitride At;Make 2 high temperature resistant of tubular reactor.
The inside coating of tubular reactor 2 is high-purity alpha-SiC or high-purity Si3N4, impurity is avoided to enter in silica flour.
It should be noted that the tubular reactor 2 in the present embodiment is made of silicon carbide;
The inside coating of tubular reactor 2 is high-purity Si3N4
The present embodiment also provides a kind of drawing method using above-mentioned pulling silicon single crystal stove growing single-crystal silicon, including following step Suddenly:
(1) by heat gas silicon source in the tubular reactor 2 in furnace chamber 1, pyrolysis generates silica flour;
(2) silica flour or silica flour heating are melted into molten silicon and enter in crucible 3;
(3) seed crystal is lifted by the molten silicon pulling growth monocrystalline silicon in crucible 3 by pulling silicon single crystal mechanism 4.
It should be noted that by the lifting seed crystal of pulling silicon single crystal mechanism 4 that the molten silicon in crucible 3 is non-in the present embodiment Continuous drawing growing single-crystal silicon.Specifically, can first thermally decompose gas silicon source, then vacuumize, then with inert atmosphere to furnace chamber 1 Interior carry out gas displacement, then carry out pulling growth monocrystalline silicon in inert atmosphere.
Gas silicon source thermally decomposes generated silica flour before entering crucible 3, it is preferred that silica flour be heated to 1200 DEG C with On temperature, it is further preferred that silica flour is heated to 1200~1400 DEG C, so that silica flour is heated again fusing on 3 top of crucible When rapidly become liquid and sink to 3 bottom of crucible.Silica flour can also be directly heated to silicon fusing point or more, silica flour is made to become liquid Molten silicon after enter back into crucible 3.
It should be noted that the outlet of the tubular reactor 2 in the present embodiment is located in the molten silicon in crucible 3.Gas Silicon source thermally decomposes to generate silica flour and hydrogen, and silica flour in molten silicon of the hydrogen caused by thermal decomposition in crucible 3 with being bubbled In molten silicon to melt crucible 3.By the way of this bubbling, to reduce the silicon liquid that silica flour or silica flour are melted into Drip the degree escaped with hydrogen.
It should be noted that before step (2) in the present embodiment, further include be pre-placed in step (i) crucible 3 it is solid Body silicon material is heated by heater the solid silicon material being melt into molten silicon.The silica flour that gas silicon source thermally decomposes to generate is with regard to conduct The raw material of supplement, to improve the utilization ratio and formation efficiency of crucible 3.
It should be noted that the middle temperature heated of step (1) in the present embodiment is 500~1000 DEG C.
It should be noted that the gas silicon source in the present embodiment is one in monosilane, dichlorosilane, trichlorosilane Kind.
In view of the thermal decomposition characteristic of different silica sources, the preferred monosilane low using heat decomposition temperature is as gas silicon Source, to reduce heat decomposition temperature, to reduce the requirement to 2 material of tubular reactor.In addition, using monosilane as gas silicon When source, can also reduce the silica flour of generation the inner wall of tubular reactor 2 deposition.
It should be noted that the grain size of the silica flour in the present embodiment is 50nm~50 μm.
Specifically, the present embodiment uses monosilane as gas silicon source.In furnace chamber 1, tubular reactor 2 is heated to When monosilane enters in tubular reactor 2 pyrolysis occurs for 800 DEG C of temperature, generates 50 nanometers to 50 microns Fine silica powder and hydrogen.The fine silica powder thermally decomposed to generate is further heated to 1300 DEG C by tubular reactor 2, on the one hand ensures first silicon On the other hand fine silica powder is preheated to the temperature close to fusing by the complete decomposition of alkane.Crucible 3 is heated to thin silicon by heater in advance It more than powder fusion temperature, when fine silica powder reaches the top of crucible 3, is molten into silicon liquid and drips and sink in crucible 3.With crucible 3 The outlet of the increase of middle molten silicon liquid level, tubular reactor 2 can be immersed in the molten silicon in crucible 3, at this point, thermally decompose to generate Hydrogen is discharged in a manner of being bubbled, and the fine silica powder escaped with hydrogen or silicon liquid drop can be greatly decreased.When the molten silicon in crucible 3 When liquid level reaches the first preset height, stopping is passed through monosilane, is then vacuumized to furnace chamber 1, being finally passed through argon gas makes Argon gas atmosphere is full of in furnace chamber 1.Crucible 3 is rotated, and seed crystal is rotated by pulling silicon single crystal mechanism 4, starts the vertical pulling of monocrystalline silicon It generates silicon single crystal rod and is constantly passed through argon gas when silicon single crystal rod is grown.When the liquid level of the molten silicon in crucible 3 is reduced to second When preset height, stop the growth of silicon single crystal rod, then passes to monosilane supplement silicon material.This method is discontinuous pulling growth The semicontinuous drawing of silicon single crystal rod may be implemented in monocrystalline silicon.
It is pre-placed solid silicon material in crucible 3, after solid silicon material is completely melt, carries out the lifting life of silicon single crystal rod It is long.When the liquid level deficiency of the molten silicon in crucible 3, by the thermal decomposition of gas silicon source to 3 feed supplement of crucible, monocrystalline may be implemented The semicontinuous drawing of silicon rod.
The present embodiment has following remarkable result:
(1) use gas silicon source that the production stage of solid silicon material is omitted for the device and method of raw material growing single-crystal silicon, On the one hand energy consumption about 2kWh/kg can be reduced, on the other hand can save production and handles the huge investment needed for solid silicon material; The process for preparing monocrystalline silicon compared with the existing technology needs first to prepare the silicon material of high temperature, then is cooled to solid silicon material, reheats At molten silicon, then drawn monocrystalline silicon, the method in the present invention, directly by gas silicon source decompose the high temperature silica flour generated be heated into it is molten Melt silicon and carry out drawn monocrystalline silicon, to which energy consumption be greatly saved;
(2) in such a way that gas silicon source thermally decomposes direct crystal pulling, silicon rod in the prior art can be avoided or silicon particle turns The process that fortune, packaging etc. are easily introduced surface contamination, to ensure the purity of the monocrystalline silicon generated.
(3) gas silicon source thermal decomposition constantly can supplement molten silicon into pulling silicon single crystal stove, relative to solid silicon material Continuous feeding, gas silicon source thermal decomposition supplement melting silicon material more can easily realize, and supplement melting silicon material speed Degree can be accomplished to be accurately controlled.
Embodiment 2
As shown in Fig. 2, the drawing device of growing single-crystal silicon in the present embodiment in embodiment 1 difference lies in:This reality The crucible 3 applied in example includes the first sub- crucible 31 and the second sub- crucible 32, and the first sub- crucible 31 is set in the second sub- crucible 32, The opening of first sub- crucible 31 and the second sub- crucible 32 is arranged in the same direction, and the first sub- crucible 31 is connected to 32 bottom of the second sub- crucible, Silica flour or silica flour are melted into molten silicon and enter in one of them sub- crucible 3, and pulling silicon single crystal mechanism 4 is for lifting seed crystal By the molten silicon pulling growth monocrystalline silicon in another sub- crucible 3.Due to the first sub- crucible 31 and 32 bottom of the second sub- crucible Connection, so the molten silicon in the first sub- crucible 31 and the second sub- crucible 32 can mutually circulate, and the first sub- crucible 31 and the The liquid level of molten silicon in two sub- crucibles 32 flushes.Specifically, the bottom of the first sub- crucible 31 opens up hole, which makes First sub- crucible 31 is connected to 32 bottom of the second sub- crucible.
It should be noted that the silica flour or silica flour in the present embodiment, which are melted into molten silicon, enters the second sub- crucible 32 Interior, pulling silicon single crystal mechanism 4 is for lifting seed crystal by the molten silicon pulling growth monocrystalline silicon in the first sub- crucible 31.
Preferably, silica flour or silica flour are melted into the height of one of the molten silicon entrance open end of sub- crucible 3 Height of the degree less than the open end of another sub- crucible 3.Specifically, the silica flour or silica flour in the present embodiment be melted into it is molten Melt silicon to enter in the second sub- crucible 32, the height of the open end of the second sub- crucible 32 is less than the open end of the first sub- crucible 31 Highly.
Tubular reactor 2 in the present embodiment is made of quartz;
The inside coating of tubular reactor 2 is high-purity alpha-SiC.
The present embodiment also provides a kind of drawing method of the drawing device growing single-crystal silicon using above-mentioned growing single-crystal silicon, packet Include following steps:
(1) by heat gas silicon source in the tubular reactor 2 in furnace chamber 1, pyrolysis generates silica flour;
(2) silica flour or silica flour heating are melted into molten silicon and enter in the second sub- crucible 32, the second sub- crucible 32 with First sub- crucible, 31 bottom is connected to, and silicon liquid drops in formation molten silicon in the second sub- crucible 32 and can gradually flow into the first sub- crucible 31 In, and the first sub- crucible 31 is flushed with the liquid level of the second sub- crucible 32;
(3) seed crystal is lifted by the molten silicon pulling growth monocrystalline silicon in the first sub- crucible 31 by pulling silicon single crystal mechanism 4.
Gas silicon source in the present embodiment is monosilane.
Specifically, the present embodiment uses monosilane as gas silicon source.In furnace chamber 1, tubular reactor 2 is heated to When monosilane enters in tubular reactor 2 pyrolysis occurs for 800 DEG C of temperature, generates 50 nanometers to 50 microns Fine silica powder and hydrogen.The fine silica powder thermally decomposed to generate is further heated to 1300 DEG C by tubular reactor 2, on the one hand ensures first silicon On the other hand fine silica powder is preheated to the temperature close to fusing by the complete decomposition of alkane.Crucible 3 is heated to 1420 in advance by heater DEG C or more, tubular reactor 2 reaches the second sub- earthenware in the top of the second sub- crucible 32, when fine silica powder is discharged by tubular reactor 2 When the top of crucible 32, it is molten into silicon liquid and drips and fall into the second sub- crucible 32, the second sub- crucible 32 and 31 bottom of the first sub- crucible Connection, silicon liquid drops in formation molten silicon in the second sub- crucible 32 and can gradually flow into the first sub- crucible 31, and the first sub- crucible 31 flush with the liquid level of the second sub- crucible 32.With the increase of molten silicon liquid level in the second sub- crucible 32, tubular reactor 2 goes out Mouth can immerse in the molten silicon in the second sub- crucible 32, at this point, the hydrogen thermally decomposed to generate is discharged in a manner of being bubbled, it can substantially It reduces the fine silica powder escaped with hydrogen or silicon liquid is dripped.
Specifically, pulling silicon single crystal mechanism 4 includes lifting piece 41 and the heat shielding 42 being connect with lifting piece 41, lifting piece 41 is used In lifting seed crystal, heat shielding 42 is coated on outside seed crystal and there are gaps between seed crystal, and heat shielding 42 is for heating.
When the silicon liquid in the first crucible 3 reaches preset height, seed of single crystal silicon is deep into silicon liquid, is then rotated Crucible 3, and seed crystal is rotated by pulling silicon single crystal mechanism 4, the vertical pulling for starting monocrystalline silicon generates silicon single crystal rod, silicon single crystal rod growth When, argon gas is passed through from silicon single crystal rod top, and reaches 3 top of crucible, last argon gas by the gap between heat shielding 42 and seed crystal Generated hydrogen is thermally decomposed with monosilane to be discharged from the offgas outlet of pulling silicon single crystal stove together.In the present embodiment, it is located at interior The height of the first sub- crucible 31 opening of layer, which is higher than, is located at the height that the second sub- crucible 32 of outer layer is open, on the first sub- crucible 31 The argon gas in portion is spread by 31 outward opening of the first sub- crucible, can prevent unfused fine silica powder or gas to a certain extent The silicon liquid drop of middle floating enters in the first sub- crucible 31 of internal layer, to substantially weaken unfused fine silica powder or gas The silicon liquid of middle floating drips the influence to monocrystalline silicon growing.
In 32 or the first sub- crucible 31 of the second sub- crucible, it is pre-placed solid silicon material, after solid silicon material is completely melt, Carry out the pulling growth of silicon single crystal rod.When the liquid level deficiency of the molten silicon in crucible 3, by the thermal decomposition of gas silicon source to Two sub- crucibles, 32 feed supplement.This method is discontinuous pulling growth monocrystalline silicon, and the semicontinuous drawing of silicon single crystal rod may be implemented.
Embodiment 3
The present embodiment also provides a kind of drawing of the drawing device growing single-crystal silicon using the growing single-crystal silicon in embodiment 1 Method, method in the present embodiment and the method in embodiment 1 difference lies in:
Gas silicon source in the present embodiment is trichlorosilane.
Embodiment 4
The present embodiment also provides a kind of drawing of the drawing device growing single-crystal silicon using the growing single-crystal silicon in embodiment 1 Method, method in the present embodiment and the method in embodiment 1 difference lies in:
Gas silicon source in the present embodiment is dichlorosilane.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses Mode, however the present invention is not limited thereto.For those skilled in the art, in the essence for not departing from the present invention In the case of refreshing and essence, various changes and modifications can be made therein, these variations and modifications are also considered as protection scope of the present invention.

Claims (12)

1. a kind of pulling silicon single crystal stove, which is characterized in that including:It is anti-to be provided with tubular type for heating in the furnace chamber for furnace chamber Answer device, crucible, pulling silicon single crystal mechanism, the heater for being heated to the crucible, gas silicon source anti-in the tubular type Pyrolysis in device is answered to generate silica flour, the silica flour or the silica flour are melted into molten silicon and enter in the crucible, The pulling silicon single crystal mechanism is set to above the crucible, and the pulling silicon single crystal mechanism is for lifting seed crystal by the crucible Interior molten silicon pulling growth monocrystalline silicon.
2. pulling silicon single crystal stove according to claim 1, which is characterized in that the crucible includes the first sub- crucible and second Sub- crucible, the first sub- crucible are set in the described second sub- crucible, the first sub- crucible and the second sub- crucible Setting, the first sub- crucible are connected to opening with the described second sub- crucible bottom in the same direction, the silica flour or silica flour melting It is entered in one of them sub- crucible as molten silicon, the pulling silicon single crystal mechanism is for lifting seed crystal by another sub- earthenware Molten silicon pulling growth monocrystalline silicon in crucible.
3. pulling silicon single crystal stove according to claim 2, which is characterized in that the silica flour or the silica flour are melted into Molten silicon enters in the described second sub- crucible, and the pulling silicon single crystal mechanism will be in the described first sub- crucible for lifting seed crystal Molten silicon pulling growth monocrystalline silicon.
4. pulling silicon single crystal stove according to claim 2 or 3, which is characterized in that the silica flour or silica flour melting As molten silicon enter one of sub- crucible open end height less than another sub- crucible open end height.
5. the pulling silicon single crystal stove according to claims 1 to 3 any one, which is characterized in that the tubular reactor Outlet is located in the molten silicon in the crucible.
6. the pulling silicon single crystal stove according to claims 1 to 3 any one, which is characterized in that the tubular reactor by One kind in quartz, carbon material, silicon carbide, silicon nitride is made;
The inside coating of the tubular reactor is SiC or Si3N4
7. a kind of drawing method using pulling silicon single crystal stove growing single-crystal silicon described in claim 1~6 any one, feature It is, includes the following steps:
(1) by heat gas silicon source in the tubular reactor in the furnace chamber, pyrolysis generates silica flour;
(2) silica flour or silica flour heating are melted into molten silicon and enter in the crucible;
(3) seed crystal is lifted by the molten silicon pulling growth monocrystalline silicon in the crucible by pulling silicon single crystal mechanism.
8. the drawing method of growing single-crystal silicon according to claim 7, which is characterized in that before the step (2), also wrap Include in step (i) crucible and be pre-placed solid silicon material, heated by the heater solid silicon material is melt into it is molten Melt silicon.
9. the drawing method of growing single-crystal silicon according to claim 7, which is characterized in that heated in the step (1) Temperature is 500~1000 DEG C.
10. the drawing method of growing single-crystal silicon according to claim 7, which is characterized in that the step (3) passes through described Pulling silicon single crystal mechanism lifts seed crystal by the discontinuous pulling growth monocrystalline silicon of molten silicon in the crucible.
11. the drawing method of growing single-crystal silicon according to claim 7, which is characterized in that the gas silicon source is first silicon One kind in alkane, dichlorosilane, trichlorosilane;Preferably, the gas silicon source is monosilane.
12. the drawing method of the growing single-crystal silicon according to claim 7~11 any one, which is characterized in that the silicon The grain size of powder is 50nm~50 μm.
CN201710028070.1A 2017-01-12 2017-01-12 A kind of drawing method of pulling silicon single crystal stove and growing single-crystal silicon Pending CN108301038A (en)

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN110184646A (en) * 2019-07-15 2019-08-30 乐山新天源太阳能科技有限公司 The preparation facilities of major diameter high-efficiency N-type monocrystalline silicon
CN110541190A (en) * 2019-10-16 2019-12-06 武汉先见科技有限公司 method for preparing silicon single crystal rod
CN111962140A (en) * 2020-08-28 2020-11-20 晶科绿能(上海)管理有限公司 Continuous crystal pulling apparatus and method for continuously pulling crystal rod

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