CN106400108A - Technique for casting high-efficiency polycrystalline silicon ingot and silicon wafer by frequent nucleation - Google Patents
Technique for casting high-efficiency polycrystalline silicon ingot and silicon wafer by frequent nucleation Download PDFInfo
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- CN106400108A CN106400108A CN201610846586.2A CN201610846586A CN106400108A CN 106400108 A CN106400108 A CN 106400108A CN 201610846586 A CN201610846586 A CN 201610846586A CN 106400108 A CN106400108 A CN 106400108A
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- ingot
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- silicon ingot
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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
-
- 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
Abstract
The invention relates to a technique for casting a high-efficiency polycrystalline silicon ingot and silicon wafer by frequent nucleation. The technique comprises seven steps of preparation of a demoulding layer, material charging, dust collection of a polycrystalline silicon ingot furnace, material feeding, preparation of crystal growing, crystal growing and furnace discharging. The frequent nucleation casting high-efficiency polycrystalline silicon ingot and silicon wafer technique has the advantages that by improving the existing polycrystalline silicon ingot furnace, a vacuum material supplementing system is arranged, and an auxiliary coolant is fed to quickly lower the temperature; the auxiliary coolant can be quickly melted, and after the nucleation is formed, and a crystal growth phase is quickly returned to, so as to quickly switch the nucleation and the crystal growing; the interference between the vacuum material supplementing system and a heat field in the furnace is avoided; by utilizing the existing polycrystalline silicon ingot furnace, the frequent nucleation is formed, and the photo-electric conversion efficiency of the produced silicon ingot reaches 19.5% or more, the efficiency distribution centralizing degree of the silicon wafer is increased by 40%, and the purpose of improving integral conversion efficiency and efficiency centralizing degree is realized.
Description
Technical field
This patent is related to solar cell polysilicon ingot casting field, and particularly a kind of multiple forming core casts efficient polycrystalline silicon ingot
And silicon chip technology.
Background technology
The silicon ingot that now production technology produces, mostly one time forming core, a vice-minister are brilliant, and therefore have silicon ingot bottom dislocation more
Low, efficiency high, top dislocation gradually rises, the shortcoming of efficiency step-down, leads to silicon ingot and the silicon chip concentration degree dispersion producing, and then
Lead to photoelectric transformation efficiency low, quality is low.
Content of the invention
For the problems referred to above, the invention discloses a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology.
For solving above technical problem, the technical scheme that the present invention provides is:
A kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology are it is characterised in that include step in detail below：
A, preparation release layer：Prepare silicon nitride powder, stir, preheat ingot casting crucible, and by the silicon nitride powder stirring
Material is sprayed on the inwall of ingot casting crucible, subsequently heats ingot casting crucible again, the silicon nitride powder on ingot casting crucible inwall is burnt
Knot, forms release layer；
B, charging：Silicon raw material is filled in ingot casting crucible；
C, polycrystal silicon ingot stove dust suction：During ingot casting, a large amount of oxides can be adsorbed in the burner hearth of polycrystal silicon ingot stove, using dust suction
Most of oxide in burner hearth absorbed by device；
D, feed intake：Using conveying equipments such as drivings, the ingot casting crucible feeding in step B is put in polycrystal silicon ingot stove；
E, heating, melting：Start polycrystal silicon ingot stove, ingot casting crucible is heated, silicon raw material in ingot casting crucible is melted, formed
Silicon solution, in stove, in temperature n1, described n1 is 1530 DEG C ~ 1560 DEG C to master control temperature control；
F, long brilliant preparation：Melt completely and finish etc. silicon raw material, be incubated 10 ~ 30 minutes；
G, long crystalline substance：With the long brilliant height of budget as H, actual (tube) length is brilliant to be h1, and crystal growing stage is divided into three ranks：
1st, the first crystal growing stage：0 ＜ h1 ＜ 0.4*H, the DS cooling starting polycrystal silicon ingot furnace interior is fast, ingot casting crucible is carried out cold
But, carry out long crystalline substance, silicon solution temperature controls in temperature n2；
2nd, the second crystal growing stage：H1=0.4*H ~ 0.5*H, by the vacuum feeding-system being arranged on polycrystal silicon ingot stove, to ingot casting
By-carriage supplement heat rejecter agent in crucible, carries out fast cooling to silicon solution, carries out a forming core optimization, and subsequent silicon solution temperature carries
Rise, continue long brilliant, now silicon solution temperature controls in temperature n3；
3rd, the 3rd crystal growing stage：H1=0.65*H ~ 0.7*H, by the vacuum feeding-system being arranged on polycrystal silicon ingot stove, Xiang Zhu
By-carriage supplement heat rejecter agent in ingot crucible, carries out fast cooling to silicon solution, carries out second nucleation optimization, continues thereafter with long crystalline substance, directly
Complete to long crystalline substance, silicon solution temperature controls in temperature n4；
H, come out of the stove：Close polycrystal silicon ingot stove, wait polycrystal silicon ingot furnace interior temperature to reduce, subsequent pressure release, finally with the conveying such as driving
Ingot casting crucible is taken out by equipment, and ingot casting is come out of the stove.
Above-mentioned a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology, wherein, described n2 is 1415 DEG C ~ 1420
DEG C, described n3 is 1410 DEG C ~ 1415 DEG C, and described n4 is 1405 DEG C ~ 1412 DEG C.
Above-mentioned a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology, wherein, described vacuum feeding-system bag
Include vaccum-pumping equipment, charging chamber, quartzy mozzle and control valve, described vaccum-pumping equipment, quartzy mozzle are all joined with charging chamber
Logical, vaccum-pumping equipment is connected to charging chamber upper end, and quartzy mozzle is connected to charging chamber lower end, and control valve is arranged at quartzy water conservancy diversion
Guan Shang, controls quartzy mozzle conveying supplement heat rejecter agent, in the lower end insertion polycrystal silicon ingot stove of quartzy mozzle, positioned at ingot casting earthenware
The top of crucible.
Above-mentioned a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology, wherein, described supplement heat rejecter agent is REC
The primary pure silicon polycrystal of fritter below the 4021 serial particle silicon materials producing or size 10MM.
Above-mentioned a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology, wherein, the sintering temperature in step A is
800℃~1100℃.
Above-mentioned a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology, wherein, described in the second crystal growing stage
In the 3rd crystal growing stage, the amount of the supplement heat rejecter agent added every time is identical, adds supplement heat rejecter agent and forming core raw material every time
Weight is than for 0.11 ~ 0.12%.
Beneficial effects of the present invention are：
A kind of multiple forming core casting efficient polycrystalline silicon ingot of the present invention and silicon chip technology, including preparation release layer, charging, polysilicon
Ingot stove dust suction, feed intake, long brilliant prepare, long brilliant and seven steps such as come out of the stove, improve existing polycrystalline ingot furnace, vacuum feed supplement system be set
System, by throwing in supplement heat rejecter agent, realizes fast cooling, simultaneously because supplement heat rejecter agent can be melted rapidly, after the completion of forming core again
Crystal growing stage can be quickly returning to, to realize forming core and long brilliant to be switched fast, meanwhile, the vacuum feeding-system of the present invention and stove again
Interior thermal field does not interfere.
In sum, the present invention utilizes existing polycrystalline ingot furnace, realizes multiple forming core, makes the silicon ingot opto-electronic conversion of production
Efficiency reaches more than 19.5%, and silicon chip efficiency distribution concentration degree improves 40%, thus realizing improving overall transformation efficiency and improving effect
The purpose of rate concentration degree.
Brief description
Fig. 1 vacuum feeding-system schematic diagram.
Specific embodiment
Embodiment one
A kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology are it is characterised in that include step in detail below：
A, preparation release layer：Prepare silicon nitride powder, stir, preheat ingot casting crucible, and by the silicon nitride powder stirring
Material is sprayed on the inwall of ingot casting crucible, subsequently heats ingot casting crucible again, the silicon nitride powder on ingot casting crucible inwall is burnt
Knot, forms release layer；
B, charging：Silicon raw material is filled in ingot casting crucible；
C, polycrystal silicon ingot stove dust suction：During ingot casting, a large amount of oxides can be adsorbed in the burner hearth of polycrystal silicon ingot stove, using dust suction
Most of oxide in burner hearth absorbed by device；
D, feed intake：Using conveying equipments such as drivings, the ingot casting crucible feeding in step B is put in polycrystal silicon ingot stove；
E, heating, melting：Start polycrystal silicon ingot stove, ingot casting crucible is heated, forming core raw material in ingot casting crucible is melted, shape
Become silicon solution, in temperature n1, described n1 is 1550 DEG C to the master control temperature control in stove；
F, long brilliant preparation：Melt completely and finish etc. silicon raw material, be incubated 25 minutes；
G, long crystalline substance：With the long brilliant height of budget as H, actual (tube) length is brilliant to be h1, and crystal growing stage is divided into three ranks：
1st, the first crystal growing stage：0 ＜ h1 ＜ 0.4*H, the DS cooling starting polycrystal silicon ingot furnace interior is fast, ingot casting crucible is carried out cold
But, carry out long crystalline substance, silicon solution temperature controls in temperature n2；
2nd, the second crystal growing stage：H1=0.45*H, by the vacuum feeding-system being arranged on polycrystal silicon ingot stove, to ingot casting crucible
Interior by-carriage supplement heat rejecter agent, carries out fast cooling to silicon solution, carries out a forming core optimization, subsequent silicon solution temperature lifting, continues
Continuous long brilliant, now silicon solution temperature controls in temperature n3；
3rd, the 3rd crystal growing stage：H1=0.67*H, by the vacuum feeding-system being arranged on polycrystal silicon ingot stove, to ingot casting crucible
Interior by-carriage supplement heat rejecter agent, carries out fast cooling to silicon solution, carries out second nucleation optimization, continues thereafter with long crystalline substance, until long brilliant
Complete, silicon solution temperature controls in temperature n4；
H, come out of the stove：Close polycrystal silicon ingot stove, wait polycrystal silicon ingot furnace interior temperature to reduce, subsequent pressure release, finally with the conveying such as driving
Ingot casting crucible is taken out by equipment, and ingot casting is come out of the stove.
Above-mentioned a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology, wherein, described n2 is 1415 DEG C,
Described n3 is 1410 DEG C, and described n4 is 1405 DEG C.
Above-mentioned a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology, wherein, described supplement heat rejecter agent is REC
The primary pure silicon polycrystal of fritter below the 4021 serial particle silicon materials producing or size 10MM.
Above-mentioned a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology, wherein, the sintering temperature in step A is
1000℃.
Above-mentioned a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology, wherein, described in the second crystal growing stage
In the 3rd crystal growing stage, the amount of the supplement heat rejecter agent added every time is identical, adds supplement heat rejecter agent and forming core raw material every time
Weight is than for 0.117%.
Embodiment two
A kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology are it is characterised in that include step in detail below：
A, preparation release layer：Prepare silicon nitride powder, stir, preheat ingot casting crucible, and by the silicon nitride powder stirring
Material is sprayed on the inwall of ingot casting crucible, subsequently heats ingot casting crucible again, the silicon nitride powder on ingot casting crucible inwall is burnt
Knot, forms release layer；
B, charging：Silicon raw material is filled in ingot casting crucible；
C, polycrystal silicon ingot stove dust suction：During ingot casting, a large amount of oxides can be adsorbed in the burner hearth of polycrystal silicon ingot stove, using dust suction
Most of oxide in burner hearth absorbed by device；
D, feed intake：Using conveying equipments such as drivings, the ingot casting crucible feeding in step B is put in polycrystal silicon ingot stove；
E, heating, melting：Start polycrystal silicon ingot stove, ingot casting crucible is heated, forming core raw material in ingot casting crucible is melted, shape
Become silicon solution, in stove, in temperature n1, described n1 is 1545 DEG C to master control temperature control；
F, long brilliant preparation：Melt completely and finish etc. silicon raw material, be incubated 25 minutes；
G, long crystalline substance：With the long brilliant height of budget as H, actual (tube) length is brilliant to be h1, and crystal growing stage is divided into three ranks：
1. the first crystal growing stage：0 ＜ h1 ＜ 0.4*H, the DS cooling starting polycrystal silicon ingot furnace interior is fast, ingot casting crucible is carried out cold
But, carry out long crystalline substance, silicon solution temperature controls in temperature n2；
2. the second crystal growing stage：H1=0.47*H, by the vacuum feeding-system being arranged on polycrystal silicon ingot stove, to ingot casting crucible
Interior by-carriage supplement heat rejecter agent, carries out fast cooling to silicon solution, carries out a forming core optimization, subsequent silicon solution temperature lifting, continues
Continuous long brilliant, now silicon solution temperature controls in temperature n3；
3. the 3rd crystal growing stage：H1=0.69*H, by the vacuum feeding-system being arranged on polycrystal silicon ingot stove, to ingot casting crucible
Interior by-carriage supplement heat rejecter agent, carries out fast cooling to silicon solution, carries out second nucleation optimization, continues thereafter with long crystalline substance, until long brilliant
Complete, silicon solution temperature controls in temperature n4；
H, come out of the stove：Close polycrystal silicon ingot stove, wait polycrystal silicon ingot furnace interior temperature to reduce, subsequent pressure release, finally with the conveying such as driving
Ingot casting crucible is taken out by equipment, and ingot casting is come out of the stove.
Above-mentioned a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology, wherein, described n2 is 1420 DEG C, described
N3 is 1415 DEG C, and described n4 is 1412 DEG C.
Above-mentioned a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology, wherein, described supplement heat rejecter agent is REC
The primary pure silicon polycrystal of fritter below the 4021 serial particle silicon materials producing or size 10MM.
Above-mentioned a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology, wherein, the sintering temperature in step A is
1050℃.
Above-mentioned a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology, wherein, described in the second crystal growing stage
In the 3rd crystal growing stage, the amount of the supplement heat rejecter agent added every time is identical, adds supplement heat rejecter agent and forming core raw material every time
Weight is than for 0.118%.
Embodiment three
As shown in figure 1, above-mentioned a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology, wherein, described vacuum feed supplement
System includes vaccum-pumping equipment 1, charging chamber 2, quartzy mozzle 3 and control valve 4, described vaccum-pumping equipment 1, quartzy mozzle 3
All with charging chamber 2 UNICOM, vaccum-pumping equipment 1 is connected to charging chamber 2 upper end, and quartzy mozzle 3 is connected to charging chamber 2 lower end, control
Valve 4 processed is arranged on quartzy mozzle 3, controls quartzy mozzle 3 conveying supplement heat rejecter agent, the lower end insertion of quartzy mozzle 3
In polycrystal silicon ingot stove 5, positioned at the top of ingot casting crucible 6.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, the change or replacement that can readily occur in,
All should cover within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection domain of claims
It is defined.
Claims (6)
1. a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology are it is characterised in that include step in detail below：
A, preparation protective layer：Prepare silicon nitride powder, stir, preheat ingot casting crucible, and by the silicon nitride powder stirring
Material is sprayed on the inwall of ingot casting crucible, subsequently heats ingot casting crucible again, the silicon nitride powder on ingot casting crucible inwall is burnt
Knot, forms protective layer；
B, charging：Forming core raw material is filled in ingot casting crucible；
C, cleaning polycrystal silicon ingot stove：During ingot casting, a large amount of oxides in the burner hearth of polycrystal silicon ingot stove, can be adsorbed, first by
Most of oxide in burner hearth absorbed by dust catcher, subsequently sprays absolute alcohol on a small quantity, and with wiping, removes the residue in burner hearth
Oxide；
D, feed intake：Using conveying equipments such as drivings, the ingot casting crucible feeding in step B is put in polycrystal silicon ingot stove；
E, heating, melting：Start polycrystal silicon ingot stove, ingot casting crucible is heated, forming core raw material in ingot casting crucible is melted, shape
Become silicon solution, silicon solution temperature controls in temperature n1, described n1 is 1530 DEG C ~ 1560 DEG C；
F, long brilliant preparation：Melt completely and finish etc. silicon raw material, be incubated 10 ~ 30 minutes；
G, long crystalline substance：With the long brilliant height of budget as H, actual (tube) length is brilliant to be h1, and crystal growing stage is divided into three ranks：
1st, the first crystal growing stage：0 ＜ h1 ＜ 0.4*H, the DS cooling starting polycrystal silicon ingot furnace interior is fast, ingot casting crucible is carried out cold
But, carry out long crystalline substance, silicon solution temperature controls in temperature n2；
2nd, the second crystal growing stage：H1=0.4*H ~ 0.5*H, by the vacuum feeding-system being arranged on polycrystal silicon ingot stove, to ingot casting
By-carriage supplement heat rejecter agent in crucible, carries out fast cooling to silicon solution, carries out a forming core optimization, and subsequent silicon solution temperature carries
Rise, continue long brilliant, now silicon solution temperature controls in temperature n3；
3rd, the 3rd crystal growing stage：H1=0.65*H ~ 0.7*H, by the vacuum feeding-system being arranged on polycrystal silicon ingot stove, Xiang Zhu
By-carriage supplement heat rejecter agent in ingot crucible, carries out fast cooling to silicon solution, carries out second nucleation optimization, continues thereafter with long crystalline substance, directly
Complete to long crystalline substance, silicon solution temperature controls in temperature n4；
H, come out of the stove：Close polycrystal silicon ingot stove, wait polycrystal silicon ingot furnace interior temperature to reduce, subsequent pressure release, finally with the conveying such as driving
Ingot casting crucible is taken out by equipment, and ingot casting is come out of the stove.
2. as claimed in claim 1 a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology it is characterised in that described
N2 is 1415 DEG C ~ 1420 DEG C, and described n3 is 1410 DEG C ~ 1415 DEG C, and described n4 is 1405 DEG C ~ 1412 DEG C.
3. as claimed in claim 1 a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology it is characterised in that described
Vacuum feeding-system includes vaccum-pumping equipment, charging chamber, quartzy mozzle and control valve, described vaccum-pumping equipment, quartzy water conservancy diversion
Guan Junyu charging chamber UNICOM, vaccum-pumping equipment is connected to charging chamber upper end, and quartzy mozzle is connected to charging chamber lower end, control valve
It is arranged on quartzy mozzle, control quartzy mozzle conveying supplement heat rejecter agent, the lower end insertion polycrystal silicon ingot of quartzy mozzle
In stove, positioned at the top of ingot casting crucible.
4. as claimed in claim 1 a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology it is characterised in that described
The primary pure silicon polycrystal of fritter below 4021 serial particle silicon materials that supplement heat rejecter agent produces for REC or size 10MM.
5. as claimed in claim 1 a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology it is characterised in that described
Sintering temperature in step A is 800 DEG C ~ 1100 DEG C.
6. as claimed in claim 1 a kind of multiple forming core casting efficient polycrystalline silicon ingot and silicon chip technology it is characterised in that described
In the second crystal growing stage and the 3rd crystal growing stage, the amount of the supplement heat rejecter agent added every time is identical, adds supplement heat rejecter every time
The weight of agent and forming core raw material is than for 0.11 ~ 0.12%.
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| CN101428273A (en) * | 2008-12-05 | 2009-05-13 | 江阴海润太阳能电力有限公司 | Silicon nitride spray finishing method for quartz crucible for polysilicon solar battery casting ingot |
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Application publication date: 20170215 |