CN106319622A - Multi-stage electrical resistivity control efficient polycrystalline silicon chip technology - Google Patents

Multi-stage electrical resistivity control efficient polycrystalline silicon chip technology Download PDF

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Publication number
CN106319622A
CN106319622A CN201610846522.2A CN201610846522A CN106319622A CN 106319622 A CN106319622 A CN 106319622A CN 201610846522 A CN201610846522 A CN 201610846522A CN 106319622 A CN106319622 A CN 106319622A
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China
Prior art keywords
ingot casting
ingot
stove
resistivity
polycrystalline silicon
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CN201610846522.2A
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Chinese (zh)
Inventor
孟涛
路景刚
王禄宝
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Jiangsu Meike Silicon Energy Co Ltd
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Jiangsu Meike Silicon Energy Co Ltd
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Priority to CN201610846522.2A priority Critical patent/CN106319622A/en
Publication of CN106319622A publication Critical patent/CN106319622A/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

Abstract

The invention provides a multi-stage electrical resistivity control efficient polycrystalline silicon chip technology, which comprises seven steps of release layer preparation, charging, polycrystalline silicon ingot furnace dust removal, material feeding, crystal growth preparation, crystal growth, furnace discharging and the like. The existing polycrystalline silicon ingot furnace is improved; a vacuum material supplementing system is installed; dopants are fed for performing co-doping; the fast regulation and optimization of the electrical resistivity is realized; the resistance uniformity is further realized; meanwhile, the defect of obvious light decay is avoided; in addition, the vacuum material supplementing system of the multi-stage electrical resistivity control efficient polycrystalline silicon chip technology does not generate interference with a heat field in the furnace.

Description

A kind of multistage resistivity controls high-efficiency polycrystalline silicon chip technology
Technical field
This patent relates to solar cell polysilicon ingot casting field, and particularly a kind of multistage resistivity controls high-efficiency polycrystalline Silicon chip technology.
Background technology
The silicon ingot that now production technology produces, its resistance is for p-type mostly, mostly mixes boron, but boron-oxygen is combined Knowing from experience the obvious optical attenuation causing battery efficiency, especially in the initial light induced attenuation stage, the output of photovoltaic module is just In initial several days begun to use, decline by a relatively large margin occurring, its main cause is exactly the boron in p-type (boron-doping) crystal silicon chip Oxygen complex reduces minority carrier life time, and the p-type polysilicon ingot mixing gallium has that electrical resistivity range is wide and yield rate is the most high Shortcoming.
Summary of the invention
For the problems referred to above, the invention discloses a kind of multistage resistivity and control high-efficiency polycrystalline silicon chip technology.
For solving above technical problem, present invention provide the technical scheme that
A kind of multistage resistivity controls high-efficiency polycrystalline silicon chip technology, it is characterised in that include step in detail below:
A, preparation release layer: prepare silicon nitride powder, stir, preheat ingot casting crucible, and the silicon nitride powder that will stir Material is sprayed on the inwall of ingot casting crucible, the most again heats ingot casting crucible, is burnt by the silicon nitride powder on ingot casting crucible inwall Knot, forms release layer;
B, charging: ingot casting raw material is filled in ingot casting crucible;
C, polycrystal silicon ingot stove dust suction: during ingot casting, can adsorb a large amount of oxide in the burner hearth of polycrystal silicon ingot stove, uses dust suction Major part oxide in burner hearth absorbed by device;
D, feed intake: use the conveying equipments such as driving that the ingot casting crucible fed in step B is put into polycrystal silicon ingot stove;
E, heating, melting: start polycrystal silicon ingot stove, ingot casting crucible is heated, ingot casting raw material in ingot casting crucible is melted, shape Becoming silicon solution, in stove, main control temperature controls in temperature n1, and described n1 is 1530 DEG C ~ 1560 DEG C;
F, long crystalline substance prepare: silicon material melts completely, is incubated 10 ~ 30 minutes;
G, long crystalline substance: with the long brilliant height of budget as H, actual (tube) length crystalline substance is h1, crystal growing stage is divided into three rank:
1, the first crystal growing stage: 0 < h1 < 0.6*H, the DS cooling starting polycrystal silicon ingot furnace interior is fast, carries out cold to ingot casting crucible But, carrying out long crystalline substance, silicon solution temperature controls in temperature n2;
2, the second crystal growing stage: h1=0.60*H ~ 0.63*H, by the vacuum feeding-system being arranged on polycrystal silicon ingot stove, Xiang Zhu By-carriage adulterant in ingot crucible, regulates resistivity, carries out a resistance optimization, and now silicon solution temperature controls in temperature n3;
3, the 3rd crystal growing stage: h1=0.80*H ~ 0.83*H, by the vacuum feeding-system being arranged on polycrystal silicon ingot stove, Xiang Zhu By-carriage adulterant in ingot crucible, regulates resistivity, carries out secondary resistance optimization, until long crystalline substance completes, silicon solution temperature controls Temperature n4;
H, come out of the stove: close polycrystal silicon ingot stove, wait polycrystal silicon ingot furnace interior temperature to reduce, pressure release subsequently, finally carry with driving etc. Ingot casting crucible is taken out by equipment, and ingot casting is come out of the stove.
Above-mentioned a kind of multistage resistivity controls high-efficiency polycrystalline silicon chip technology, and wherein, described ingot casting raw material is contained within p-type Gallium elemental body, described p-type gallium elemental body is 0.01 ~ 0.1:1(g/Kg with the weight ratio of ingot casting raw material).
Above-mentioned a kind of multistage resistivity controls high-efficiency polycrystalline silicon chip technology, and wherein, described n2 is 1410 DEG C ~ 1417 DEG C, described n3 is 1404 DEG C ~ 1412 DEG C, and described n4 is 1400 DEG C ~ 1406 DEG C.
Above-mentioned a kind of multistage resistivity controls high-efficiency polycrystalline silicon chip technology, and wherein, described vacuum feeding-system includes Vaccum-pumping equipment, charging chamber, quartz mozzle and control valve, described vaccum-pumping equipment, quartz mozzle all with the chamber UNICOM that feeds, Vaccum-pumping equipment is connected to the upper end, chamber that feeds, and quartz mozzle is connected to the lower end, chamber that feeds, and control valve is arranged at quartz mozzle On, controlling quartz mozzle conveying adulterant, the lower end of quartz mozzle is inserted in polycrystal silicon ingot stove, is positioned at the upper of ingot casting crucible Side.
Above-mentioned a kind of multistage resistivity controls high-efficiency polycrystalline silicon chip technology, and wherein, described adulterant is that p-doped mother closes Gold bullion, the resistivity of described p-doped foundry alloy silico briquette is 0.002 Ω m ~ 0.007 Ω cm.
Above-mentioned a kind of multistage resistivity controls high-efficiency polycrystalline silicon chip technology, and wherein, the sintering temperature in step A is 800℃~1100℃。
Above-mentioned a kind of multistage resistivity controls high-efficiency polycrystalline silicon chip technology, wherein, described in the second crystal growing stage and In 3rd crystal growing stage, the amount of the adulterant every time added can be different, add the weight ratio of adulterant and ingot casting raw material every time It is 0.1 ~ 1:1(g/Kg).
The invention have the benefit that
A kind of multistage resistivity of the present invention controls high-efficiency polycrystalline silicon chip technology, including preparing release layer, charging, polycrystal silicon ingot Stove dedusting, feed intake, long crystalline substance prepares, long brilliant and seven steps such as come out of the stove, and improves existing polycrystalline ingot furnace, arranges vacuum feed supplement system System, by throwing in adulterant, carries out codope, it is achieved resistivity quickly regulate optimization, and then realize resistance homogenization, simultaneously It also avoid the obvious shortcoming of optical attenuation, and, the vacuum feeding-system of the present invention does not interferes with thermal field in stove.
Accompanying drawing explanation
The resistivity curve figure of Fig. 1 present invention.
What Fig. 2 did not use multi-phase containment mixes gallium resistivity curve.
Fig. 3 vacuum feeding-system schematic diagram.
Detailed description of the invention
Embodiment one
A kind of multistage resistivity controls high-efficiency polycrystalline silicon chip technology, it is characterised in that include step in detail below:
A, preparation release layer: prepare silicon nitride powder, stir, preheat ingot casting crucible, and the silicon nitride powder that will stir Material is sprayed on the inwall of ingot casting crucible, the most again heats ingot casting crucible, is burnt by the silicon nitride powder on ingot casting crucible inwall Knot, forms release layer;
B, charging: ingot casting raw material is filled in ingot casting crucible;
C, polycrystal silicon ingot stove dedusting: during ingot casting, can adsorb a large amount of oxide in the burner hearth of polycrystal silicon ingot stove, uses dust suction Major part oxide in burner hearth absorbed by device;
D, feed intake: use the conveying equipments such as driving that the ingot casting crucible fed in step B is put into polycrystal silicon ingot stove;
E, heating, melting: start polycrystal silicon ingot stove, ingot casting crucible is heated, ingot casting raw material in ingot casting crucible is melted, shape Becoming silicon solution, in stove, master control temperature controls in temperature n1, and described n1 is 1540 DEG C;
F, long crystalline substance prepare: wait solid silicon feedstock to melt completely, be incubated 25 minutes;
G, long crystalline substance: with the long brilliant height of budget as H, actual (tube) length crystalline substance is h1, crystal growing stage is divided into three rank:
1, the first crystal growing stage: 0 < h1 < 0.6*H, the DS cooling starting polycrystal silicon ingot furnace interior is fast, carries out cold to ingot casting crucible But, carrying out long crystalline substance, silicon solution temperature controls in temperature n2;
2, the second crystal growing stage: h1=0.6H, by the vacuum feeding-system being arranged on polycrystal silicon ingot stove, in ingot casting crucible By-carriage adulterant, regulates resistivity, carries out a resistance optimization, and now silicon solution temperature controls in temperature n3;
3, the 3rd crystal growing stage: h1=0.8*H, by the vacuum feeding-system being arranged on polycrystal silicon ingot stove, in ingot casting crucible By-carriage adulterant, regulates resistivity, carries out secondary resistance optimization, until long crystalline substance completes, 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, pressure release subsequently, finally carry with driving etc. Ingot casting crucible is taken out by equipment, and ingot casting is come out of the stove.
Above-mentioned a kind of multistage resistivity controls high-efficiency polycrystalline silicon chip technology, and wherein, described ingot casting raw material is contained within p-type Gallium elemental body, described p-type gallium elemental body is 0.0294:1(g/Kg with the weight ratio of ingot casting raw material), i.e. gallium is 25g, ingot casting raw material For 850KG.
Above-mentioned a kind of multistage resistivity controls high-efficiency polycrystalline silicon chip technology, and wherein, described n2 is 1416 DEG C, described n3 Being 1409 DEG C, described n4 is 1404 DEG C.
Above-mentioned a kind of multistage resistivity controls high-efficiency polycrystalline silicon chip technology, and wherein, described adulterant is that p-doped mother closes Gold bullion, the resistivity of described p-doped foundry alloy block is 0.005 Ω cm.
Above-mentioned a kind of multistage resistivity controls high-efficiency polycrystalline silicon chip technology, and wherein, the sintering temperature in step A is 1020℃。
Above-mentioned a kind of multistage resistivity controls high-efficiency polycrystalline silicon chip technology, wherein, described in the second crystal growing stage and In 3rd crystal growing stage, the amount of the adulterant of interpolation is respectively 600g and 330g;
Embodiment two
As it is shown in figure 1, above-mentioned a kind of multistage resistivity controls high-efficiency polycrystalline silicon chip technology, wherein, described vacuum feed supplement system System includes vaccum-pumping equipment 1, charging chamber 2, quartz mozzle 3 and control valve 4, and described vaccum-pumping equipment 1, quartz mozzle 3 are equal With charging chamber 2 UNICOM, vaccum-pumping equipment 1 is connected to the upper end, chamber 2 that feeds, and quartz mozzle 3 is connected to the lower end, chamber 2 that feeds, controls Valve 4 is arranged on quartz mozzle 3, controls quartz mozzle 3 and carries adulterant, and polysilicon is inserted in the lower end of quartz mozzle 3 In ingot stove 5, it is positioned at the top of ingot casting crucible 6.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto, Any those familiar with the art in the technical scope that the invention discloses, the change that can readily occur in or replacement, All should contain within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection domain of claims It is as the criterion.

Claims (7)

1. a multistage resistivity controls high-efficiency polycrystalline silicon chip technology, it is characterised in that include step in detail below:
A, preparation release layer: prepare silicon nitride powder, stir, preheat ingot casting crucible, and the silicon nitride powder that will stir Material is sprayed on the inwall of ingot casting crucible, the most again heats ingot casting crucible, is burnt by the silicon nitride powder on ingot casting crucible inwall Knot, forms release layer;
B, charging: ingot casting raw material is filled in ingot casting crucible;
C, polycrystal silicon ingot stove dust suction: during ingot casting, can adsorb a large amount of oxide in the burner hearth of polycrystal silicon ingot stove, uses dust suction Major part oxide in burner hearth absorbed by device;
D, feed intake: use the conveying equipments such as driving that the ingot casting crucible fed in step B is put into polycrystal silicon ingot stove;
E, heating, melting: start polycrystal silicon ingot stove, ingot casting crucible is heated, ingot casting raw material in ingot casting crucible is melted, shape Becoming silicon solution, in stove, main control temperature controls in temperature n1, and described n1 is 1530 DEG C ~ 1560 DEG C;
F, long crystalline substance prepare: silicon material melts completely, is incubated 10 ~ 30 minutes;
G, long crystalline substance: with the long brilliant height of budget as H, actual (tube) length crystalline substance is h1, crystal growing stage is divided into three rank:
(1), the first crystal growing stage: 0 < h1 < 0.6*H, the DS cooling starting polycrystal silicon ingot furnace interior is fast, carries out ingot casting crucible Cooling, carries out long crystalline substance, and silicon solution temperature controls in temperature n2;
(2), the second crystal growing stage: h1=0.60*H ~ 0.63*H, by the vacuum feeding-system being arranged on polycrystal silicon ingot stove, to By-carriage adulterant in ingot casting crucible, regulates resistivity, carries out a resistance optimization, and now silicon solution temperature controls in temperature n3;
(3), the 3rd crystal growing stage: h1=0.80*H ~ 0.83*H, by the vacuum feeding-system being arranged on polycrystal silicon ingot stove, to By-carriage adulterant in ingot casting crucible, regulates resistivity, carries out secondary resistance optimization, until long crystalline substance completes, 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, pressure release subsequently, finally carry with driving etc. Ingot casting crucible is taken out by equipment, and ingot casting is come out of the stove.
The most above-mentioned a kind of multistage resistivity controls high-efficiency polycrystalline silicon chip technology, and wherein, described ingot casting raw material is contained within p-type gallium Elemental body, described p-type gallium elemental body is 0.01 ~ 0.1:1(g/Kg with the weight ratio of ingot casting raw material).
3. a kind of multistage resistivity as claimed in claim 1 controls high-efficiency polycrystalline silicon chip technology, it is characterised in that described n2 Being 1410 DEG C ~ 1417 DEG C, described n3 is 1404 DEG C ~ 1412 DEG C, and described n4 is 1400 DEG C ~ 1406 DEG C.
4. multistage resistivity as claimed in claim 1 a kind of controls high-efficiency polycrystalline silicon chip technology, it is characterised in that described very Empty feeding-system includes vaccum-pumping equipment, charging chamber, quartz mozzle and control valve, described vaccum-pumping equipment, quartz mozzle All with charging chamber UNICOM, vaccum-pumping equipment is connected to the upper end, chamber that feeds, and quartz mozzle is connected to the lower end, chamber that feeds, and control valve sets Being placed on quartz mozzle, control quartz mozzle conveying adulterant, the lower end of quartz mozzle is inserted in polycrystal silicon ingot stove, position Top in ingot casting crucible.
5. multistage resistivity as claimed in claim 1 a kind of controls high-efficiency polycrystalline silicon chip technology, it is characterised in that described in mix Miscellaneous dose is p-doped foundry alloy block, and the resistivity of described p-doped foundry alloy silico briquette is 0.002 Ω m ~ 0.007 Ω cm.
6. a kind of multistage resistivity as claimed in claim 1 controls high-efficiency polycrystalline silicon chip technology, it is characterised in that step A In sintering temperature be 800 DEG C ~ 1100 DEG C.
7. multistage resistivity as claimed in claim 1 a kind of controls high-efficiency polycrystalline silicon chip technology, it is characterised in that described In second crystal growing stage and the 3rd crystal growing stage, the amount of the adulterant every time added can be different, add adulterant and casting every time The weight ratio of ingot raw material is 0.1 ~ 1:1(g/Kg).
CN201610846522.2A 2016-09-26 2016-09-26 Multi-stage electrical resistivity control efficient polycrystalline silicon chip technology Pending CN106319622A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN101654804A (en) * 2009-09-24 2010-02-24 浙江大学 Method for controlling specific resistance of gallium-doped Czochralski silicon in crystal growth process
CN102242395A (en) * 2011-06-17 2011-11-16 常州天合光能有限公司 Continuous feeding device for growth of silicon single crystal and single crystal furnace equipped with same
CN102560645A (en) * 2011-09-02 2012-07-11 江苏协鑫硅材料科技发展有限公司 Method for controlling resistivity during crystal silicon forming process, and device thereof
CN103088407A (en) * 2009-01-05 2013-05-08 法国原子能委员会 Method For Solidifying A Semiconductor With Adding Charges Of A Doped Semiconductor During The Crystallisation
CN103966665A (en) * 2014-05-15 2014-08-06 阿特斯光伏电力(洛阳)有限公司 Gallium-doped polycrystalline silicon ingot and preparation method thereof
CN104451869A (en) * 2014-11-20 2015-03-25 江西赛维Ldk太阳能高科技有限公司 Silicon liquid extraction device and polycrystalline silicon cast ingot doping method
CN104532345A (en) * 2014-12-23 2015-04-22 阿特斯(中国)投资有限公司 Manufacturing method of polycrystalline silicon cast ingot and polycrystalline silicon cast ingot

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN103088407A (en) * 2009-01-05 2013-05-08 法国原子能委员会 Method For Solidifying A Semiconductor With Adding Charges Of A Doped Semiconductor During The Crystallisation
CN101654804A (en) * 2009-09-24 2010-02-24 浙江大学 Method for controlling specific resistance of gallium-doped Czochralski silicon in crystal growth process
CN102242395A (en) * 2011-06-17 2011-11-16 常州天合光能有限公司 Continuous feeding device for growth of silicon single crystal and single crystal furnace equipped with same
CN102560645A (en) * 2011-09-02 2012-07-11 江苏协鑫硅材料科技发展有限公司 Method for controlling resistivity during crystal silicon forming process, and device thereof
CN103966665A (en) * 2014-05-15 2014-08-06 阿特斯光伏电力(洛阳)有限公司 Gallium-doped polycrystalline silicon ingot and preparation method thereof
CN104451869A (en) * 2014-11-20 2015-03-25 江西赛维Ldk太阳能高科技有限公司 Silicon liquid extraction device and polycrystalline silicon cast ingot doping method
CN104532345A (en) * 2014-12-23 2015-04-22 阿特斯(中国)投资有限公司 Manufacturing method of polycrystalline silicon cast ingot and polycrystalline silicon cast ingot

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