CN105154972A - Square silicon core production method - Google Patents
Square silicon core production method Download PDFInfo
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- CN105154972A CN105154972A CN201510525356.1A CN201510525356A CN105154972A CN 105154972 A CN105154972 A CN 105154972A CN 201510525356 A CN201510525356 A CN 201510525356A CN 105154972 A CN105154972 A CN 105154972A
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Abstract
A square silicon core production method includes: mixing original polycrystalline silicon, original bar materials, carbon head materials, top-and-tail materials, fragmental polycrystalline, offcut materials and granulated silicon; heating the materials for melting, and allowing impurity volatilization for 2.5-3.5h after melting of the materials is finished; carrying out crystal pulling, keeping the seeding temperature at 1225-1325 DEG C, keeping a crucible position between 15mm to 82mm, controlling seeding diameters to range from 4mm to 6mm and seeding length to range from 120mm to 180mm, and keeping head pulling rate at 0.88-0.95mm/min; shouldering, crystallizing and closing; cutting to obtain square silicon cores. By adoption of the square silicon core production method and scientific and reasonable production process, potential crack rate of square silicon cores is reduced from 4-5% to 1.5-2%, proportion of polycrystalline silicon core round bars in silicon core round bars after crystal pulling is greatly decreased, the proportion of monocrystalline silicon core round bars is increased from 4% to 21%.
Description
Technical field
The invention belongs to silicon single crystal and technical field of polysilicon production, be specifically related to a kind of method of producer silicon core.
Background technology
Silicon single crystal is a kind of very important semiconductor material, and the development of its production technique is divided into following several stages:
First stage does thermal barrier with molybdenum filament or tantalum pipe, easy to use, and production unit is simple, is in order to centre can be effective in the silicon material preparing zone melting method silicon single crystal with sour eating away tantalum with tantalum pipe.But under high temperature, atoms metal extends influence polysilicon purity and quality, and this technique is replaced by silicon core thermal barrier very soon.
Subordinate phase is that zone melting method produces silicon core (circle silicon core): silicon is semi-conductor, there is the temperature negative resistance effect that more high resistance is lower, the silicon core drawn with zone melting method after the heating or after high-voltage breakdown low-pressure heating become thermal barrier in reduction furnace, carry out reduction reaction deposition growing polysilicon, the polysilicon quality of production significantly improves.The production technique of zone melting method silicon core is also several times changed, from once drawing one to draw several to save the time of tearing stove blow-on open and consuming to a heat, and then develop into Yi La Duogen, a heat draws for several times, make a heat can produce more than ten silicon core, production efficiency improves greatly.But zone melting method silicon core is produced and required higher to operative employee, the much more difficult realizations of Auto-control of the process, silicon core is thin again, and operation must stare at any time thus labour intensity is strengthened, and production cost is also relatively high.
Phase III uses vertical pulling method to produce silicon core pole, after butt truncates, become the idiosome of cutting side's silicon core, afterwards by sticky stick, upper rod, wiring, threading, discharge water, cut, lower rod, separation, grinding core punching, corrosion cleaning, inspection, vacuum packaging etc., the square silicon core needed for formation.Seventy or eighty follow the square silicon core of this silicon core pole cutting at least, and more than 200 at most, effect improves greatly.Although effect improves, but find aborning, occur in the silicon core pole side of cutting silicon core process that the hidden square silicon core split is many, hidden splitting not only causes macroscopic irregularity, the most important thing is output characteristic and the use of the side's of impact silicon core, produce the hidden reason split and be mostly, because inappropriate technology in crystal production process produces thermal stresses and dislocation, during the cutting of the side's of adding silicon core, easily to produce excessive mechanical stress, therefore square silicon core more easily produces hidden splitting, and concrete technology defect is as follows:
1. after material terminates, the impurity in raw material does not fully vapor away, and impurity is trapped in quartz crucible;
2. seeding temperature does not reach best;
3. crucible position is not in optimum position, affects into brilliant difficulty;
4. seeding diameter is large, and dislocation is not got rid of totally;
5. head pulling rate is too fast, does not mate with the product of required drawing;
6. crucible is followed more improper than design, causes silicon liquid level not at same relative position.
Not only silicon core in the side's of causing is hidden splits for above-mentioned defective workmanship, makes the ratio of the silicon single crystal core pole of production lower simultaneously, makes deterioration in quality.
Summary of the invention
Object of the present invention is just a kind of method providing producer silicon core for solving the deficiencies in the prior art, reduces its hidden rate of splitting, and improves the ratio of silicon single crystal core pole.
The object of the invention is with following technical proposals realize:
A method for producer silicon core, comprises the following steps:
1) feed intake get virgin polycrystalline silicon, primary bar, carbon head material, end to end material, broken polycrystalline, edge skin material mix with grain silicon, adopt phosphorus silicon mother alloy as doping agent, drop in quartz crucible;
2) material is by thrown heating material melting, and after material terminates, impurity volatilizes is 2.5 ~ 3.5h;
3) crystal pulling seeding temperature remains between 1225 ~ 1325 DEG C; Crucible position is between 15 ~ 82mm; Control the scope 4 ~ 6mm of seeding diameter, seeding length is 120 ~ 180mm; Head pulling rate remains between 0.88 ~ 0.95mm/min, then carry out shouldering, etc. brilliant, ending operation;
4) the silicon core pole formed after the crystal pulling of the side's of cutting silicon core, through cutting brilliant, the cutting side of obtaining silicon core.
The each raw materials by weight portion ratio fed intake in step 1) is: virgin polycrystalline silicon: primary bar: carbon head material: expect end to end: broken polycrystalline: edge skin material: grain silicon=(30 ~ 70): (30 ~ 40): (20 ~ 40): (5 ~ 10): (5 ~ 35): (15 ~ 35): (5 ~ 20), the adding proportion of phosphorus silicon mother alloy is 0.05/10000th ~ 0.17 of each raw material total mass.
In step 1), primary bar is the primary polycrystalline of length 200 ~ 300mm, and when feeding intake, primary bar stands in the middle of crucible and places.
In step 3) by the diameter of quartz crucible, isometrical diameter, pulling rate, crucible rise calculate rational crucible follow than, keep crystal pulling liquid level relative position not change.
Seeding pot position is 50 ~ 70mm.
Use the method for producer silicon core provided by the invention, by scientific and reasonable production technique, not only the hidden rate of splitting of the side's of making silicon core is reduced to 1.5 ~ 2% by 4 ~ 5% before, and the polysilicon core pole ratio greatly reduced after crystal pulling in silicon core pole, the ratio of whole silicon single crystal core pole is promoted to 21% by 4% before.
Embodiment
embodiment 1
The method of producer silicon core provided by the invention, comprises the following steps:
1) feed intake that to get virgin polycrystalline silicon, primary bar, carbon head material, end to end material, broken polycrystalline, edge skin material and grain silicon be (30 ~ 70) by ratio of weight and the number of copies: (30 ~ 40): (20 ~ 40): (5 ~ 10): (5 ~ 35): (15 ~ 35): (5 ~ 20) mix, adopt phosphorus silicon mother alloy as doping agent, phosphorus silicon mother alloy adds according to calculation result, general adding proportion is 0.05/10000th ~ 0.17 of each raw material total mass, drops in quartz crucible; Primary bar is the primary polycrystalline of length 200 ~ 300mm, Substitute For Partial virgin polycrystalline silicon, when feeding intake, primary bar stands in the middle of crucible and places, broken polycrystalline and grain silicon filling chink, single stove about charging capacity 18kg (23 cun of crucibles) can be increased, thus the side's of adding silicon core 4 ~ 16/stove, reduce production cost;
2) material is by thrown heating material melting, after material terminates, is vapored away by the impurity in raw material in order to abundant, and than the original volatilizes increasing by 1.5 ~ 2.5h, total volatilizes is 2.5 ~ 3.5h;
3) crystal pulling seeding optimum temps remains between 1225 ~ 1325 DEG C; Best crucible position is between 15 ~ 82mm; Control the scope 4 ~ 6mm of seeding diameter, seeding length is 120 ~ 180mm, fully the thermal stresses in seeding process and mechanical stress is excluded; Reduce and stablize head pulling rate, remain between 0.88 ~ 0.95mm/min, make pulling rate smooth transition, avoid the big ups and downs of pulling rate and temperature, by the diameter of quartz crucible, isometrical diameter, pulling rate, crucible rise calculate rational crucible follow than, keep crystal pulling liquid level relative position not change; Then carry out shouldering, etc. brilliant, ending operation;
4) the silicon core pole formed after the crystal pulling of the side's of cutting silicon core, through cutting brilliant, the cutting side of obtaining silicon core.
Use primary bar Substitute For Partial virgin polycrystalline silicon in the raw material of producer silicon core of the present invention, improve single stove charging capacity, and the flavoring food not using impurity more, and after material terminates, increase impurity volatilizes further, reduce impurity and be detained; Then scientific and reasonable control crystal pulling process, eliminate internal stress and dislocation, the side's of minimizing silicon core is hidden splits rate, improves the ratio of silicon single crystal core pole, obtains good product quality.
embodiment 2
The method of producer silicon core provided by the invention, comprises the following steps:
1) feed intake get virgin polycrystalline silicon 50kg, primary bar 30kg, carbon head material 30kg, expect 8kg end to end, broken polycrystalline 20kg, edge skin material 20kg mix with grain silicon 10kg, add 2g phosphorus silicon mother alloy as doping agent, drop in quartz crucible;
2) material is by thrown heating material melting, and after material terminates, impurity volatilizes is 3h;
3) crystal pulling seeding optimum temps remains on 1300 DEG C; Seeding crucible position is 60.5mm; Control seeding diameter 5mm, seeding length is 150mm, fully the thermal stresses in seeding process and mechanical stress is excluded; Reduce and stablize head pulling rate, remain on 0.9mm/min, make pulling rate smooth transition, avoid the big ups and downs of pulling rate and temperature, by the diameter of quartz crucible, isometrical diameter, pulling rate, crucible rise calculate rational crucible follow than, keep crystal pulling liquid level relative position not change; Then carry out shouldering, etc. brilliant, ending operation;
4) the silicon core pole formed after the crystal pulling of the side's of cutting silicon core, through cutting brilliant, the cutting side of obtaining silicon core.
In embodiment 3-16, the processing parameter of producer silicon core is in Table 1-2, and other are with embodiment 2.
the process parameter table of table 1 embodiment 3-9 producer silicon core
。
the process parameter table of table 2 embodiment 10-16 producer silicon core
Claims (5)
1. a method for producer silicon core, is characterized in that comprising the following steps:
1) feed intake get virgin polycrystalline silicon, primary bar, carbon head material, end to end material, broken polycrystalline, edge skin material mix with grain silicon, adopt phosphorus silicon mother alloy as doping agent, drop in quartz crucible;
2) material is by thrown heating material melting, and after material terminates, impurity volatilizes is 2.5 ~ 3.5h;
3) crystal pulling seeding temperature remains between 1225 ~ 1325 DEG C; Crucible position is between 15 ~ 82mm; Control the scope 4 ~ 6mm of seeding diameter, seeding length is 120 ~ 180mm; Head pulling rate remains between 0.88 ~ 0.95mm/min, then carry out shouldering, etc. brilliant, ending operation;
4) the silicon core pole formed after the crystal pulling of the side's of cutting silicon core, through cutting brilliant, the cutting side of obtaining silicon core.
2. the method for producer silicon core as claimed in claim 1, it is characterized in that each raw materials by weight portion ratio fed intake in step 1) is: virgin polycrystalline silicon: primary bar: carbon head material: expect end to end: broken polycrystalline: edge skin material: grain silicon=(30 ~ 70): (30 ~ 40): (20 ~ 40): (5 ~ 10): (5 ~ 35): (15 ~ 35): (5 ~ 20), the adding proportion of phosphorus silicon mother alloy is 0.05/10000th ~ 0.17 of each raw material total mass.
3. the method for producer silicon core as claimed in claim 1, is characterized in that in step 1), primary bar is the primary polycrystalline of length 200 ~ 300mm, and when feeding intake, primary bar stands in the middle of crucible and places.
4. the method for producer silicon core as claimed in claim 1, it is characterized in that in step 3) by the diameter of quartz crucible, isometrical diameter, pulling rate, crucible rise calculate rational crucible follow than, keep crystal pulling liquid level relative position not change.
5. the method for producer silicon core as claimed in claim 1, is characterized in that seeding pot position is 50 ~ 70mm.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105970288A (en) * | 2016-06-22 | 2016-09-28 | 江苏拜尔特光电设备有限公司 | Novel polycrystalline silicon core rod drawing method |
| CN107587188A (en) * | 2017-08-31 | 2018-01-16 | 河南协鑫光伏科技有限公司 | A kind of silicon core pole cooling means |
| CN109554760A (en) * | 2019-01-31 | 2019-04-02 | 内蒙古通威高纯晶硅有限公司 | A kind of trace doped method of masterbatch for avoiding silicon core from making the transition |
| CN111676510A (en) * | 2020-06-22 | 2020-09-18 | 四川永祥多晶硅有限公司 | Method for manufacturing silicon core by using non-washing-free material |
| CN112301426A (en) * | 2019-08-02 | 2021-02-02 | 宁夏隆基硅材料有限公司 | Method for manufacturing silicon single crystal rod |
| CN113293431A (en) * | 2021-06-02 | 2021-08-24 | 内蒙古和光新能源有限公司 | Square silicon core and preparation method thereof |
| CN113322515A (en) * | 2021-06-02 | 2021-08-31 | 内蒙古和光新能源有限公司 | Production method of silicon core round rod |
| CN114752994A (en) * | 2022-03-14 | 2022-07-15 | 中国恩菲工程技术有限公司 | Method and device for reducing crystal hidden crack of straightened silicon core rod |
| CN114855262A (en) * | 2022-07-05 | 2022-08-05 | 江苏鑫华半导体科技股份有限公司 | Pretreatment method for zone-melting polycrystalline silicon rod |
| CN115287756A (en) * | 2022-06-23 | 2022-11-04 | 内蒙古通威高纯晶硅有限公司 | Method for preparing square silicon core by using crushed material |
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| CN101498033A (en) * | 2009-01-20 | 2009-08-05 | 刘朝轩 | Method for crystal crushed aggregate drawing silicon core and simple apparatus |
| CN102345164A (en) * | 2011-10-11 | 2012-02-08 | 天威四川硅业有限责任公司 | Efficient preparation method of silicon cores and silicon core preparation furnace |
| CN104264221A (en) * | 2014-09-10 | 2015-01-07 | 河南协鑫光伏科技有限公司 | Square silicon core material for producing primary polysilicon and preparation method thereof |
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2015
- 2015-08-25 CN CN201510525356.1A patent/CN105154972A/en active Pending
Patent Citations (3)
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| CN101498033A (en) * | 2009-01-20 | 2009-08-05 | 刘朝轩 | Method for crystal crushed aggregate drawing silicon core and simple apparatus |
| CN102345164A (en) * | 2011-10-11 | 2012-02-08 | 天威四川硅业有限责任公司 | Efficient preparation method of silicon cores and silicon core preparation furnace |
| CN104264221A (en) * | 2014-09-10 | 2015-01-07 | 河南协鑫光伏科技有限公司 | Square silicon core material for producing primary polysilicon and preparation method thereof |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105970288A (en) * | 2016-06-22 | 2016-09-28 | 江苏拜尔特光电设备有限公司 | Novel polycrystalline silicon core rod drawing method |
| CN107587188A (en) * | 2017-08-31 | 2018-01-16 | 河南协鑫光伏科技有限公司 | A kind of silicon core pole cooling means |
| CN109554760A (en) * | 2019-01-31 | 2019-04-02 | 内蒙古通威高纯晶硅有限公司 | A kind of trace doped method of masterbatch for avoiding silicon core from making the transition |
| CN112301426A (en) * | 2019-08-02 | 2021-02-02 | 宁夏隆基硅材料有限公司 | Method for manufacturing silicon single crystal rod |
| CN112301426B (en) * | 2019-08-02 | 2022-08-12 | 宁夏隆基硅材料有限公司 | Method for manufacturing silicon single crystal rod |
| CN111676510A (en) * | 2020-06-22 | 2020-09-18 | 四川永祥多晶硅有限公司 | Method for manufacturing silicon core by using non-washing-free material |
| CN113293431A (en) * | 2021-06-02 | 2021-08-24 | 内蒙古和光新能源有限公司 | Square silicon core and preparation method thereof |
| CN113322515A (en) * | 2021-06-02 | 2021-08-31 | 内蒙古和光新能源有限公司 | Production method of silicon core round rod |
| CN114752994A (en) * | 2022-03-14 | 2022-07-15 | 中国恩菲工程技术有限公司 | Method and device for reducing crystal hidden crack of straightened silicon core rod |
| CN115287756A (en) * | 2022-06-23 | 2022-11-04 | 内蒙古通威高纯晶硅有限公司 | Method for preparing square silicon core by using crushed material |
| CN115287756B (en) * | 2022-06-23 | 2023-09-08 | 内蒙古通威高纯晶硅有限公司 | Method for preparing square silicon core by using crushed materials |
| CN114855262A (en) * | 2022-07-05 | 2022-08-05 | 江苏鑫华半导体科技股份有限公司 | Pretreatment method for zone-melting polycrystalline silicon rod |
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Application publication date: 20151216 |