CN105239152A - Production method of solar-grade czochralski silicon - Google Patents
Production method of solar-grade czochralski silicon Download PDFInfo
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- CN105239152A CN105239152A CN201510822124.2A CN201510822124A CN105239152A CN 105239152 A CN105239152 A CN 105239152A CN 201510822124 A CN201510822124 A CN 201510822124A CN 105239152 A CN105239152 A CN 105239152A
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Abstract
The invention relates to the technical field of czochralski silicon. A production method comprises the eight steps of charging, melting, temperature stabilizing, seeding, diameter enlarging, equal-diameter growth, ending and the like. In the seeding process, a crucible position is adjusted to make the distance from a silicon liquid level to a guide cylinder range from 25 mm to 28 mm. The method is easy and convenient to operate and easy to achieve, crystal defects which may occur in the crystallization process can be effectively reduced, the problems of black chips and black angle-shaped sheets in the czochralski silicon are reduced, the quality of monocrystal is obviously improved, the service life of the monocrystal is obviously prolonged, goods returning caused by quality defects of products is avoided, and unnecessary fund waste is reduced for enterprises.
Description
Technical field
The present invention relates to pulling of silicon single crystal technical field, be specifically related to a kind of production method of solar level pulling of silicon single crystal.
Background technology
Sun power is one of following most important green energy resource, and as the core of high efficiency solar cell, colory silicon single crystal is the major products that people research and develop always.
The production method of silicon single crystal mainly contains vertical pulling method (CZ), zone melting method (FZ) and epitaxial method, and wherein vertical pulling method and zone melting method are for extending silicon single crystal bar, and epitaxial method is for extending monocrystalline silicon thin film.The silicon single crystal produced due to vertical pulling method is widely used in semiconductor integrated circuit, diode, epitaxial wafer substrate, and the essential domain such as solar cell, is thus subject to the special concern of people.
At present in the production field of pulling of silicon single crystal, oxygen is a kind of usual impurities in pulling of silicon single crystal, and this is mainly caused by the production technique of silicon single crystal.Practice shows, the oxygen in silicon single crystal mainly concentrates on its head, if the head oxygen level of silicon single crystal is too high, will causes so-called " black chip " and " black gusset plate " problem, thus affect quality product.
The harm of oxygen is, oxygen can form Thermal donor and new promoted university, and the resistivity evenness of silicon single crystal is deteriorated; In addition, oxygen also with the formation close relation of microdefect in pulling of silicon single crystal, and the microdefect of silicon chip surface also can have influence on the yield rate of device in device thermal oxidation technology.Therefore, in the detection of silicon single crystal, generally the black chip in silicon chip and black gusset plate phenomenon are taked to the attitude of zero tolerance at present.But, the current method but also lacking the black chip of a kind of simple, effective, easy minimizing and black gusset plate.
Summary of the invention
The technical problem to be solved in the present invention is for above-mentioned the deficiencies in the prior art, a kind of production method of solar level pulling of silicon single crystal is provided, it is for the defect of current pulling of silicon single crystal production technique, prior art is improved, by reducing the crucible position in seeding process, reduce the oxygen level of head of single crystal, thus reach the object reducing black chip and black gusset plate in pulling of silicon single crystal.
Technical scheme of the present invention is: a kind of production method of solar level pulling of silicon single crystal, comprises the steps:
(1) reinforced: silicon raw material and doping agent are put into quartz crucible by semiconductor type as required;
(2) melt: single crystal growing furnace cut out and vacuumizes, making the pressure in single crystal growing furnace maintain below 4Pa, then rising to 90 ~ 94 kilowatts by disposable for heating power;
(3) surely warm: after silicon melting sources becomes liquid, heating power to be down to 40 kilowatts and to drop into temperature auto-programming, temperature auto-programming makes in-furnace temperature keep constant and maintain constant temperature 1.5 hours;
(4) seeding: adjustment crucible position makes silicon liquid liquid level be 25 ~ 28mm apart from the distance of guide shell, is turned by crystalline substance and is set to 6 circle per minutes, crucible turns and is set to 2 circle per minutes, then seed crystal is down to silicon liquid liquid level place and carries out seeding; The total length of seeding is 150 ~ 160mm, and during seeding, average pull rate controls at 3 ~ 6mm/min, and the initial stage, casting speed control was at 1 ~ 3mm/min, and seeding to reach casting speed control after 30mm at 3 ~ 6mm/min;
(5) shouldering: after seeding completes, is down to 0.7mm/min by pulling rate, and heating power reduces by 5 kilowatts, 3 ~ 4 hours shouldering time;
(6) turn shoulder: when silicon rod diameter also has 5 ~ 10mm apart from isometrical diameter, carried by pulling rate to 2.0mm/min, carry out turning shoulder;
(7) isodiametric growth; When silicon rod diameter reaches isometrical diameter, the initial pulling rate of wire diameter automatic such as pulling rate to be down to, to be set to 1.15mm/min etc. the initial pulling rate of wire diameter automatic, setting crucible lifting speed, then drops into isometrical auto-programming and carries out isodiametric growth;
(8) finish up: after isodiametric growth completes, exit isometrical auto-programming, stop crucible liter, pulling rate is carried to 1.0mm/min, drop into ending auto-programming, put off blowing out when length reaches diameter value.
Seeding total length in step (4) is preferably 160 millimeters.
The beneficial effect that produces of technique scheme is adopted to be: the inventive method effectively can reduce black chip in pulling of silicon single crystal and black gusset plate problem, its principle is, oxygen element under normal circumstances in quartz crucible at high temperature can generate silicon oxide and discharge with air-flow, but partial oxidation silicon can incorporate silicon liquid again, the oxygen element entered in the unit time in single crystal is caused to increase, oxygen level raises, and after using present method, increase the distance between guide shell and liquid level, decrease the probability that oxygen element enters monocrystalline, thus the oxygen level reduced in monocrystalline, decrease the black chip because excess oxygen content brings and black gusset plate problem.
Present method is simple, and it effectively reduces black chip in pulling of silicon single crystal and black gusset plate phenomenon, improves life-span and the quality of monocrystalline.The silicon single crystal that this method is made has fine qualities, and can be used for producing the products such as solar cell.
Embodiment
Below the present embodiment is described in further detail, but the present invention is not limited to specific embodiment.
Embodiment 1:
A production method for solar level pulling of silicon single crystal, comprises the steps:
(1) reinforced: silicon raw material and doping agent are put into quartz crucible by semiconductor type as required;
(2) melt: single crystal growing furnace cut out and vacuumizes, making the pressure in single crystal growing furnace maintain below 4Pa, then rising to 90 kilowatts by disposable for heating power;
(3) surely warm: after silicon melting sources becomes liquid, heating power to be down to 40 kilowatts and to drop into temperature auto-programming, temperature auto-programming makes in-furnace temperature keep constant and maintain constant temperature 1.5 hours;
(4) seeding: adjustment crucible position makes silicon liquid liquid level be 28mm apart from the distance of guide shell, is turned by crystalline substance and is set to 6 circle per minutes, crucible turns and is set to 2 circle per minutes, then seed crystal is down to silicon liquid liquid level place and carries out seeding; The total length of seeding is 150mm, and during seeding, average pull rate controls at 6mm/min, and the initial stage, casting speed control was at 1mm/min, and seeding to reach casting speed control after 30mm at 6mm/min;
(5) shouldering: after seeding completes, is down to 0.7mm/min by pulling rate, and heating power reduces by 5 kilowatts, 3 hours shouldering time;
(6) turn shoulder: when silicon rod diameter also has 10mm apart from isometrical diameter, carried by pulling rate to 2.0mm/min, carry out turning shoulder;
(7) isodiametric growth; When silicon rod diameter reaches isometrical diameter, the initial pulling rate of wire diameter automatic such as pulling rate to be down to, to be set to 1.15mm/min etc. the initial pulling rate of wire diameter automatic, setting crucible lifting speed, then drops into isometrical auto-programming and carries out isodiametric growth;
(8) finish up: after isodiametric growth completes, exit isometrical auto-programming, stop crucible liter, pulling rate is carried to 1.0mm/min, drop into ending auto-programming, put off blowing out when length reaches diameter value.
Embodiment 2:
A production method for solar level pulling of silicon single crystal, comprises the steps:
(1) reinforced: silicon raw material and doping agent are put into quartz crucible by semiconductor type as required;
(2) melt: single crystal growing furnace cut out and vacuumizes, making the pressure in single crystal growing furnace maintain below 4Pa, then rising to 94 kilowatts by disposable for heating power;
(3) surely warm: after silicon melting sources becomes liquid, heating power to be down to 40 kilowatts and to drop into temperature auto-programming, temperature auto-programming makes in-furnace temperature keep constant and maintain constant temperature 1.5 hours;
(4) seeding: adjustment crucible position makes silicon liquid liquid level be 25mm apart from the distance of guide shell, is turned by crystalline substance and is set to 6 circle per minutes, crucible turns and is set to 2 circle per minutes, then seed crystal is down to silicon liquid liquid level place and carries out seeding; The total length of seeding is 160mm, and during seeding, average pull rate controls at 3mm/min, and the initial stage, casting speed control was at 3mm/min, and seeding to reach casting speed control after 30mm at 3mm/min;
(5) shouldering: after seeding completes, is down to 0.7mm/min by pulling rate, and heating power reduces by 5 kilowatts, 4 hours shouldering time;
(6) turn shoulder: when silicon rod diameter also has 5mm apart from isometrical diameter, carried by pulling rate to 2.0mm/min, carry out turning shoulder;
(7) isodiametric growth; When silicon rod diameter reaches isometrical diameter, the initial pulling rate of wire diameter automatic such as pulling rate to be down to, to be set to 1.15mm/min etc. the initial pulling rate of wire diameter automatic, setting crucible lifting speed, then drops into isometrical auto-programming and carries out isodiametric growth;
(8) finish up: after isodiametric growth completes, exit isometrical auto-programming, stop crucible liter, pulling rate is carried to 1.0mm/min, drop into ending auto-programming, put off blowing out when length reaches diameter value.
The beneficial effect that produces of technique scheme is adopted to be: the inventive method effectively can reduce black chip in pulling of silicon single crystal and black gusset plate problem, its principle is, oxygen element under normal circumstances in quartz crucible at high temperature can generate silicon oxide and discharge with air-flow, but partial oxidation silicon can incorporate silicon liquid again, the oxygen element entered in the unit time in single crystal is caused to increase, oxygen level raises, and after using present method, increase the distance between guide shell and liquid level, decrease the probability that oxygen element enters monocrystalline, thus the oxygen level reduced in monocrystalline, decrease the black chip because excess oxygen content brings and black gusset plate problem.
Claims (2)
1. a production method for solar level pulling of silicon single crystal, is characterized in that: comprise the steps:
(1) reinforced: silicon raw material and doping agent are put into quartz crucible by semiconductor type as required;
(2) melt: single crystal growing furnace cut out and vacuumizes, making the pressure in single crystal growing furnace maintain below 4Pa, then rising to 90 ~ 94 kilowatts by disposable for heating power;
(3) surely warm: after silicon melting sources becomes liquid, heating power to be down to 40 kilowatts and to drop into temperature auto-programming, temperature auto-programming makes in-furnace temperature keep constant and maintain constant temperature 1.5 hours;
(4) seeding: adjustment crucible position makes silicon liquid liquid level be 25 ~ 28mm apart from the distance of guide shell, is turned by crystalline substance and is set to 6 circle per minutes, crucible turns and is set to 2 circle per minutes, then seed crystal is down to silicon liquid liquid level place and carries out seeding; The total length of seeding is 150 ~ 160mm, and during seeding, average pull rate controls at 3 ~ 6mm/min, and the initial stage, casting speed control was at 1 ~ 3mm/min, and seeding to reach casting speed control after 30mm at 3 ~ 6mm/min;
(5) shouldering: after seeding completes, is down to 0.7mm/min by pulling rate, and heating power reduces by 5 kilowatts, 3 ~ 4 hours shouldering time;
(6) turn shoulder: when silicon rod diameter also has 5 ~ 10mm apart from isometrical diameter, carried by pulling rate to 2.0mm/min, carry out turning shoulder;
(7) isodiametric growth; When silicon rod diameter reaches isometrical diameter, the initial pulling rate of wire diameter automatic such as pulling rate to be down to, to be set to 1.15mm/min etc. the initial pulling rate of wire diameter automatic, setting crucible lifting speed, then drops into isometrical auto-programming and carries out isodiametric growth;
(8) finish up: after isodiametric growth completes, exit isometrical auto-programming, stop crucible liter, pulling rate is carried to 1.0mm/min, drop into ending auto-programming, put off blowing out when length reaches diameter value.
2. the production method of a kind of solar level pulling of silicon single crystal according to claim 1, is characterized in that, the seeding total length in described step (4) is 160 millimeters.
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| CN201510822124.2A CN105239152A (en) | 2015-11-24 | 2015-11-24 | Production method of solar-grade czochralski silicon |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105696071A (en) * | 2016-03-23 | 2016-06-22 | 黄山市东晶光电科技有限公司 | Process method capable of effectively overcoming Kyropoulos-method crystal cracking |
| CN106319621A (en) * | 2016-09-22 | 2017-01-11 | 东莞市联洲知识产权运营管理有限公司 | Large-size czochralski silicon single crystal growth method |
| CN106637402A (en) * | 2016-12-22 | 2017-05-10 | 卡姆丹克太阳能（江苏）有限公司 | Flat ending method of monocrystal silicon and preparation method of monocrystal silicon |
| CN107955965A (en) * | 2017-11-22 | 2018-04-24 | 邢台晶龙电子材料有限公司 | A kind of method that vertical pulling method prepares monocrystalline silicon |
-
2015
- 2015-11-24 CN CN201510822124.2A patent/CN105239152A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105696071A (en) * | 2016-03-23 | 2016-06-22 | 黄山市东晶光电科技有限公司 | Process method capable of effectively overcoming Kyropoulos-method crystal cracking |
| CN106319621A (en) * | 2016-09-22 | 2017-01-11 | 东莞市联洲知识产权运营管理有限公司 | Large-size czochralski silicon single crystal growth method |
| CN106637402A (en) * | 2016-12-22 | 2017-05-10 | 卡姆丹克太阳能（江苏）有限公司 | Flat ending method of monocrystal silicon and preparation method of monocrystal silicon |
| CN106637402B (en) * | 2016-12-22 | 2019-04-09 | 卡姆丹克太阳能（江苏）有限公司 | The flat ending method of monocrystalline silicon and preparation method |
| CN107955965A (en) * | 2017-11-22 | 2018-04-24 | 邢台晶龙电子材料有限公司 | A kind of method that vertical pulling method prepares monocrystalline silicon |
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