CN104328482A - Growing method of large diameter float zone silicon crystal - Google Patents
Growing method of large diameter float zone silicon crystal Download PDFInfo
- Publication number
- CN104328482A CN104328482A CN201410523050.8A CN201410523050A CN104328482A CN 104328482 A CN104328482 A CN 104328482A CN 201410523050 A CN201410523050 A CN 201410523050A CN 104328482 A CN104328482 A CN 104328482A
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- diameter
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- polycrystal
- monocrystalline
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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
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
- C30B13/08—Single-crystal growth by zone-melting; Refining by zone-melting adding crystallising materials or reactants forming it in situ to the molten zone
- C30B13/10—Single-crystal growth by zone-melting; Refining by zone-melting adding crystallising materials or reactants forming it in situ to the molten zone with addition of doping materials
-
- 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
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
- C30B13/28—Controlling or regulating
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention provides a growing method of a large diameter float zone silicon crystal, wherein the growing method comprises: loading into a furnace, evacuating, inflating, preheating, melting a material, seeding, growing narrow neck, expanding shoulder, maintaining, growing in an equal diameter manner, ending, cooling, and removing and cleaning the furnace. According to the present invention, with control of the generator output power, the polycrystal material descending speed and other parameters, the problems of easy stacking caused by difficult melting of the large diameter polycrystal material, and the low crystal forming rate caused by the poor process repeatability, the dislocation produced during the shoulder expanding process and the like under the conditions of the original process and method are overcome, the crystal forming rate and the qualification rate of the large diameter float zone silicon crystal are increased, the labor intensity is reduced, and the repeatability and the reproducibility are good.
Description
Technical field
The present invention relates to a kind of growth method of large diameter zone melting silicon single crystal.
Background technology
Floating zone melting comprises tears prepurging open, preheating, material, seeding, drawing-down neck, expand shoulder, turn shoulder, keep, ending, several step such as blowing out, existing method mainly controls the growth of silicon single-crystal by the artificial control radio-frequency generator output rating height of operator and polycrystal downstream rate, tearing prepurging open, preheating, material, seeding, after drawing-down neck terminates, by operator artificial do not stop regulate radio-frequency generator output rating and polycrystal downstream rate to play to control the object expanding shoulder process, and artificial change output rating and polycrystal downstream rate turn shoulder, keep, the steps such as ending.Utilize existing method, manual operation factor is too much, and process repeatability is poor, and labor intensity of operating staff is large, easily because individual misoperation causes crystal pulling failure.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, provides a kind of growth method of large diameter zone melting silicon single crystal, effectively can improve process repeatability difference, expand the problem easily producing dislocation in shoulder process.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of growth method of large diameter zone melting silicon single crystal, is characterized in that, utilizes zone melting single-crystal stove to carry out following operation:
(1) shove charge: by crystal clamper in the polycrystalline bar loading area smelting furnace after cleaning corrosion, seed crystal is loaded on seed crystal fixed chuck;
(2) find time, inflate, preheating: preheating ring is put in below polycrystalline bar, above district's fuse circle, closes fire door and vacuumize, after pour argon gas, when furnace pressure reaches 2.6-6.5bar, stop fast aeration, use instead and inflate at a slow speed, open drain tap and carry out stream argon; After inflation, preheating is carried out to polycrystalline bar;
(3) material, seeding: withdrawn from by preheating ring, carries out material, after polycrystal fusing, seed crystal and molten silicon is carried out welding, carries out shaping, seeding after welding to melting zone;
(4) grow thin neck: after seeding terminates, carry out the growth of thin neck, thin neck diameter is at 2-6mm, and length is at 30-60mm;
(5) expand shoulder: expand shoulder process, by the actual single crystal diameter recorded, regulate the output rating of radio-frequency generator and the downstream rate of polycrystal;
(6) maintenance, isodiametric growth: when expanding shoulder diameter and being greater than required diameter, monocrystalline keeps, and starts isodiametric growth, in Crystal fsometric Growing process, the speed of rotation of polycrystal is 0.1-1 rev/min, and single crystal growing speed is at 1.5-2.5mm/min, and monocrystalline speed of rotation is 6-25 rev/min;
(7) finish up: when monocrystalline is pulled to polycrystal afterbody, start to finish up, reduce silicon single-crystal diameter gradually, when reaching desired value when finishing up to single crystal diameter, melting zone is pulled open, at this moment the lower shaft of zone melting furnace hauls monocrystalline and continues to move downward, and upper axle changes with polycrystal and moves upward, and closes argon gas;
(8) lower the temperature, tear prepurging open: slow cooling is carried out to crystal, after having redness to become black to crystal afterbody, tear prepurging open.
Preferably, the diameter of the polycrystalline bar in described step (1) is 145-175mm.
Further, in described step (2) stage stove, the output frequency of radio-frequency generator is 2-4MHz.
Further, described step (5) expands in shoulder process, and the pass of single crystal diameter and radio-frequency generator output rating and polycrystal downstream rate is: single crystal diameter=[(polycrystal diameter
2× polycrystal downstream rate)/monocrystalline downstream rate]
1/2; Radio-frequency generator output rating and single crystal diameter linear.
Further, when in described step (6), expansion shoulder diameter is greater than 8 inches, monocrystalline keeps, and starts isodiametric growth.Cooling duration in described step (8) is 50-90min.
The advantage that the present invention has and positively effect are: by control generator output rating and the isoparametric method of polycrystal downstream rate, under overcoming original technique and method condition, major diameter polycrystal fusing difficulty, easily cause the problem of windrow, process repeatability is poor, expand in shoulder process and produce the low problem of crystal forming rate that the problems such as dislocation cause, improve crystal forming rate and the qualification rate of large diameter zone melting silicon single crystal, reduce personnel labor intensity, repeatable reproducibility is good.
Accompanying drawing explanation
Fig. 1 is the graph of a relation of radio-frequency generator output rating and single crystal diameter.
Fig. 2 is the graph of a relation of single crystal diameter and polycrystal downstream rate and monocrystalline downstream rate.
Embodiment
Embodiment 1
A growth method for 8 inches of zone-melted silicon single crystals, utilizes zone melting single-crystal stove to carry out following operation: (1) shove charge: by crystal clamper in the polycrystalline bar loading area smelting furnace after cleaning corrosion, loaded by seed crystal on seed crystal fixed chuck; The diameter of polycrystalline bar is 145-175mm.
(2) find time, inflate, preheating: preheating ring is put in below polycrystalline bar, above district's fuse circle, closes fire door and vacuumize, after pour argon gas, when furnace pressure reaches 2.6-6.5bar, stop fast aeration, use instead and inflate at a slow speed, open drain tap and carry out stream argon; After inflation, preheating is carried out to polycrystalline bar; The diameter range of district's fuse circle is 280-350mm, has multi-stage stairs and inclined design above pinprick coil, and has 2-5 length to be the assist openings of 20-150mm, the thickness range 20-35mm of pin hole coil, and the output frequency of radio-frequency generator is 2-4 megahertz.
(3) material, seeding: withdrawn from by preheating ring, carries out material, after polycrystal fusing, seed crystal and molten silicon is carried out welding, carries out shaping, seeding after welding to melting zone;
(4) grow thin neck: after seeding terminates, carry out the growth of thin neck, thin neck diameter is at 2-6mm, and length is at 30-60mm;
(5) expand shoulder: expand shoulder process, by the actual single crystal diameter recorded, regulate the output rating of radio-frequency generator and the downstream rate of polycrystal; As shown in Figure 1, 2, single crystal diameter=[(polycrystal diameter
2× polycrystal downstream rate)/monocrystalline downstream rate]
1/2; Radio-frequency generator output rating and single crystal diameter linear.
(6) maintenance, isodiametric growth: when expansion shoulder diameter is greater than 8 inches, monocrystalline keeps, and starts isodiametric growth, in Crystal fsometric Growing process, the speed of rotation of polycrystal is 0.1-1 rev/min, and single crystal growing speed is at 1.5-2.5mm/min, and monocrystalline speed of rotation is 6-25 rev/min;
(7) finish up: when monocrystalline is pulled to polycrystal afterbody, start to finish up, reduce silicon single-crystal diameter gradually, when reaching desired value when finishing up to single crystal diameter, melting zone is pulled open, at this moment the lower shaft of zone melting furnace hauls monocrystalline and continues to move downward, and upper axle changes with polycrystal and moves upward, and closes argon gas;
(8) lower the temperature, tear prepurging open: carry out slow cooling to crystal, cooling duration is 50-90min, after having redness to become black, tears prepurging open to crystal afterbody.
This patent is in implementation process, and under effectively solving original method and processing condition, major diameter polycrystal fusing difficulty, easily causes the problem of windrow, process repeatability is poor, easily produces the problem such as easy to crack in dislocation, keep-process in expansion shoulder process.Under original processing condition, diameter cannot melt smoothly more than the polycrystal of 135mm and flow down from district's fuse circle, cannot pulling monocrystal, monocrystalline produces dislocation and causes the ratio of crystal pulling failure to account for 92% of total frequency of failure in expansion shoulder process, after have employed growth method of the present invention, this ratio is reduced to 57%, has greatly reduced to expand and produce dislocation in shoulder process and the ratio that causes crystal pulling failure.
Above one embodiment of the present of invention have been described in detail, but described content being only preferred embodiment of the present invention, can not being considered to for limiting practical range of the present invention.All equalizations done according to the present patent application scope change and improve, and all should still belong within patent covering scope of the present invention.
Claims (6)
1. a growth method for large diameter zone melting silicon single crystal, is characterized in that, utilizes zone melting single-crystal stove to carry out following operation:
(1) shove charge: by crystal clamper in the polycrystalline bar loading area smelting furnace after cleaning corrosion, seed crystal is loaded on seed crystal fixed chuck;
(2) find time, inflate, preheating: preheating ring is put in below polycrystalline bar, above district's fuse circle, closes fire door and vacuumize, after pour argon gas, when furnace pressure reaches 2.6-6.5bar, stop fast aeration, use instead and inflate at a slow speed, open drain tap and carry out stream argon; After inflation, preheating is carried out to polycrystalline bar;
(3) material, seeding: withdrawn from by preheating ring, carries out material, after polycrystal fusing, seed crystal and molten silicon is carried out welding, carries out shaping, seeding after welding to melting zone;
(4) grow thin neck: after seeding terminates, carry out the growth of thin neck, thin neck diameter is at 2-6mm, and length is at 30-60mm;
(5) expand shoulder: expand shoulder process, by the actual single crystal diameter recorded, regulate the output rating of radio-frequency generator and the downstream rate of polycrystal;
(6) maintenance, isodiametric growth: when expanding shoulder diameter and being greater than required diameter, monocrystalline keeps, and starts isodiametric growth, in Crystal fsometric Growing process, the speed of rotation of polycrystal is 0.1-1 rev/min, and single crystal growing speed is at 1.5-2.5mm/min, and monocrystalline speed of rotation is 6-25 rev/min;
(7) finish up: when monocrystalline is pulled to polycrystal afterbody, start to finish up, reduce silicon single-crystal diameter gradually, when reaching desired value when finishing up to single crystal diameter, melting zone is pulled open, at this moment the lower shaft of zone melting furnace hauls monocrystalline and continues to move downward, and upper axle changes with polycrystal and moves upward, and closes argon gas;
(8) lower the temperature, tear prepurging open: slow cooling is carried out to crystal, after having redness to become black to crystal afterbody, tear prepurging open.
2. growth method according to claim 1, is characterized in that: the diameter of the polycrystalline bar in described step (1) is 145-175mm.
3. growth method according to claim 1, is characterized in that: in described step (2) stage stove, the output frequency of radio-frequency generator is 2-4MHz.
4. growth method according to claim 1, is characterized in that: described step (5) expands in shoulder process, and the pass of single crystal diameter and radio-frequency generator output rating and polycrystal downstream rate is: single crystal diameter=[(polycrystal diameter
2× polycrystal downstream rate)/monocrystalline downstream rate]
1/2; Radio-frequency generator output rating and single crystal diameter linear.
5. growth method according to claim 1, is characterized in that: when in described step (6), expansion shoulder diameter is greater than 8 inches, monocrystalline keeps, and starts isodiametric growth.
6. growth method according to claim 1: it is characterized in that: the cooling duration in described step (8) is 50-90min.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410523050.8A CN104328482A (en) | 2014-09-30 | 2014-09-30 | Growing method of large diameter float zone silicon crystal |
| PCT/CN2014/088600 WO2016049947A1 (en) | 2014-09-30 | 2014-10-15 | Method for growing large diameter float zone silicon monocrystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410523050.8A CN104328482A (en) | 2014-09-30 | 2014-09-30 | Growing method of large diameter float zone silicon crystal |
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| CN104328482A true CN104328482A (en) | 2015-02-04 |
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| CN201410523050.8A Pending CN104328482A (en) | 2014-09-30 | 2014-09-30 | Growing method of large diameter float zone silicon crystal |
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| WO (1) | WO2016049947A1 (en) |
Cited By (6)
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| CN107002276A (en) * | 2015-10-26 | 2017-08-01 | 北京京运通科技股份有限公司 | Melt the automatic growth method and system of crystal in area |
| CN107366017A (en) * | 2017-09-04 | 2017-11-21 | 青海鑫诺光电科技有限公司 | A kind of monocrystalline silicon ending equipment and its application method |
| CN109252209A (en) * | 2018-07-26 | 2019-01-22 | 天津中环领先材料技术有限公司 | A method of improving zone-melted silicon single crystal polycrystalline bar utilization rate |
| CN109440183A (en) * | 2018-12-20 | 2019-03-08 | 天津中环领先材料技术有限公司 | Optimized large-diameter zone-melting silicon single crystal ending method |
| CN110318096A (en) * | 2019-06-28 | 2019-10-11 | 北京天能运通晶体技术有限公司 | Zone-melted silicon single crystal ending method and drawing method |
| CN112195507A (en) * | 2020-09-28 | 2021-01-08 | 湖南稀土金属材料研究院 | Method for preparing rare earth metal single crystal |
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| CN113668045A (en) * | 2021-08-24 | 2021-11-19 | 包头美科硅能源有限公司 | Device and method for preparing monocrystalline silicon by directly using granular silicon in zone-melting method |
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Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6059875A (en) * | 1999-01-11 | 2000-05-09 | Seh America, Inc. | Method of effecting nitrogen doping in Czochralski grown silicon crystal |
| CN1325700C (en) * | 2006-04-21 | 2007-07-11 | 天津市环欧半导体材料技术有限公司 | Large-diameter zone-melting silicon single crystal growth method |
| CN1325701C (en) * | 2006-04-26 | 2007-07-11 | 天津市环欧半导体材料技术有限公司 | Process for preparing vapor pre-doping and neutron irradiation doping combined zone-melted silicon single crystal |
| JP2011157239A (en) * | 2010-02-03 | 2011-08-18 | Toyota Motor Corp | Method for manufacturing silicon single crystal, and ingot of silicon single crystal |
| CN101845667A (en) * | 2010-06-30 | 2010-09-29 | 峨嵋半导体材料研究所 | Method for producing high-resistivity monocrystalline silicon |
-
2014
- 2014-09-30 CN CN201410523050.8A patent/CN104328482A/en active Pending
- 2014-10-15 WO PCT/CN2014/088600 patent/WO2016049947A1/en active Application Filing
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| CN107002276A (en) * | 2015-10-26 | 2017-08-01 | 北京京运通科技股份有限公司 | Melt the automatic growth method and system of crystal in area |
| CN107002276B (en) * | 2015-10-26 | 2020-03-20 | 北京京运通科技股份有限公司 | Automatic growth method and system of zone-melting crystal |
| CN107366017A (en) * | 2017-09-04 | 2017-11-21 | 青海鑫诺光电科技有限公司 | A kind of monocrystalline silicon ending equipment and its application method |
| CN109252209A (en) * | 2018-07-26 | 2019-01-22 | 天津中环领先材料技术有限公司 | A method of improving zone-melted silicon single crystal polycrystalline bar utilization rate |
| CN109440183A (en) * | 2018-12-20 | 2019-03-08 | 天津中环领先材料技术有限公司 | Optimized large-diameter zone-melting silicon single crystal ending method |
| CN109440183B (en) * | 2018-12-20 | 2020-11-13 | 天津中环领先材料技术有限公司 | Optimized large-diameter zone-melting silicon single crystal ending method |
| CN110318096A (en) * | 2019-06-28 | 2019-10-11 | 北京天能运通晶体技术有限公司 | Zone-melted silicon single crystal ending method and drawing method |
| CN112195507A (en) * | 2020-09-28 | 2021-01-08 | 湖南稀土金属材料研究院 | Method for preparing rare earth metal single crystal |
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| WO2016049947A1 (en) | 2016-04-07 |
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Application publication date: 20150204 |