CN1490436A - Silicon seed crystal holder for monocrystal silicon by vertical pulling process - Google Patents

Silicon seed crystal holder for monocrystal silicon by vertical pulling process Download PDF

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Publication number
CN1490436A
CN1490436A CNA021311854A CN02131185A CN1490436A CN 1490436 A CN1490436 A CN 1490436A CN A021311854 A CNA021311854 A CN A021311854A CN 02131185 A CN02131185 A CN 02131185A CN 1490436 A CN1490436 A CN 1490436A
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China
Prior art keywords
hole
clamper
silicon seed
silicon
seed
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CNA021311854A
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Chinese (zh)
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CN1200148C (en
Inventor
屠海令
戴小林
吴志强
周旗钢
张果虎
万关良
王学锋
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Youyan Semiconductor Silicon Materials Co ltd
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Beijing General Research Institute for Non Ferrous Metals
Grinm Semiconductor Materials Co Ltd
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Priority to CN 02131185 priority Critical patent/CN1200148C/en
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Publication of CN1200148C publication Critical patent/CN1200148C/en
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Abstract

A clamper of silicon seel crystal for growing the monocrystalline silicon by straight pull method has a top jointer for connecting the seed crystal axle, and a main body which is composed of an upper part and a lower part containing a through empty cavity with big diameter for upper half and small diameter for lower half. It can be used to prepare the silicon crystal with 500 kg in weight. Its advantage is high safety of silicon seed crystal which can not be broken.

Description

A kind of silicon seed crystal holder for monocrystal silicon by vertical pulling process
Technical field
The present invention relates to a kind of silicon seed crystal holder for monocrystal silicon by vertical pulling process.
Background technology
Silicon single crystal generally is used to make unicircuit and other electron component as a kind of semiconductor material.Most semiconductor silicon single crystal body adopts the vertical pulling method manufacturing, and vertical pulling method is made the single crystal growing furnace diagrammatic cross-section of silicon single-crystal and seen accompanying drawing 1.In the method for growing silicon single crystal that vertical pulling method is made; silicon crystal is grown in the growth room; the growth room comprises stainless steel cylinder 8; heat-preservation cylinder 7; graphite heater 6; quartz crucible 11; the quartz crucible supporting apparatus 10 of graphite system etc.; silicon crystal is done shielding gas with the rare gas element argon gas when growth; the following manufacture method of general employing: polysilicon is put in the quartz crucible 11; heat fused; then; to melt silicon and slightly do cooling; give certain condensate depression; the silicon single crystal 1 (being called seed crystal) of a particular crystal orientation is packed in the silicon seed clamper 13; the upper end of silicon seed clamper 13 is connected with seed shaft 12 by web member; seed crystal is fixed in the lower end of clamper 13, and seed crystal 1 is contacted with silicon melt 3, by the temperature of adjusting melt and the pulling speed that seed crystal makes progress; seed body is grown up; when the diameter of silicon crystal 2 during near aimed dia, improve pulling speed, make the nearly permanent growth in thickness of single crystal.In the last stage of process of growth, silicon melt 3 not completely dissolve as yet in the quartz crucible 11, by increasing the heat supplied in crystalline pulling speed and the quartzy crucible of adjustment, crystal is reduced gradually, thereby form a tail shape cone, when sharp enough hour of cone, crystal will break away from melt, thereby finished the crystalline process of growth.
In the czochralski silicon monocrystal manufacturing processed, need a kind of silicon single crystal that particular crystal orientation is arranged, be commonly referred to seed crystal.It is by the cutting of the silicon single-crystal in certain crystal orientation or drills through and form.Crystal orientation commonly used is<100 〉,<111,<110,<511 etc.Seed crystal is generally right cylinder or rectangular parallelepiped, and one or more breach are arranged above it, with pin or wire seed crystal is fixed in the workpiece that is called the silicon seed clamper.
In the czochralski silicon monocrystal manufacturing processed, the silicon seed clamper is essential parts, seed crystal need be fixed in the silicon seed clamper well, guarantee that seed crystal is unlikely to come off in promoting the seed crystal process, silicon seed clamper lower end structure the silicon monocrystal growth process finished smoothly, so will match with the shape of the silicon seed of clamping.In general, the silicon seed clamper is made by metal molybdenum material or graphite, and a connecting parts that connects with seed shaft is arranged, and silicon seed clamper lower end can be used for fixedly silicon seed, and its shape basis is different and different with the shape of the silicon seed of clamping.
Present domestic seed crystal generally adopts rectangular parallelepiped, one side has a plurality of breach in the upper end of rectangular parallelepiped, silicon seed clamper 13 lower ends are the cylinder that a vertical breach is arranged, shape matches with the rectangular parallelepiped seed crystal, seed crystal 1 half is embedded in the lower end of clamper 13, with metal molybdenum filament 15 the two is fixed together, molybdenum filament 15 just in time enters in the breach of seed crystal 1, plays the fixedly effect of seed crystal 1.Domestic seed crystal and silicon seed clamper synoptic diagram are seen accompanying drawing 2.This kind clamper is fit to make the silicon crystal of minor diameter, generally can only make diameter less than 160 millimeters, and weight is no more than the silicon crystal of 60Kg.When seed crystal is used to make crystal greater than this scope, just, reduce access times easily in the gap portions fracture of seed crystal, increase cost.Because metal molybdenum is different with the coefficient of expansion of silicon, after repeatedly using, cause molybdenum filament loosening easily simultaneously, make seed crystal fall into melt, cause the preparation process failure.
The external right cylinder that is shaped as that also has a kind of seed crystal that adopts, a cylindrical side is fluted, the right cylinder that is shaped as hollow of silicon seed clamper 13 lower ends, hole with metal molybdenum pin 14 identical sizes is wherein also arranged, can pack into the lower end of clamper 13 of right cylinder seed crystal 1, the groove of seed crystal 1 is relative with the clamper lateral orifices, and metal molybdenum pin 14 inserts in the hole, and plays the fixedly effect of seed crystal 1.External seed crystal and silicon seed clamper synoptic diagram are seen accompanying drawing 3.This kind clamper also only is fit to make the silicon crystal of minor diameter, generally can make diameter less than 160 millimeters, and weight is no more than the silicon crystal of 60Kg.When making large diameter crystal, or after repeatedly using, seed crystal also easily in the fracture of porose place, makes seed crystal fall into melt, equally also causes the preparation process failure.
The development of semiconductor silicon material is very fast now, and crystal develops to major diameter, high weight direction gradually, and diameter has been increased to 450 millimeters, and weight also surpasses 250Kg.In this case, present existing seed crystal and clamping device thereof can not meet the demands, and also dangerous, seed crystal ruptures easily, in order to reduce this situation, generally adopt every seed crystal only to use 1~5 crystal growth, have so just increased manufacturing cost.In order to satisfy and promote the development of silicon materials, need design a kind of major diameter crystalline silicon seed clamper that is suitable for preparing.
Summary of the invention
The object of the present invention is to provide a kind of vertical pulling method to prepare the used silicon seed clamper of silicon single-crystal, this invention has overcome above-mentioned shortcoming, can guarantee the safe handling of silicon seed, avoids the silicon seed fracture, can be used to prepare the silicon crystal of weight up to 500Kg.
To achieve these goals, silicon seed clamper of the present invention 13 upper ends are a connecting parts 13c who is connected with seed shaft 12, it is characterized in that described silicon seed clamper 13 lower ends comprise silicon seed clamper top 13a and silicon seed clamper bottom 13b, for detachably to connect, described silicon seed clamper bottom 13b includes the cavity of a up big and down small and up/down perforation between described silicon seed clamper top 13a and the described silicon seed clamper bottom 13b.
The cavity of described silicon seed clamper bottom 13b includes the shape hole of falling from power at least, or is two the stair-stepping post of one-tenth holes, and the described shape hole of falling from power is rounding platform hole or chamfered edge platform hole, and described post hole is cylindrical hole or prismatic hole.
The cavity of described silicon seed clamper bottom 13b also has a post hole below the shape hole of falling from power except that the shape hole of falling from power is arranged, or a post hole is arranged above the shape hole of falling from power, or at the shape hole upper and lower of falling from power one post hole is arranged respectively.
The limit number in described prismatic hole or chamfered edge platform hole is 3~16, and preferred limit number is 4~10.
The side in described chamfered edge platform hole or rounding platform hole and the angle theta between the vertical line are 10 °~<90 °, and preferred θ is 10 °~60 °.
The cavity of described silicon seed clamper bottom 13b respectively is wherein a kind of of a rounding platform hole and a cylindrical hole, a chamfered edge platform hole and a prismatic hole, a cylindrical hole and a rounding platform hole and a cylindrical hole, a prismatic hole and a chamfered edge platform hole and a prismatic hole, a rounding platform hole, a chamfered edge platform hole, two stepped cylindrical holes or two stepped prismatic holes etc.
The connecting parts 13c that described clamper is connected with seed shaft 12 can be thread connection or pin connects, and can be thread connection or sell between described clamper top 13a and the described clamper bottom 13b to connect.
The present invention to the outer shape of described clamper top 13a and bottom 13b without limits.Can be wherein a kind of of the molectron of right cylinder, prism, round platform and cylinder or terrace with edge and prismatical molectron etc.
Described silicon seed clamper is made by metal molybdenum or graphite.
Described silicon seed clamper is in order to satisfy the requirement of silicon seed shape, make seed crystal can inlay card at clamper bottom 13b, to bear the weight of the silicon single-crystal of constantly growing up.
The silicon seed of clamper clamping of the present invention comprises silicon seed top 1a and the silicon seed bottom 1b that is connected as a single entity, wherein said silicon seed top 1a is a kind of in rounding platform, chamfered edge platform or the cylinder, described silicon seed bottom 1b is a cylinder, when described silicon seed top 1a was cylinder, the cross section of described silicon seed top 1a cylinder was greater than the cross section of described silicon seed bottom 1b cylinder.Described cylinder is right cylinder or prism.
The limit number of described prism or chamfered edge platform is 3~16, and preferred limit number is 4~10.
The side of described silicon seed top 1 a rounding platform or chamfered edge platform is 10 °~<90 ° with the angle theta of axle, and preferred angle theta is 10 °~60 °.
In order to improve the intensity of seed crystal, also have a cylinder 1c at the top of seed crystal 1a, cylinder 1c be right cylinder or prism.The limit number of described prism is 3~16, and preferred limit number is 4~10.This moment, silicon seed was made up of three different cylinders of cross section that are connected as a single entity.
Between clamper of the present invention top 13a and the described clamper bottom 13b for detachably to connect, therefore when described silicon seed is used at crystal for straight drawing monocrystal growth, earlier described clamper top 13a and described clamper bottom 13b are disassembled, described clamper bottom 13b then packs described silicon seed into from above, again described clamper top 13a is connected with described clamper bottom 13b, silicon seed just is fixed in the described clamper like this, can be used for the growth of the silicon single-crystal of large volume, high weight.
Described silicon seed is used for the growth of crystal for straight drawing monocrystal; silicon single-crystal is grown in the growth room; when growth, do shielding gas with the rare gas element argon gas; earlier quartz crucible 11 is put into the quartz crucible supporting apparatus 10 of graphite system; polysilicon is put into quartz crucible 11; the described silicon seed 1 silicon seed clamper bottom 13b that packs into; clamper top 13a connects with clamper bottom 13b; clamper 13 is fixing with seed shaft 12 again; the furnace chamber that closes, and vacuumize, heating makes the silicon fusing then; after silicon melts fully, progressively reduce the temperature of molten silicon near the silicon fusing point.Quartz crucible 11 is being rotated under the drive of seed shaft 12 with silicon seed clamper 13 under the drive of graphite axis 9, silicon seed 1 is slowly descended, and contact with molten silicon, upwards promote seed crystal with certain speed then, the purpose of this process mainly is to eliminate the dislocation defects that forms because of thermal shocking in the seed crystal.When treating that seed crystal rises to certain-length, pulling speed is slowed down, slightly reduce the temperature of melt simultaneously, make the seed crystal enlarged diameter, when the seed crystal diameter increases to than low approximately 10 millimeter of aimed dia, increase pulling speed, make crystal be close to the equal diameter growth.Store the silicon material not for a long time in quartz crucible 11, improve pulling speed again, suitably increase the power of heating simultaneously, make crystal diameter be changed to a back taper, when boring point enough hour, it can break away from silicon melt, and at this moment the crystalline process of growth finishes.When being cooled to be close to room temperature, crystal can be taken off in crystal.
The present invention has designed the silicon seed clamper of special shape, can satisfy the development need of semiconductor silicon material, can be used for making the preparation of the semiconductor grade silicon single-crystal of unicircuit and other electron component.Adopt silicon seed clamper of the present invention can prolong the work-ing life of seed crystal greatly, the silicon seed access times are reached more than 40 times, reduce the tooling cost of silicon crystal, the silicon crystal weight of producing is during up to 500Kg, can guarantee the safe handling of silicon seed, avoid the silicon seed fracture, can be used to prepare the silicon crystal of weight up to 500Kg.
Description of drawings
Figure 1 shows that the single crystal growing furnace diagrammatic cross-section of vertical pulling method manufacturing silicon single-crystal
Figure 2 shows that existing domestic seed crystal and silicon seed clamper synoptic diagram
Figure 3 shows that existing external seed crystal and silicon seed clamper synoptic diagram
Figure 4 shows that silicon seed clamper sectional view of the present invention
Figure 5 shows that silicon seed clamper of the present invention and seed crystal synoptic diagram
Figure 6 shows that silicon seed clamper of the present invention bottom sectional view
Figure 7 shows that another silicon seed clamper bottom sectional view of the present invention
Figure 8 shows that the another silicon seed clamper of the present invention bottom sectional view
Figure 9 shows that another silicon seed clamper bottom sectional view of the present invention
Among the figure, 1 is silicon seed, the 2nd, and silicon single crystal bar, the 3rd, silicon melt, the 4th, loam cake, the 5th, carbon lagging material, the 6th, graphite heater, the 7th, heat-preservation cylinder, the 8th, stainless steel cylinder, the 9th, graphite axis, the 10th, the quartz crucible supporting apparatus of graphite system, the 11st, quartz crucible, the 12nd, seed shaft, the 13rd, clamper, 13a are clamper top, 13b is the clamper bottom, 13c is the clamper connecting parts, the 14th, and molybdenum pin, the 15th, molybdenum filament, 1a is silicon seed top, and 1b is the silicon seed bottom, and 1c is the cylinder that add on silicon seed top.
Embodiment
Below be embodiments of the invention, the embodiment that the present invention provides is in order to further specify the specific embodiments of the invention scheme, rather than is used for limiting protection scope of the present invention.
Embodiment 1
Figure 4 shows that the sectional view of silicon seed clamper of the present invention.Clamper top 13a, clamper bottom 13b that silicon seed clamper of the present invention comprises a connecting parts 13c who is connected with seed shaft 12, is connected as a single entity with connecting parts, described clamper bottom 13b one contains the right cylinder of the cavity of up big and down small and up/down perforation, and described clamper top 13a is a right cylinder.
Between described clamper top 13a and the described clamper bottom 13b is thread connection, and the connecting parts 13c that described clamper is connected with seed shaft 12 is that pin connects, and connecting parts 13c is a pair of ear structure.
The cavity of described clamper bottom 13b is a rounding platform hole and a cylindrical hole, and the side in rounding platform hole is 15 ° with the angle theta of axle.
Figure 5 shows that silicon seed clamper of the present invention and seed crystal synoptic diagram.Described clamper top 13a and described clamper bottom 13b disassemble, the seed crystal 1 silicon seed clamper bottom 13b that packs into, and seed crystal 1 shape of the cavity shape of described clamper bottom 13b and clamping is complementary, and plays clamping and the fixedly effect of seed crystal.
Figure 6 shows that the sectional view of silicon seed clamper bottom 13b of the present invention.The cavity of clamper bottom 13b is a rounding platform hole and a cylindrical hole, and the side in rounding platform hole is 15 ° with the angle theta of axle, and silicon seed clamper bottom 13b has a helicitic texture, and 13a connects with clamper top.
Embodiment 2
Figure 7 shows that another silicon seed clamper bottom 13b sectional view of the present invention.As different from Example 1, described clamper bottom 13b cavity is a rounding platform.
Embodiment 3
Figure 8 shows that the another silicon seed clamper of the present invention bottom 13b sectional view.As different from Example 1, described clamper bottom 13b cavity is two stair-stepping cylindrical holes, and the aperture of last cylindrical hole is greater than the aperture of following cylindrical hole.
Embodiment 4
As different from Example 1, for pin is connected, described clamper bottom 13b cavity is one to fall six terrace with edge holes and one or six prismatic holes between described clamper top 13a and the described clamper bottom 13b, and the angle theta of six terrace with edge hole sides and axle of falling is 60 °.
Embodiment 5
Figure 9 shows that another silicon seed clamper bottom 13b sectional view.
As different from Example 1, the cavity of described clamper bottom 13b is the hole of up big and down small and up/down perforation, is shaped as a cylindrical hole, a rounding platform hole and a cylindrical hole.
Embodiment 6
As different from Example 3, described clamper bottom 13b cavity is for falling six terrace with edge holes and six prismatic holes.
Embodiment 7
As different from Example 5, the cavity shape of described clamper bottom 13b is respectively a prismatic hole, a chamfered edge platform hole and a prismatic hole, and the limit number in terrace with edge hole and prismatic hole is 8, and the terrace with edge side is 75 ° with the angle theta of axle.
The silicon seed clamper that the present invention designs can guarantee that seed crystal itself can not rupture in silicon crystal weight during up to 500Kg.Silicon seed can use repeatedly like this, prolongs the work-ing life of seed crystal greatly, reduces the tooling cost of silicon crystal.Can be used to make the preparation of the semiconductor grade silicon single-crystal of unicircuit and other electron component, satisfy the development need of semiconductor silicon material.

Claims (11)

1. silicon seed crystal holder for monocrystal silicon by vertical pulling process, described silicon seed clamper (13) upper end is a connecting parts (13c) that is connected with seed shaft (12), it is characterized in that described silicon seed clamper (13) lower end comprises silicon seed clamper top (13a) and seedholder bottom (13b), for detachably to connect, described silicon seed clamper bottom (13b) includes the cavity of a up big and down small and up/down perforation between described silicon seed clamper top (13a) and the described silicon seed clamper bottom (13b).
2. silicon seed clamper according to claim 1, the cavity that it is characterized in that described silicon seed clamper bottom (13b) is for including the shape hole of falling from power at least, or be two the stair-stepping post of one-tenth holes, the described shape hole of falling from power is rounding platform hole or chamfered edge platform hole, and described post hole is cylindrical hole or prismatic hole.
3. silicon seed clamper according to claim 2, the cavity that it is characterized in that described silicon seed clamper bottom (13b) is except that having the shape hole of falling from power, one post hole is also arranged below the shape hole of falling from power, or a post hole is arranged above the shape hole of falling from power, or one post hole is respectively arranged at the shape hole upper and lower of falling from power.
4. silicon seed clamper according to claim 2 is characterized in that the limit number in described prismatic hole or chamfered edge platform hole is 3~16.Preferred limit number is 4~10.
5. silicon seed clamper according to claim 4 is characterized in that the limit number in described prismatic hole or chamfered edge platform hole is 4~10.
6. silicon seed clamper according to claim 2 is characterized in that the side in described chamfered edge platform hole or rounding platform hole and the angle theta between the vertical line are 10 °~<90 °.
7. silicon seed clamper according to claim 6 is characterized in that the side in described chamfered edge platform hole or rounding platform hole and the angle theta between the vertical line are 10 °~60 °.
8. silicon seed clamper according to claim 1, the cavity that it is characterized in that described silicon seed clamper bottom (13b) respectively are wherein a kind of of a rounding platform hole and a cylindrical hole, a chamfered edge platform hole and a prismatic hole, a cylindrical hole and a rounding platform hole and a cylindrical hole, a prismatic hole and a chamfered edge platform hole and a prismatic hole, a rounding platform hole, a chamfered edge platform hole, two stepped cylindrical holes or two stepped prismatic holes.
9. silicon seed clamper according to claim 1, it is characterized in that connecting parts (13c) that described clamper is connected with seed shaft (12) can be thread connection or pin connects, can be thread connection or sell between described clamper top (13a) and the described clamper bottom (13b) and connect.
10. silicon seed clamper according to claim 1, the profile that it is characterized in that described clamper top (13a) and described clamper bottom (13b) are wherein a kind of of the molectron of right cylinder, prism, round platform and cylinder or terrace with edge and prismatical molectron.
11. silicon seed clamper according to claim 1 is characterized in that described silicon seed clamper made by metal molybdenum or graphite.
CN 02131185 2002-10-15 2002-10-15 Silicon seed crystal holder for monocrystal silicon by vertical pulling process Expired - Lifetime CN1200148C (en)

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CN1200148C CN1200148C (en) 2005-05-04

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101781792A (en) * 2009-12-23 2010-07-21 常州亿晶光电科技有限公司 Crystal clamp part for broaching silicon rod
CN102051681A (en) * 2010-12-31 2011-05-11 镇江荣德新能源科技有限公司 Seed crystal for preparing single crystal silicon
CN102492983A (en) * 2011-12-22 2012-06-13 浙江金瑞泓科技股份有限公司 Seed chuck used for growth of czochralski silicon single-crystal
CN102628179A (en) * 2012-05-04 2012-08-08 杭州海纳半导体有限公司 Seed crystal holder for producing monocrystalline silicon by straight-pulling method and usage thereof
CN102660767A (en) * 2012-05-28 2012-09-12 哈尔滨工业大学 Cooling transitional joint for directional solidification equipment of electromagnetic cold crucible
CN103361716A (en) * 2012-04-06 2013-10-23 有研半导体材料股份有限公司 Seed crystal holder
CN110230093A (en) * 2019-07-10 2019-09-13 深圳市全普科技有限公司 A kind of seed crystal clamping pulling apparatus for monocrystalline silicon growing furnace
CN113463182A (en) * 2021-07-07 2021-10-01 西安奕斯伟硅片技术有限公司 Method for drawing silicon single crystal rod and silicon single crystal rod

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101781792A (en) * 2009-12-23 2010-07-21 常州亿晶光电科技有限公司 Crystal clamp part for broaching silicon rod
CN102051681A (en) * 2010-12-31 2011-05-11 镇江荣德新能源科技有限公司 Seed crystal for preparing single crystal silicon
CN102492983A (en) * 2011-12-22 2012-06-13 浙江金瑞泓科技股份有限公司 Seed chuck used for growth of czochralski silicon single-crystal
CN103361716A (en) * 2012-04-06 2013-10-23 有研半导体材料股份有限公司 Seed crystal holder
CN102628179A (en) * 2012-05-04 2012-08-08 杭州海纳半导体有限公司 Seed crystal holder for producing monocrystalline silicon by straight-pulling method and usage thereof
CN102628179B (en) * 2012-05-04 2015-12-16 杭州海纳半导体有限公司 Seedholder and the using method of silicon single crystal is prepared for vertical pulling method
CN102660767A (en) * 2012-05-28 2012-09-12 哈尔滨工业大学 Cooling transitional joint for directional solidification equipment of electromagnetic cold crucible
CN102660767B (en) * 2012-05-28 2015-06-10 哈尔滨工业大学 Cooling transitional joint for directional solidification equipment of electromagnetic cold crucible
CN110230093A (en) * 2019-07-10 2019-09-13 深圳市全普科技有限公司 A kind of seed crystal clamping pulling apparatus for monocrystalline silicon growing furnace
CN113463182A (en) * 2021-07-07 2021-10-01 西安奕斯伟硅片技术有限公司 Method for drawing silicon single crystal rod and silicon single crystal rod

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CI01 Publication of corrected invention patent application

Correction item: Patentee|Address

Correct: GRINM SEMICONDUCTOR MATERIALS Co.,Ltd.|101300 Beijing city Shunyi District Shuanghe Linhe Industrial Development Zone on the south side of the road

False: GRINM SEMICONDUCTOR MATERIALS Co.,Ltd.|101300 Beijing city Shunyi District Shuanghe Linhe Industrial Development Zone on the south side of the road

Number: 33

Volume: 31

ERR Gazette correction
CP01 Change in the name or title of a patent holder

Address after: 101300 south side of Shuanghe Road, Linhe Industrial Development Zone, Shunyi District, Beijing

Patentee after: Youyan semiconductor silicon materials Co.,Ltd.

Address before: 101300 south side of Shuanghe Road, Linhe Industrial Development Zone, Shunyi District, Beijing

Patentee before: GRINM SEMICONDUCTOR MATERIALS Co.,Ltd.

CP01 Change in the name or title of a patent holder
CX01 Expiry of patent term

Granted publication date: 20050504

CX01 Expiry of patent term