CN101363132A - Method of pulling up silicon single crystal - Google Patents

Method of pulling up silicon single crystal Download PDF

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Publication number
CN101363132A
CN101363132A CNA2008101459052A CN200810145905A CN101363132A CN 101363132 A CN101363132 A CN 101363132A CN A2008101459052 A CNA2008101459052 A CN A2008101459052A CN 200810145905 A CN200810145905 A CN 200810145905A CN 101363132 A CN101363132 A CN 101363132A
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neck
single crystal
footpath
aforementioned
pulling
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Inventor
南俊郎
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Coorstek KK
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Covalent Materials Corp
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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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/20Controlling or regulating
    • C30B15/22Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal
    • C30B15/24Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal using mechanical means, e.g. shaping guides
    • 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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/30Mechanisms for rotating or moving either the melt or the crystal
    • 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 method of pulling up a silicon single crystal in which a variation rate of a neck diameter is controlled to be within a predetermined range, and a dislocation in a neck is eliminated. When pulling up the silicon single crystal, a single crystal with a predetermined crystal diameter is grown by bringing a seed crystal into contact with a material silicon melt, pulling up the seed crystal, growing the neck, and then increasing a diameter. The above-mentioned neck diameter is increased and decreased to grow the neck, during which a neck diameter variation rate is greater than or equal to 0.05 and less than 0.5, assuming that a value obtained in such a manner that a neck diameter difference (A-B) between adjoining inflection points is divided by a neck length L between the above-mentioned inflection points P1 and P2 is the neck diameter variation rate.

Description

The method of pulling up of silicon single crystal
Technical field
The present invention relates to a kind of method of pulling up of silicon single crystal, this method adopts Czochralski method (the Magnetic field applied Czochralski Method method that applies magnetic field; Hereinafter referred to as the MCZ method).
Background technology
As the manufacture method of silicon single crystal, be extensive use of the CZ method and apply the MCZ method in magnetic field, this is owing to can obtain dislocation-free or lattice defect is few and bore is big, purity is high single crystal with comparalive ease.
When using CZ manufactured silicon single crystal, for example, in single crystal pulling apparatus as shown in Figure 2, in the hot-zone by well heater 7 and thermal insulator 8 heat tracings in chamber 9, the crystal seed 1 that will be made of silicon single crystal is with after the raw silicon liquations 5 of fillings in the quartz crucible 6 contact, slowly lift while making it rotation, after forming neck 2, crystal diameter is slowly increased form shoulder 3, form the vertical tube part of constant diameter then, form operation through these, be grown to silicon single crystal 4.
In above-mentioned CZ method, in the past, for the dislocation of getting rid of dislocation that crystal seed causes or being caused by thermal shocking when contacting with liquation, the neck of formation was very thin, about the about 3mm of diameter.
But, in recent years, highly integrated, the cost that is accompanied by semiconductor device reduces, the raising of production efficiency, in order to obtain bigbore wafer, need to make heavy weight silicon single crystal, the neck of such in the past path can not tolerate the big weight of single crystal rod, causes taking place Serious Accidents such as disrumpent feelings, that single crystal rod falls.
For these, for example, in the Japanese kokai publication hei 9-249482 communique (patent documentation 1), disclose and hanged down 1~12rpm when the speed of rotation of crystal seed forms than vertical tube part when neck is formed, thereby can suppress to follow the natural convection of crystal seed rotation, the shape of crystalline growth interface is protruded in lower end more, even neck is directly attenuated, also can get rid of dislocation.
In addition, in the TOHKEMY 2004-83320 communique (patent documentation 2), disclose by making neck form crucible speed of rotation in the operation below 1rpm, apply simultaneously the following magnetic field of 0.1 tesla in the horizontal direction, proceed to increase the footpath operation stop to apply this magnetic field during the stage, thereby can prevent dislocation.
And, in the Japanese kokai publication hei 7-300388 communique (patent documentation 3), 2.5~15 times of thickness of crystal seed the length that makes the necking section of successive taper in the crystal seed are disclosed are, the diameter that makes the necking section in the fixing approximately footpath of successive wherein is 0.09~0.9 times of crystal seed thickness, rangeability is below the 1mm, the length of this necking section is 200~600mm, applies 1000~5000 Gausses' horizontal magnetic field.
In addition, in the flat 11-199384 communique of Japanese Patent Application (patent documentation 4), disclose, directly changed quantitative change greatly more than the 0.5mm/mm, can suppress dislocation and take place by the neck that makes per unit length as the neck that makes shape thin in the middle of so-called that neck directly increases and decreases.
But described in above-mentioned patent documentation 1, when forming the less neck in crystal footpath about diameter 3~6mm, even under the situation that changes the crystallization rotation, the downward protrusion degree in crystalline growth interface can not become big yet.With regard to having the effect of getting rid of dislocation, would rather be by changing pull rate, but when forming the very thin neck in above-mentioned such footpath, by controlling downward protrusion degree, the effect of getting rid of dislocation is little.
In addition, as the method for above-mentioned patent documentation 2 records, if making the magneticstrength of horizontal magnetic field is below 0.1 tesla, then raw silicon liquation amount can not fully suppress natural convection and follow the melt temperature of natural convection to change for a long time.
In addition, in the method for above-mentioned patent documentation 3 records, the design necking section is effective to suppressing dislocation, but it is elongated to form operating time of above-mentioned long-neck portion, is unfavorable for practicality.In addition, necking section diameter variation amplitude is represented the concavo-convex amplitude on this surface, only viscous deformation from preventing that stress concentration from causing, and the viewpoint that obtains abundant intensity is represented.
In addition, in the method for above-mentioned patent documentation 4 records, if increase the variable quantity in neck footpath, then the thermograde of neck outside surface becomes big during necking down, and dislocation desity increases, and occurs dislocation on the contrary and is difficult to situation about eliminating.Particularly in the MCZ method, when the liquation convection current was suppressed, the regular variation that is called as the molten surface temperature of spoke pattern (spoke pattern) showed significantly, and the variable quantity in neck footpath becomes excessive, and it is very difficult that dislocation-freeization becomes.
Summary of the invention
The present invention is based on following discovery and finish: in order to remove the dislocation in the neck in early days, the solid-liquid interface of the monocrystalline that is lifted is protruded downwards, and the variation that makes the neck footpath effectively is in the specified conditions scope and grow into neck.
That is, the object of the present invention is to provide the method for pulling up of silicon single crystal, this method can suppress neck footpath velocity of variation within the limits prescribed in the growth of the silicon single crystal that uses the MCZ method, gets rid of the dislocation in the neck in early days.
The method of pulling up of silicon single crystal of the present invention, it is characterized in that: lift at silicon single crystal and (crystal seed is contacted and lifts with the raw silicon liquation, after growing into neck, increase the footpath and grow into regulation crystal single crystal directly) in, make aforementioned neck directly increase and decrease the growth of carrying out neck, at this moment, poor divided by the neck length between the aforementioned point of inflection with the neck footpath between the point of inflection (point of inflection) of the aforementioned neck footpath adjacency that increases and decreases, the value that obtains is during as neck footpath velocity of variation, and this velocity of variation is more than 0.05 and less than 0.5.
By suppressing the variation in neck footpath as mentioned above, grow into neck, thereby can get rid of dislocation in early days.
During the growth of aforementioned neck, preferably apply cusped magnetic field more than 100 Gausses at the crucible wall, making the crystallization speed of rotation is below the above 15rpm of 1rpm, is greater than 8rpm and below 15rpm in the crucible speed of rotation that rotates up with aforementioned crystallization phases negative side.
Perhaps in addition preferred, during aforementioned neck growth, apply the above horizontal magnetic field of 2000 Gausses, making the crystallization speed of rotation is below the above 15rpm of 1rpm, is below the above 3rpm of 0.5rpm in the crucible speed of rotation that rotates up with aforementioned crystallization phases negative side.
By the neck of under the applying condition of this magnetic field, growing, can suppress to influence the temperature variation in the neck long period directly, effectively suppress the variation in neck footpath.
As mentioned above,, in the growth of the silicon single crystal that uses the CZ method, can suppress the velocity of variation in neck footpath, get rid of the dislocation in the neck in early days according to the method for pulling up of silicon single crystal of the present invention.
Therefore,, can realize the shorteningization of neck operation,, also can realize the reduction of production time loss even when carrying out bad the doing over again of causing of neck according to method of pulling up of the present invention.
Description of drawings
Fig. 1 is the synoptic diagram of explanation neck footpath velocity of variation.
Fig. 2 is the sketch chart of monocrystalline silicon growing in the explanation single crystal pulling apparatus.
Embodiment
Below, the present invention will be described in more detail.
The method of pulling up of silicon single crystal of the present invention, it is characterized in that: crystal seed is contacted and lifts with the raw silicon liquation, after growing into neck, increase the footpath to grow into the single crystal in regulation crystal footpath, in this silicon single crystal lifts, make aforementioned neck directly increase and decrease the growth of carrying out neck, at this moment, neck footpath velocity of variation is more than 0.05 and less than 0.5.
Said neck footpath velocity of variation among the present invention is in the neck footpath of increase and decrease shown in Figure 1, with the point of inflection P1 of this neck footpath adjacency, between P2 increase neck footpath A with dwindle directly poor (A-B) value of obtaining divided by the neck length between aforementioned point of inflection P1, P2 directly of the neck between the B of neck.
When neck directly increased or reduces, maximum stress occurred in the neck periphery, and when it surpassed the boundary of dislocation inhibition, dislocation desity increased, and in neck, got rid of dislocation and became difficult.
Therefore, preferred neck is directly fixing, but in fact, because the temperature variation of raw silicon liquation, the variation in neck footpath can not be suppressed fully.
To this, in the present invention, by growing into neck,, thereby can get rid of dislocation in early days, interior dislocation-freeization of the short period of time possibility that becomes so that aforementioned neck footpath velocity of variation is 0.05 or more and less than 0.5.
In order to be suppressed at more than 0.05 aforementioned neck footpath velocity of variation and less than 0.5, the temperature variation that suppresses the raw silicon molten surface that neck contacted, the temperature variation that particularly influences the longer cycle in neck footpath is effective, do not apply in the CZ method or the single crystal pulling in the cusped magnetic field in magnetic field, it is effective increasing the crucible speed of rotation in the scope that can stablize pulling single crystal.
In addition, the liquation amount surpasses in the MCZ method of 100kg, between certain neck length, aforementioned neck footpath velocity of variation is controlled at less than 0.05, in fact is very difficult.
As mentioned above, influence the viewpoint of the temperature variation of neck longer cycle directly from inhibition, in order to control the thermal convection of raw silicon liquation, when aforementioned neck is grown, preferably apply magnetic field so that the cusped magnetic field in the sidewall of crucible more than 100 Gausses, at this moment, preferred crucible speed of rotation is greater than 8rpm and below 15rpm.
During cusped magnetic field less than 100 Gausses in the aforementioned sidewall of crucible, can not be suppressed the effect of liquation convection current fully.
In addition, aforementioned crucible speed of rotation is 8rpm when following, the low temperature part of raw silicon molten surface, and the zonal low temperature field that promptly is called as the spoke pattern becomes remarkable.If this low temperature part crosscut is as the neck growth part at silicon raw material molten surface center, then neck directly changes, and aforementioned neck footpath velocity of variation is maintained the difficulty that becomes below 0.5, and neck is too thick sometimes, and neck too carefully ruptures on the contrary sometimes.
On the other hand, when the crucible speed of rotation during the neck growth surpasses 15rpm, when shoulder after the neck growth and vertical tube part growth, in order to suppress oxygen concn, usually, the crucible speed of rotation is reduced to below the 10rpm, but this rapid speed of rotation change, generation convection current confusion makes crystallization occur dislocationization easily.
Perhaps in addition, the magnetic approach that aforementioned neck applies when growing also can be a horizontal magnetic field, at this moment, in order to make neck directly stable, and the temperature variation in the long period of inhibition raw silicon liquation, preferred magneticstrength is more than 2000 Gausses, and the crucible speed of rotation is below the above 3rpm of 0.5rpm.
During aforementioned magnetic field undercapacity 2000 Gausses, can not fully suppress the raw silicon liquation convection current that magnetic field causes, the low temperature part that generates on the direction parallel with magnetic field is sometimes with the crosscut of neck growth part, and neck directly changes, and is difficult to neck footpath velocity of variation is suppressed at below 1.0.
In addition, under the situation of horizontal magnetic field, when the crucible speed of rotation surpassed 3rpm, it is big that the temperature variation of raw silicon liquation becomes, and the neck footpath is unstable, and the growth of constant diameter portion (vertical tube part) is also unstable.Therefore, preferred crucible speed of rotation is little, but from the growth efficiency viewpoint of monocrystalline, is preferably more than the 0.5rpm.
In addition, with aforementioned crucible reverse direction on the crystalline speed of rotation of rotating, during arbitrary magnetic field in applying cusped magnetic field or horizontal magnetic field, from keeping the stable viewpoint in neck footpath, for getting final product more than the 1rpm.But, in the shoulder after the neck growth operation, the growth of vertical tube part,, need to reduce the crystallization rotation in order to suppress distortion, when aforementioned speed of rotation surpasses 15rpm, be accompanied by rapid condition and change, the possibility that dislocation occurs strengthens, and is not preferred therefore.
Embodiment
Below, further specifically describe the present invention based on embodiment, but the present invention is not limited to following embodiment.
[embodiment 1~6, comparative example 1~5]
In the quartz crucible of 24 inches of diameters, fill raw silicon liquation 100kg, use CZ method single crystal pulling apparatus, the growth neck grows into silicon single crystal then so that average neck directly is 4.5mm.
In neck when growth,, condition is respectively as the embodiment 1~6 of table 1 and the magnetic field as shown in the comparative example 1~5 applies and crucible speed of rotation, crystallization speed of rotation, single crystal pulling speed.
Measure maximum neck footpath velocity of variation respectively and get rid of from the growth starting position to dislocation after the length of position.
Sum up these and the results are shown in table 1.
In addition, the measured value of magneticstrength is the measured value of crucible wall under the situation of cusped magnetic field, is the measured value at center under the situation of horizontal magnetic field.The neck footpath is measured by vernier callipers.In addition, the length of the position after getting rid of to dislocation from the growth starting position is carried out the visual mensuration of dislocation and is judged by the etching evaluation (JIS H0609 benchmark) of selecting etching solution.
Table 1
Figure A200810145905D00081
As shown in Table 1, under the situation in the arbitrary magnetic field in applying cusped magnetic field or horizontal magnetic field,, can be suppressed at more than 0.05 neck footpath velocity of variation and less than 0.5, at this moment can confirm to get rid of in early days dislocation by under defined terms, lifting.

Claims (3)

1. the method for pulling up of a silicon single crystal, it is characterized in that: crystal seed is contacted and lifts with the raw silicon liquation, after growing into neck, increase the footpath to grow into the single crystal in regulation crystal footpath, in this silicon single crystal lifts, make aforementioned neck directly increase and decrease the growth of carrying out neck, at this moment, poor divided by the neck length between the aforementioned point of inflection with the neck footpath between the point of inflection of the aforementioned neck footpath adjacency of increase and decrease, the value that obtains is during as neck footpath velocity of variation, and aforementioned neck footpath velocity of variation is more than 0.05 and less than 0.5.
2. the method for pulling up of silicon single crystal according to claim 1, it is characterized in that: when aforementioned neck is grown, apply cusped magnetic field more than 100 Gausses at the crucible wall, making the crystallization speed of rotation is below the above 15rpm of 1rpm, in the crucible speed of rotation that rotates up with aforementioned crystallization phases negative side greater than 8rpm and below 15rpm.
3. the method for pulling up of silicon single crystal according to claim 1, it is characterized in that: when aforementioned neck is grown, apply the above horizontal magnetic field of 2000 Gausses, making the crystallization speed of rotation is below the above 15rpm of 1rpm, is below the above 3rpm of 0.5rpm in the crucible speed of rotation that rotates up with aforementioned crystallization phases negative side.
CNA2008101459052A 2007-08-07 2008-08-07 Method of pulling up silicon single crystal Pending CN101363132A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102220632A (en) * 2011-06-23 2011-10-19 英利能源(中国)有限公司 Technical method of N-type Czochralski silicon monocrystal
CN103290470A (en) * 2013-05-21 2013-09-11 杭州海纳半导体有限公司 Diameter transitional czochralski silicon growing method
CN105040099A (en) * 2014-04-21 2015-11-11 环球晶圆日本股份有限公司 Single crystal extraction method
CN108866621A (en) * 2017-05-16 2018-11-23 上海新昇半导体科技有限公司 A kind of silicon single crystal seeding structure and technique

Families Citing this family (2)

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Publication number Priority date Publication date Assignee Title
KR101458037B1 (en) * 2013-01-14 2014-11-04 주식회사 엘지실트론 Method and apparatus for manufacturing ingot having single crystals
KR102104072B1 (en) * 2018-01-19 2020-04-23 에스케이실트론 주식회사 Method and apparatus for silicon single crystal growth

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5578284A (en) * 1995-06-07 1996-11-26 Memc Electronic Materials, Inc. Silicon single crystal having eliminated dislocation in its neck
JP3598972B2 (en) * 2000-12-20 2004-12-08 三菱住友シリコン株式会社 Method for producing silicon single crystal
US6514337B2 (en) * 2001-02-07 2003-02-04 Seh America, Inc. Method of growing large-diameter dislocation-free<110> crystalline ingots
JP2007022864A (en) * 2005-07-19 2007-02-01 Sumco Corp Method for manufacturing silicon single crystal

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102220632A (en) * 2011-06-23 2011-10-19 英利能源(中国)有限公司 Technical method of N-type Czochralski silicon monocrystal
CN102220632B (en) * 2011-06-23 2012-12-12 英利能源(中国)有限公司 Technical method of N-type Czochralski silicon monocrystal
CN103290470A (en) * 2013-05-21 2013-09-11 杭州海纳半导体有限公司 Diameter transitional czochralski silicon growing method
CN103290470B (en) * 2013-05-21 2016-06-29 杭州海纳半导体有限公司 The pulling of silicon single crystal growing method of diameter transitions
CN105040099A (en) * 2014-04-21 2015-11-11 环球晶圆日本股份有限公司 Single crystal extraction method
CN105040099B (en) * 2014-04-21 2017-12-12 环球晶圆日本股份有限公司 Monocrystalline extracting method
CN108866621A (en) * 2017-05-16 2018-11-23 上海新昇半导体科技有限公司 A kind of silicon single crystal seeding structure and technique

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