CN105040099B - Monocrystalline extracting method - Google Patents
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Abstract
Shorten since being formed stretched portion to the extraction time that crystal is cut off from fused solution, monocrystalline is extracted in the case where not producing dislocation, improves yield rate.Including the 1st process, the 2nd process and the 3rd process, the 1st process forms stretched portion（C2）, the 2nd process is after foregoing 1st process, and in the final process that stretched portion is formed, lower convex form prominent downwards is formed in crystal lower end（C3）3rd process cuts off the foregoing lower convex form formed in foregoing 2nd process from foregoing silicon melt, in foregoing 2nd process, the magnetic flux density of horizontal magnetic field is controlled than foregoing 1st process to the scope in 800~1000 Gausses lower, crystal extraction rate is controlled than foregoing 1st process to the scope in 0.2~0.5mm/min lower, Crystal Rotation speed is controlled into scope in 1~3rpm lower than foregoing 1st process, by crucible rotation speed control 0.5~5rpm scope.
Description
Technical field
The present invention relates to basis to cut krousky crystal growth method（Hereinafter referred to as " CZ methods "）Culture monocrystalline extracts list simultaneously
Brilliant monocrystalline extracting method.
Background technology
On the culture of monocrystalline silicon, CZ methods are widely used.In the method, as shown in figure 4, by calciner 55
The heat of side heater 52 is in quartz glass crucibles 50（Hereinafter referred to only crucible 50）The interior fused solution M for forming silicon.Then, exist
In the range of surrounding is surrounded by emission shield 51, crystal seed P is contacted with fused solution M surface M1, rotate crucible 50,
And crystal seed P is rotated in the reverse direction while is extracted upward, thus form monocrystalline C in crystal seed P lower end.
Specifically, carry out melting the necking down of crystal seed P terminal part to form neck P1, it is from neck P1 that crystal is straight
Footpath, which expands, to form shoulder C1, also to be formed and will form the stretched portion C2 of product section.
Here, when stretched portion C2 reaches certain length, it is necessary to monocrystalline C is cut off from fused solution M, if in stretched portion C2
Cut off in the state of thick, then the bottom of the monocrystalline C after cutting off produces temperature change drastically, is produced in monocrystalline
Gliding dislocations, monocrystalline rate decline.
Therefore, following processes are carried out in the past：After stretched portion C2 is formed, the afterbody for slowly collapsing crystal diameter is formed,
In the state of monocrystalline C and melting liquid level M1 contact surface is fully reduced, monocrystalline C is cut off from melting liquid level M1.
But in the formation process of foregoing afterbody, activity time is longer, and cannot function as because crystal diameter is smaller
Product uses, and turns into the reason for yield rate is low.Therefore, shortening or omitting the afterbody formation process turns into problem.
For it is such the problem of, in Japanese Unexamined Patent Publication 2012-36042 publications, disclose following methods：Stretched portion shape
Cheng Hou, in the state of the lifting stopping of crucible is made, stop the extraction of monocrystalline silicon completely, will be contacted with the crystal of fused solution
End（Solid liquid interface）Downwards prominent lower convex form is integrally formed into long face after, cut off monocrystalline from fused solution.
That is, following methods are utilized：Although in stretched portion during C2 extraction, the shape of crystal lower end is prominent to crystal side
Convex shape, but by stopping extracting, crystal lower end flattens, afterwards, along direction growth prominent downwards.
The judgement of sufficient convex form whether is formed in crystal lower end, is the apparent weight for the monocrystalline that monitoring is cultured（From
The weight of monocrystalline silicon subtracts the buoyancy of fused solution）Change, based on weight change carry out.
According to such monocrystalline extracting method, the manufacture of monocrystalline can be shortened compared with implementing conventional afterbody formation process
Time.
But in monocrystalline extracting method disclosed in Japanese Unexamined Patent Publication 2012-36042 publications, for crystal lower end is formed
For lower convex form, it is necessary to stop the lifting of crucible, and the state for stopping crystal extraction is maintained into given time, so can not
With significantly shortening the time compared with implementing the situation of conventional afterbody formation process.
Further, since changed by the apparent weight for detecting monocrystalline to carry out whether forming appropriate convex in crystal lower end
The judgement of shape, if the precision of weight measure is relatively low, appropriate convex form can not be obtained, there is the danger that dislocation is produced in crystal
Danger.That is, in the case where the formation of convex form is insufficient, temperature change drastically is produced in crystal bottom, is had in monocrystalline
The danger of gliding dislocations is produced, in the case of in extremely sharp convex state, fused solution supercooling is so as to the danger in the presence of dislocation
Danger.
The content of the invention
The present invention is carried out in the previous case, and the purpose of invention is to provide a kind of monocrystalline extracting method, is cut in basis
Krousky crystal growth method from crucible extraction monocrystalline silicon monocrystalline extracting method in, can shorten since stretched portion formed to
Extraction time untill cutting off monocrystalline from fused solution, monocrystalline is extracted in the case where not producing dislocation, improve yield rate.
To solve foregoing problems, the monocrystalline extracting method for being related to the present invention forms silicon melt in crucible, to foregoing silicon
Fused solution applies horizontal magnetic field, and extracts monocrystalline silicon from foregoing silicon melt according to krousky crystal growth method is cut, and it is special
Sign is that the monocrystalline extracting method includes the 1st process, the 2nd process and the 3rd process, and the 1st process forms stretched portion, institute
The 2nd process is stated after foregoing 1st process, in the final process that stretched portion is formed, forms what is protruded downwards in crystal lower end
Lower convex form, the 3rd process cut off the foregoing lower convex form formed in foregoing 2nd process from foregoing silicon melt,
In foregoing 2nd process, crystal extraction rate is located at 0.2~0.5mm/min scope to cultivate crystal, by the magnetic of horizontal magnetic field
Flux density controls the scope in 800~1000 Gausses than foregoing 1st process lower, by Crystal Rotation speed than foregoing 1st work
Sequence controls the scope in 1~4rpm lower, by crucible rotation speed control 0.5~5rpm scope.
It is further preferred, that in foregoing 2nd process, crystal extraction rate is located to 0.3~0.5mm/min scope
To cultivate crystal, by Crystal Rotation speed control 1~3rpm scope, by crucible rotation speed control 0.5~3rpm's
Scope.
Moreover it is preferred that the length of the vertical of the lower convex form formed in foregoing crystal lower end is 10~30mm's
In the range of.
According to this method, in stretched portion forming process, it can be formed in crystal lower end and protruded downwards in a short time
Lower convex form.
As a result, monocrystalline can be cut off from fused solution in the case of indeformable not produce the state of dislocation, can
Significantly shorten the extraction time untill monocrystalline is cut off from fused solution since being formed stretched portion, improve yield rate.
According to the present invention, krousky crystal growth method is cut from the monocrystalline extracting method of crucible extraction monocrystalline silicon in basis
In, the extraction time untill monocrystalline is cut off from fused solution since being formed stretched portion can be shortened, dislocation can not produced
In the case of extract monocrystalline, improve yield rate.
Brief description of the drawings
Fig. 1 is the section view for representing to implement to be related to the partial structurtes of the monocrystalline extraction element of the monocrystalline extracting method of the present invention
Figure.
Fig. 2 is the flow chart of the flow of monocrystalline extracting method for representing to implement in Fig. 1 monocrystalline extraction element.
Fig. 3 is to represent to be formed in crystal lower end in stretched portion forming process according to the monocrystalline extracting method for being related to the present invention
Lower convex form length sectional view.
Fig. 4 is the sectional view for illustrating monocrystalline abstraction process.
Embodiment
Hereinafter, the embodiment for being related to the monocrystalline extracting method of the present invention is illustrated based on accompanying drawing.Fig. 1 is to represent real
Apply the sectional view of the partial structurtes for the monocrystalline extraction element for being related to the monocrystalline extracting method of the present invention.
The monocrystalline extraction element 1 possesses body of heater 10, and the body of heater 10 is overlappingly formed in columnar main chamber 10a top
There is concubine 10b, the monocrystalline extraction element 1 is also equipped with carbon pedestal（Or graphite base）2 and quartz glass crucibles 3（Only claim below
Make crucible 3）, the carbon pedestal（Or graphite base）2 can rotate around vertical axis and can set up and down in the body of heater 10
Put, the quartz glass crucibles 3（Hereinafter referred to only crucible 3）Kept by foregoing carbon pedestal 2.
Foregoing crucible 3 has the stretched portion 3a and bottom 3b that is formed under it, can be with the rotation of carbon pedestal 2 together around lead
The axle that hangs down rotates.
In addition, in the lower section of carbon pedestal 2, rotary driving part 14 and lifting drive division 15, the rotary driving part are provided with
14 be rotation motor for making the carbon pedestal 2 be rotated around vertical axis etc., and the lifting drive division 15 makes the lifting moving of carbon pedestal 2.
In addition, being connected with rotation driving control unit 14a on rotary driving part 14, liter is connected with lifting drive division 15
Drive control part 15a drops.
In addition, monocrystalline extraction element 1 possesses heater 4 and extraction mechanism 9, the heater 4 will fill by resistance heating
The raw semiconductor filled in crucible 3（Raw material polysilicon）Melt to form silicon melt M（Hereinafter referred to only fused solution M）, institute
State extraction mechanism 9 and roll wire rod 6, extract the monocrystalline C being cultured.It is provided with the end for the wire rod 6 that foregoing extraction mechanism 9 has
Crystal seed P.
In addition, the heater-driven control unit 4a of control delivery is connected with side heater 4, in extraction mechanism 9
On, be connected with carry out its rotation driving control rotation driving control unit 5a.
In addition, in the monocrystalline extraction element 1, it is provided with the outside of body of heater 2 and applies magnetic field magnet coil 8.When right
When the application magnetic field magnet coil 8 applies set electric current, apply given strength relative to the silicon melt M in crucible 3
Horizontal magnetic field.Applying the magnetic field solenoid controlled portion 8a on magnet coil 8, being connected with its action control of progress.
I.e., in the present embodiment, implement to cultivate the MCZ methods of monocrystalline to applying magnetic field in fused solution M（Magnetic control vertical pulling
Method）, silicon melt M convection current is thus controlled, realizes the stabilization of single crystallization.
In addition, in the top for the fused solution M being formed in crucible 3, the emission shield surrounded around monocrystalline C is configured with
7.The upper and lower part of the emission shield 7 forms opening, cover relative in culture it is monocrystalline C, from side heater 4
With fused solution M etc. unnecessary radiant heat, and by the air-flow rectification in stove.In addition, lower end and the melting of emission shield 7
Gap between liquid level is controlled as, and the desired characteristic of the corresponding monocrystalline to be cultivated, maintains set distance.
In addition, the monocrystalline extraction element 1 possesses the computer 11 with storage device 11a and operation control device 11b, rotation
Turn drive control part 14a, lifting drive control part 15a, solenoid controlled portion 8a, rotation driving control unit 9a to be connected to
Operation control device 11b.
In the monocrystalline extraction element 1 so formed, for example, in the case of culture diameter 300mm monocrystalline C, it is as follows
It is described to be extracted.That is, raw material polysilicon is loaded to crucible 3 first（Such as 350kg）, the storage device based on computer 11
The program stored in 11a starts crystal culture processes.
First, set gaseous environment is set as in body of heater 10（The predominantly gaseous environment of argon gas）, it is loaded in crucible 3
Raw material polysilicon be melted by the heating of side heater 4, turn into fused solution M.And then crucible 3 is in set height position
Put with set rotary speed（rpm）Carry out spinning movement.
Then, magnetic field is being applied with flowing through set electric current in magnet coil 8, to be set in 1000 in fused solution M
Magnetic flux density in the range of~4000 Gausses（Such as 3000 Gauss）Start to apply horizontal magnetic field.
In addition, wire rod 6 is lowered, crystal seed P is contacted with fused solution M, melt the necking down of crystal seed P terminal part, starts
Form neck P1（Fig. 2 step S1）.
When forming neck P1, using the delivery of counter-lateral quadrents heater 4, extraction rate, apply magnetic field intensity etc. as ginseng
Count to adjust extraction conditions, rotation crystal seed P is started with set rotary speed along the direction opposite with the direction of rotation of crucible 3.
Then, crystal diameter, which is gently expanded, to form shoulder C1, is transferred to be formed and will form the stretched of product section
Portion C2 the 1st process（Fig. 2 step S2）.
In stretched portion C2 formation, for example, extraction rate is controlled in 0.6~0.8mm/min scope, Crystal Rotation
Speed is controlled in 5~8rpm scope, and crucible rotation speed is controlled in 0.5~1rpm scope.By being set such
Monocrystalline extraction is carried out under fixed condition, diameter 300mm monocrystalline silicon can be cultivated to extract.In addition, during stretched portion C2 extraction
Crystal lower end shape is in the convex shape prominent to crystal side.
With the formation in monocrystalline silicon C stretched portion, the carbon pedestal 2 of storage crucible 3 is raised movement, maintains melting liquid level M1
The emission shield 7 fixed relative to position and the position of side heater 4.
In addition, suppressing fused solution M free convection by applying magnetic field, the magnetic flux density in the magnetic field is set at
The scope of 1000~4000 Gausses, more preferably it is set at 2000~3000 Gausses.
Then, when when stretched portion, C2 is formed into set length, be transferred to stretched portion formation final process, i.e., the 2nd
Process（Fig. 2 step S3）.In addition, the transfer to the 2nd process is preferably at the time of the curing degree of crystal is 0.7~0.85
Carry out.If in the scope of such curing degree, the remaining molten liquid after crystal extraction can be substantially ensured that, so can incite somebody to action
Raw material adds again（Reloading）To remaining molten liquid, crystal is extracted again.In addition, in the case where not making decrease in yield,
Crystal can be pulled away from while ensuring crystal being pulled away from required sufficient remaining molten liquid.
Then, in the 2nd process, crystal extraction rate continues the training of monocrystalline in 0.2~0.5mm/min scope
Support, more preferably crystal extraction rate continues the culture of monocrystalline, the magnetic of horizontal magnetic field in 0.3~0.5mm/min scope
Flux density is the scope of 800~1000 Gausses, and Crystal Rotation speed is 1~4rpm scope, more preferably drop to 1~
3rpm scope.And then crucible rotation speed changes to 0.5~5rpm scope, more preferably changes to 0.5~3rpm's
Scope.
Here, when being transferred to 2 process from the 1st process, if only the magnetic flux density of horizontal magnetic field is lower set in
The scope of 800~1000 Gausses, then fused solution M is unstable, is also easy to produce crystal modification, but due to adjustment crystal extraction rate, crystalline substance
The value of body rotary speed and crucible rotation speed, it is controlled in certain scope, so crystal modification can not occur.
By setting the value of each parameter in this wise, as shown in figure 3, monocrystalline C lower end shape（Extracted from foregoing stretched portion C2
When convex shape）It is changing into the lower convex form being recessed to fused solution M sides.Specifically, in the bowl-type do not rocked in interface
Shape.
Then, as shown in figure 3, in a short time, being formed in crystal lower end downward with more than 10mm below 30mm length
Just prominent lower convex form C3.In addition, the length h of foregoing lower convex form C3 vertical is that will melt liquid level M1 height
The germ nucleus axle CA's that is set in the case of the 0 and point of contact Pt of solid liquid interface（Negative direction）Highly.It is here, convex under foregoing
In the case that shape C3 length h is less than 10mm, the shape of crystal lower end is close to flat, so the contact area with fused solution M
Become big, become prone to produce dislocation.Foregoing lower convex form C3 length more than 30mm in the case of, fused solution M supercooling,
There is the danger for producing and misplacing before cutting off crystal from fused solution M.
Then, when forming foregoing lower convex form C3 in crystal lower end, it is transferred to the 3rd process（Fig. 2 step S4）.This
In 3 processes, foregoing lower convex form C3 and fused solution M contact area slowly reduces, by formed sufficiently lower convex form C3 come
Monocrystalline C and fused solution M are cut off.
As described above according to embodiments of the present invention are related to, in the stretched portion forming process of monocrystalline, in crystal lower end
Formed in the 2nd process of lower convex form prominent downwards, continue monocrystalline by 0.2~0.5mm/min of crystal extraction rate
Culture, at the same respectively the magnetic flux density in controlled level magnetic field 800~1000 Gausses scope, Crystal Rotation speed 1~
3rpm scope, scope of the crucible rotation speed in 0.5~5rpm.Thus, crystal necking down in a short time, formation are dashed forward downwards
The lower convex form gone out.
As a result, monocrystalline can be cut off from fused solution in the case of indeformable with the state of dislocation-free, significantly shorten
Extraction time since being formed stretched portion untill monocrystalline is cut off from fused solution, it is possible to increase yield rate.
In addition, the crystal manufactured according to the monocrystalline extracting method for being related to the present invention, can be used as such as FR（Focusing ring）With
Crystal use.
Embodiment
The monocrystalline extracting method for being related to the present invention is further detailed based on embodiment.In the present embodiment, make
Monocrystalline extraction is carried out with the monocrystalline extraction element represented in the foregoing embodiment, the crystal of extraction is verified.
Specifically, it is the 2nd process in the final process that stretched portion is formed after the 1st process in stretched portion is formed（Solidification
During rate 0.77）In, implement according to magnetic flux density, crystal extraction rate, Crystal Rotation speed, crucible rotation speed each condition portion
Point embodiment 1~8, comparative example 1~13.Then, for the crystal being extracted, judge in the case of can carrying out dislocation-free
Extract, with the presence or absence of deformation, the length of lower convex form.The diameter of the monocrystalline to be cultivated is 390mm, and 350kg is loaded in crucible
Silicon crystal raw material.
In addition, the condition of the 1st process is set to, magnetic flux density is 3000 Gausses, and crystal extraction rate is 0.6~0.8mm/
Min, Crystal Rotation speed are 6rpm, and crucible rotation speed is 0.5rpm.
Embodiment 1~8, the condition and evaluation result of comparative example 1~13 are represented in table 1.In addition, in the result of table 1,
Zero condition represented can obtain dislocation-free and the monocrystalline without deformation, realize the significantly contracting of monocrystalline extraction time compared with the past
Short, the condition that △ is represented can obtain dislocation-free and the monocrystalline without deformation, but the consuming time is needed in extraction, × the bar represented
Part can produce dislocation or deformation.
Table 1
| Magnetic field intensity （Gauss） | Crystal Rotation （rpm） | Crucible rotation （rpm） | Extraction rate （mm/min） | Dwell time （hr） | Dislocation | Deformation | Lower convexity | As a result | |
| Comparative example 1 | 500 | 2 | 0.5 | 0.5 | - | Have | Have | - | × |
| Comparative example 2 | 700 | 2 | 0.5 | 0.5 | - | Have | Have | - | × |
| Embodiment 1 | 800 | 2 | 0.5 | 0.5 | - | Nothing | Nothing | It is convex under 21mm | ○ |
| Comparative example 3 | 1000 | 0.5 | 0.5 | 0.5 | - | Have | Have | - | × |
| Embodiment 2 | 1000 | 1 | 0.5 | 0.5 | - | Nothing | Nothing | It is convex under 15mm | ○ |
| Comparative example 4 | 1000 | 2 | 0.3 | 0.5 | - | Have | Nothing | It is convex under 5mm | × |
| Comparative example 5 | 1000 | 2 | 0.5 | 0.1 | - | Nothing | Nothing | It is convex under 19mm | △ |
| Embodiment 3 | 1000 | 2 | 0.5 | 0.2 | - | Nothing | Nothing | It is convex under 17mm | ○ |
| Embodiment 4 | 1000 | 2 | 0.5 | 0.5 | - | Nothing | Nothing | It is convex under 13mm | ○ |
| Comparative example 6 | 1000 | 2 | 0.5 | 0.6 | - | Have | Have | - | × |
| Embodiment 5 | 1000 | 2 | 0.5 | 0.4 | - | Nothing | Nothing | It is convex under 15mm | ○ |
| Embodiment 6 | 1000 | 2 | 3 | 0.5 | - | Nothing | Nothing | It is convex under 15mm | ○ |
| Embodiment 7 | 1000 | 2 | 5 | 0.5 | - | Nothing | Nothing | It is convex under 18mm | ○ |
| Comparative example 7 | 1000 | 2 | 7 | 0.5 | - | Have | Have | - | × |
| Embodiment 8 | 1000 | 3 | 0.5 | 0.5 | - | Nothing | Nothing | It is convex under 10mm | ○ |
| Comparative example 8 | 1000 | 5 | 0.5 | 0.5 | - | Have | Have | - | × |
| Comparative example 9 | 1100 | 2 | 0.5 | 0.5 | - | Have | Nothing | It is convex under 6mm | × |
| Comparative example 10 | 2000 | 2 | 0.5 | 0.5 | - | Have | Nothing | It is convex | × |
| Comparative example 11 | 3000 | 2 | 0.5 | 0 | 1 | Have | Nothing | It is convex | × |
| Comparative example 12 | 3000 | 2 | 0.5 | 0 | 2 | Nothing | Nothing | It is flat | △ |
| Comparative example 13 | 3000 | 2 | 0.5 | 0.5 | - | Have | Nothing | It is convex | × |
In embodiment 1~8, since stretched portion formed to from fused solution cut off crystal expend the time be about 24 hours with
Under.
On the other hand, after being formed in stretched portion set dwell time comparative example 12 in, since stretched portion formed to from
Fused solution cut off crystal expend the time be less than about 25.5 hours.
The embodiment as a result, stretched portion formed final process be the bar in embodiment 1~8 in the 2nd process
Part, i.e. the magnetic flux density of horizontal magnetic field is in the scope of 800~1000 Gausses, and crystal extraction rate is in 0.2~0.5mm/min（More
Preferably 0.3~0.5mm/min）Scope, Crystal Rotation speed is in 1~4rpm（More preferably 1~3rpm）Scope,
Crucible rotation speed is in 0.5~5rpm（More preferably 0.5~3rpm）Scope, formed in a short time in crystal lower end
The lower convex form prominent downwards of more than 10mm below 30mm length, it can shorten since being formed stretched portion to from melting
Liquid cuts off the extraction time of crystal.
Also, confirm that the lower convex form of more than 10mm below 30mm length can be formed in crystal lower end, obtain error-free
Position and the monocrystalline without deformation.
Claims (3)
1. a kind of monocrystalline extracting method, the monocrystalline extracting method forms silicon melt in crucible, and the silicon melt is applied
Add horizontal magnetic field, and monocrystalline silicon extracted from the silicon melt according to krousky crystal growth method is cut, it is characterised in that
Including the 1st process, the 2nd process and the 3rd process,
1st process forms stretched portion,
2nd process is after the 1st process, in the final process that stretched portion is formed, is formed downwards in crystal lower end
Prominent lower convex form,
3rd process cuts off the lower convex form formed in the 2nd process from the silicon melt,
Dwell time is not provided between foregoing 1st process and foregoing 2nd process,
In the 2nd process,
Crystal extraction rate is located at 0.2~0.5mm/min scope to cultivate crystal,
The magnetic flux density of horizontal magnetic field is controlled into scope in 800~1000 Gausses lower than the 1st process,
Crystal Rotation speed is controlled into scope in 1~4rpm lower than the 1st process,
By crucible rotation speed control 0.5~5rpm scope.
2. monocrystalline extracting method as claimed in claim 1, it is characterised in that
In the 2nd process,
Crystal extraction rate is located at 0.3~0.5mm/min scope to cultivate crystal,
By Crystal Rotation speed control 1~3rpm scope,
By crucible rotation speed control 0.5~3rpm scope.
3. monocrystalline extracting method as claimed in claim 1 or 2, it is characterised in that
In the crystal lower end, the length of the vertical of the lower convex form of formation is in the range of 10~30mm.
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| JP2014087151A JP2015205793A (en) | 2014-04-21 | 2014-04-21 | Method for drawing up single crystal |
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| JP6642410B2 (en) | 2016-12-20 | 2020-02-05 | 株式会社Sumco | Method for producing silicon single crystal |
| CN109763167B (en) * | 2019-03-15 | 2021-01-26 | 内蒙古和光新能源有限公司 | Semiconductor monocrystalline silicon drawing machine |
| CN111379030A (en) * | 2020-05-03 | 2020-07-07 | 朱雪玉 | Novel semiconductor crystal bar arrangement forming die |
| CN115233298B (en) * | 2022-07-25 | 2023-09-01 | 北京麦竹吉科技有限公司 | Back-immersed non-ending Czochralski method and silicon single crystal |
| CN115233297A (en) * | 2022-07-25 | 2022-10-25 | 北京麦竹吉科技有限公司 | Czochralski single crystal pulling method without ending and silicon single crystal |
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| CN101319350A (en) * | 2007-06-08 | 2008-12-10 | 硅电子股份公司 | Single crystal manufacturing method |
| CN101363132A (en) * | 2007-08-07 | 2009-02-11 | 科发伦材料株式会社 | Method of pulling up silicon single crystal |
| CN102197166A (en) * | 2008-12-24 | 2011-09-21 | 昭和电工株式会社 | Process for producing single-crystal sapphire |
| CN101525764A (en) * | 2009-04-16 | 2009-09-09 | 峨嵋半导体材料研究所 | Method for preparing vacuum zone melting high resistant silicon single crystal |
| CN101805925A (en) * | 2010-02-20 | 2010-08-18 | 西安隆基硅材料股份有限公司 | Gallium and indium doped single crystal silicon material for solar battery and preparation method thereof |
| CN102373504A (en) * | 2010-08-06 | 2012-03-14 | 硅电子股份公司 | Silicon single crystal production method |
| CN101974779A (en) * | 2010-11-03 | 2011-02-16 | 天津市环欧半导体材料技术有限公司 | Method for preparing (110) float zone silicon crystal |
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| CN105040099A (en) | 2015-11-11 |
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