CN110318096A - Zone-melted silicon single crystal ending method and drawing method - Google Patents
Zone-melted silicon single crystal ending method and drawing method Download PDFInfo
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- CN110318096A CN110318096A CN201910571165.7A CN201910571165A CN110318096A CN 110318096 A CN110318096 A CN 110318096A CN 201910571165 A CN201910571165 A CN 201910571165A CN 110318096 A CN110318096 A CN 110318096A
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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
-
- 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
- C30B13/30—Stabilisation or shape controlling of the molten zone, e.g. by concentrators, by electromagnetic fields; Controlling the section of the crystal
-
- 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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- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
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- Electromagnetism (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
This application involves a kind of zone-melted silicon single crystal ending method and drawing methods, wherein ending method includes: when the technique of current growing single crystals reaches end isodiametric growth and opens the condition of ending, close isodiametric growth operation, the upper axis and lower axle for controlling the zone melting single-crystal furnace of pulling monocrystal body stop decline, and reduce power;When monocrystalline solid-liquid interface starts to shrink, control lower axle opens decline, and when monocrystalline ending waist starts to attenuate, axis opens decline in control, and continues to reduce power preset time;Aforesaid operations are executed repeatedly, until axis is begun to ramp up in control, and when the diameter of monocrystalline solid-liquid interface is contracted to the first default value, polycrystal raw material is separated with monocrystal after reaching preset condition.It both can effectively solve the problems, such as monocrystalline dislocation, while production cost can also be effectively reduced, improve the yield rate of monocrystalline compared to slow ending mode in the related technology.
Description
Technical field
This disclosure relates to semiconductor process technique field more particularly to a kind of zone-melted silicon single crystal ending method and drawing side
Method.
Background technique
It is a kind of method for monocrystal growth for being different from vertical pulling method that zone-melting process, which produces monocrystalline silicon, it will using radio-frequency induction coil
The melting zone of high-purity polycrystal material heating and melting, generation is in by the magnetic supporting power that the surface tension and heating coil of molten silicon provide
Suspended state, then the process using seed crystal welding polycrystalline bar by crystal growth and ending is drawn into monocrystalline.
The growth course of zone-melted silicon single crystal be mainly prepurging, shove charge, evacuation, preheating, material, seeding, shouldering, turn shoulder, etc.
Diameter, ending, cooling, blowing out.Wherein, in the related art, during drawing zone-melted silicon single crystal, to the receipts of zone-melted silicon single crystal
Tail operation is all usually by the way of finishing up slowly, this allows for zone-melted silicon single crystal epilog than relatively time-consuming.
Summary of the invention
In view of this, area can be effectively reduced the present disclosure proposes a kind of zone-melted silicon single crystal ending method and drawing method
The ending time of silicon crystal improves ending rate.
According to the one side of the disclosure, a kind of zone-melted silicon single crystal ending method is provided, comprising:
S100 closes institute when the technique of current growing single crystals, which reaches, to be terminated isodiametric growth and open the condition of ending
Isodiametric growth operation is stated, control draws the upper axis of the zone melting single-crystal furnace of the monocrystal and lower axle stops decline, and reduces power;
S200 controls the lower axle and opens decline, and open in monocrystalline ending waist when monocrystalline solid-liquid interface starts to shrink
When beginning attenuates, controls the upper axis and open decline, and continue to reduce the power preset time;
S100 and S200 is executed repeatedly, until controlling the upper axis after reaching preset condition and beginning to ramp up, and in the list
When the diameter of brilliant solid-liquid interface is contracted to the first default value, polycrystal raw material is separated with monocrystal.
In one possible implementation, the condition for terminating isodiametric growth and opening ending is based on current set
Monocrystal size determine.
In one possible implementation, based on current set monocrystal size, determining terminates isodiametric growth simultaneously
Open the condition of ending, comprising:
When between the current set monocrystal is having a size of 4 inches -6 inches, the end isodiametric growth is determined
And open the condition of ending are as follows: the residue length of polycrystal raw material is 5mm -10mm;
When the current set monocrystal is having a size of 3 inches or less, determines the end isodiametric growth and open
The condition of ending are as follows: the upper axis of the zone melting single-crystal furnace drops to lower limit.
It is described default when in one possible implementation, between the monocrystal is having a size of 4 inches -6 inches
Condition is that monocrystalline ending diameter is contracted between 40mm -60mm;
When the monocrystal is having a size of 3 inches or less, the preset condition is the diameter of the monocrystalline solid-liquid interface
For the one third of the diameter of the monocrystal.
It is described default when in one possible implementation, between the monocrystal is having a size of 4 inches -6 inches
Condition is that monocrystalline ending diameter is contracted to 50mm.
In one possible implementation, the value range of first default value is 10mm -30mm.
In one possible implementation, the value of first default value is 20mm.
In one possible implementation, the reduction rate of the power are as follows: every 5s declines the isometrical power of 0.5%*.
In one possible implementation, the upper axis fall off rate are as follows: upper axis decrease speed when isodiametric growth;Institute
State lower axle fall off rate are as follows: the lower axle decrease speed when monocrystal isodiametric growth;The upper axis climbing speed are as follows: 1mm/
min。
According to another aspect of the present disclosure, a kind of zone-melted silicon single crystal drawing method is additionally provided, including front is any described
Zone-melted silicon single crystal finish up method.
The zone-melted silicon single crystal ending method of the embodiment of the present disclosure, passes through and completes isodiametric growth technique during crystal-pulling
Afterwards, by the way of adjusting upper axle speed, lower circular velocity and power simultaneously, quick ending has been achieved the purpose that.Compared to correlation
Slow ending mode in technology, both can effectively solve the problems, such as monocrystalline dislocation, while production cost can also be effectively reduced, mention
The yield rate of high monocrystalline.
According to below with reference to the accompanying drawings to detailed description of illustrative embodiments, the other feature and aspect of the disclosure will become
It is clear.
Detailed description of the invention
Comprising in the description and constituting the attached drawing of part of specification and specification together illustrates the disclosure
Exemplary embodiment, feature and aspect, and for explaining the principles of this disclosure.
Fig. 1 shows the flow chart of the zone-melted silicon single crystal ending method of the embodiment of the present disclosure.
Specific embodiment
Various exemplary embodiments, feature and the aspect of the disclosure are described in detail below with reference to attached drawing.It is identical in attached drawing
Appended drawing reference indicate element functionally identical or similar.Although the various aspects of embodiment are shown in the attached drawings, remove
It non-specifically points out, it is not necessary to attached drawing drawn to scale.
Dedicated word " exemplary " means " being used as example, embodiment or illustrative " herein.Here as " exemplary "
Illustrated any embodiment should not necessarily be construed as preferred or advantageous over other embodiments.
In addition, giving numerous details in specific embodiment below to better illustrate the disclosure.
It will be appreciated by those skilled in the art that without certain details, the disclosure equally be can be implemented.In some instances, for
Method, means, element and circuit well known to those skilled in the art are not described in detail, in order to highlight the purport of the disclosure.
Fig. 1 shows the flow chart of the zone-melted silicon single crystal ending method of the embodiment of the present disclosure.Refering to fig. 1, implement in the disclosure
It first include step S100 in the zone-melted silicon single crystal ending method of example, it is isometrical to reach end in the technique of current growing single crystals
When growing and opening the condition of ending, isodiametric growth operation is closed.And control pulling monocrystal body zone melting single-crystal furnace upper axis and
Lower axle stops decline, and reduces power.
Here, it should be pointed out that in one possible implementation, whether the technique of current growing single crystals reaches
Terminate isodiametric growth and open the condition of ending, can be determined based on the size of current set monocrystal.That is, according to working as
The specification of preceding grown monocrystal, to determine the unlocking condition of tailing-in technique.By according to the monocrystalline currently grown
The specification of body determines when to open tailing-in technique so that when each drawn monocrystalline silicon, the opening time of tailing-in technique with
The monocrystal currently grown more matches, and the opening time that this also allows for tailing-in technique is more accurate.
Wherein, the condition for terminating isodiametric growth and opening tailing-in technique is being determined based on current set monocrystal size
When, it may include following two mode.
As: monocrystal size by 4 inches -6 inches between (that is, the size of the monocrystal currently grown be greater than etc.
In 4 inches and it is less than or equal to 6 inches) when, terminate isodiametric growth and open the condition of ending (that is, the time for opening ending) are as follows:
The residue length of polycrystal raw material is between 5mm -10mm.That is, the size in the monocrystal currently grown is 4 English
When between very little -6 inches, when any value during the residue length of polycrystal raw material is between 5mm -10mm, list can be terminated
Brilliant isodiametric growth process, and open epilog.
When the size of monocrystal is 3 inches or less, terminates isodiametric growth and open the condition of ending are as follows: zone melting single-crystal furnace
Upper axis drop to lower limit.That is, when the size of the monocrystal currently grown is 3 inches or less, in zone melting single-crystal furnace
When upper axis drops to lower limit, the isodiametric growth process of monocrystalline can be terminated, and open ending operation.
Wherein, it will be appreciated by persons skilled in the art that the size of monocrystal described herein refers to monocrystal
Diameter.That is, the diameter of monocrystal is between 4 inches -6 inches or the diameter of monocrystal is 3 inches or less.
When the technique of current growing single crystals, which reaches, to be terminated isodiametric growth and open the condition of ending, isodiametric growth is closed
Operation, the upper axis and lower axle for controlling the zone melting single-crystal furnace of pulling monocrystal body stop decline, and after reducing power for a period of time, in list
When brilliant solid-liquid interface starts to shrink, step S200 is executed, control lower axle opens decline, and in monocrystalline ending waist (that is, monocrystal
By shouldering, the position come is being drawn out after isodiametric growth) start to attenuate when, axis opens decline and continues to reduce in control
Power preset time.Step S100 and step S200 is executed repeatedly, until executing step S300, control after reaching preset condition
Upper axis is begun to ramp up, and when the diameter of monocrystalline solid-liquid interface is contracted to the first default value, by polycrystal raw material and monocrystal
Separation.
The zone-melted silicon single crystal ending method of the embodiment of the present disclosure as a result, by completing isometrical life during crystal-pulling
After long technique, by the way of adjusting upper axle speed, lower circular velocity and power simultaneously, quick ending is achieved the purpose that.It compares
In slow ending mode in the related technology, monocrystalline dislocation both can be effectively solved the problems, such as, while production can also be effectively reduced
Cost improves the yield rate of monocrystalline.
Wherein, it should be noted that step S100 and step S200 is executed repeatedly, until after reaching preset condition in control
Axis begin to ramp up in preset condition, based on institute's pulled crystal size difference it is different.In a kind of possible realization side
In formula, when the size of monocrystal is between 4 inches -6 inches, preset condition can be set as monocrystalline ending diameter and be contracted to
Between 40mm -60mm.Such as: preset condition can be set to monocrystalline ending diameter and be contracted to 50mm or so.Monocrystal having a size of
At 3 inches or less, preset condition can be set as the diameter of monocrystalline solid-liquid interface as the one third of the diameter of monocrystal.
Further, the value range of the first default value can be set to 10mm -30mm.As: the first default value
Value can be set to 20mm.By setting 20mm for the first default value, so that carrying out polycrystal raw material and monocrystal
When separation, it can be realized and quickly and accurately separated between polycrystal raw material and monocrystal, both avoided monocrystalline solid-liquid interface
The excessive phenomenon for causing polycrystal raw material not thorough enough when separating with monocrystal of diameter, while preventing monocrystalline solid-liquid interface
Diameter is too small to lead to the case where solidifying between polycrystal raw material and monocrystal, so that the matter for drawing the monocrystal for being in be effectively ensured
Amount.
The method that is, zone-melted silicon single crystal of the embodiment of the present disclosure finishes up utilizes to improve the maximum of polycrystal raw material
Rate, reduce production cost, improve production efficiency, reach terminate the isodiametric growth stage start epilog when, by upper axis
Three speed, lower axle speed and power parameters are adjusted, the purpose that Lai Shixian zone-melted silicon single crystal quickly finishes up.
Wherein, by could be adjusted to carry out zone-melted silicon single crystal to three upper axle speed, lower axle speed and power parameters
Epilog when, the monocrystal of different specification size, corresponding tailing-in technique parameter is different.For example:
When the size of monocrystal is 4 inches -6 inches, tailing-in technique is carried out in polycrystal raw material also surplus 5mm -10mm.
When ending, the speed of the speed and lower axle that first stop upper axis is taken, and slowly reduces power.Have and to receive in monocrystalline solid-liquid interface
Sign when, i.e. the diameter of monocrystalline solid-liquid interface before stopping upper axle speed and lower axle speed compared to starting to be reduced
When, open lower axle decrease speed.And when monocrystalline ending waist attenuates, axis starts to rotate in control, so that upper axis is begun to decline.Together
When, continue to reduce power preset time.Herein, it should be noted that in this embodiment, preset time can be received according to monocrystalline
The variable condition of tail waist determines.By executing the decrease speed of the decrease speed and lower axle that stop upper axis repeatedly, lower axle is opened
The operation of decrease speed and upper axis decrease speed causes to solidify to guarantee that monocrystalline ending waist is unlikely to meticulous.To monocrystalline ending waist
When diameter is contracted to 50mm or so, by controlling the lifter switch of upper axis, so that upper axis opens lifting operations, and in monocrystalline solid-liquid
When the diameter of interface is contracted to 20mm or so, quickly polycrystal raw material is separated with monocrystal.
When the size of monocrystal is 3 inches or less, terminate in isodiametric growth technique, upper axis drops to lower limit (that is, single
The extreme lower position that set upper axis can decline in brilliant furnace) when finish up.In ending, stop the lower reduction of speed of lower axle first
The decrease speed of degree and upper axis, and slowly reduce power.When monocrystalline solid-liquid interface has the sign to be received, that is to say, that
The diameter of monocrystalline solid-liquid interface starts to start before the decrease speed compared to the decrease speed and upper axis that stop lower axle
When diminution, the lifter switch of lower axle is opened, so that lower axle is begun to decline, and continues slowly to reduce power, until monocrystalline solid-liquid is handed over
When interface is contracted to the one third of the diameter of monocrystal, then controls axis and begin to ramp up.The diameter of equal monocrystalline solid-liquid interface
When being contracted to 20mm or so, quickly polycrystal raw material is separated with monocrystal.
In addition it is also necessary to which required power is not also identical, it is noted that the diameter due to monocrystal is different.By monocrystalline
Body separates rear power with polycrystal raw material and should not exceed 55% isometrical power (herein, isometrical power is referred in pulling monocrystal body
When, the power that is applied), to avoid sparking.
Correspondingly, based on any zone-melted silicon single crystal ending method in front, the disclosure additionally provides a kind of zone melting and refining silicon
Crystal-pulling method.Since the tailing-in technique in the zone-melted silicon single crystal drawing method of the embodiment of the present disclosure is using disclosure reality
The zone-melted silicon single crystal ending method of example is applied, therefore overlaps will not be repeated.
In order to illustrate more clearly of the zone-melted silicon single crystal drawing method of the embodiment of the present disclosure, below with a specific embodiment into
Row is explained in more detail.
For example, this specific embodiment uses JQ900 type zone melting single-crystal furnace, draws 6 inches of zone melting single-crystals below.
Firstly, shove charge, evacuation, applying argon gas: that is, utilizing burner hearth, coil, heat-preservation cylinder, the polycrystalline of wiping furnace paper wiping single crystal growing furnace
Feed collet holder, seedholder.Polycrystal raw material is hung on polycrystal material clamper, and seed crystal is clamped on seedholder.
Meanwhile in order to improve the stability of monocrystalline and qualification rate, in the embodiments of the present disclosure, also the pin piece in single crystal growing furnace is added
Greatly, after thickening processing (that is, the thickness of pin piece is increased to 0.2cm, diameter increases to 80mm), pin piece is pressed from both sides mounted in monocrystalline
In holder.Then, fire door is closed, fire door screw is tightened, vacuumizes, applying argon gas.Wherein, vacuumize, the operation of applying argon gas can be with
The program of inflation is evacuated by being arranged in the operator control panel of single crystal growing furnace.Such as: argon flow can be set to 20L/min, take out true
Furnace chamber pressure is 0.050mbar after sky, and starting, which is evacuated to evacuation automatically, to be terminated.
Then, preheating, the material of polycrystal raw material are carried out: that is, opening generator power, being adjusted to current-mode, and adjust electricity
Stream setting value is preheated to 25% pair of silicon rod (that is, polycrystal raw material).It is micro- red to polycrystal raw material, generator is adjusted to voltage-mode
Formula adjusts voltage setting value 30% -50%, turns 3rpm/min, left and right material in starting.
Secondly, carrying out seeding, drawing and attenuating diameter operation: by seed crystal and melting zone point contact, while opening the lifting of upper axis and lower axle
Device adjusts voltage setting value to 40% -60%, to grow thin footpath.Wherein, thin footpath diameter is 2mm-3mm, and length is
40mm—50mm。
Then, it executes the process of shouldering, coil offset and isodiametric growth: that is, thin footpath starts shouldering after the completion of drawing, using
The rotation speed and power control of upper axis grow angle, and with the shape in power control melting zone, offset coil is extremely during crystal pulling
4.6mm left and right.When single crystal diameter is greater than 50mm, the automatic growth program on opening operation screen is isometrical to monocrystalline.
Then, it the operation for executing ending, putting off: that is, when polycrystal raw material residue length is in 5mm or so, closes automatic raw
Long-range order.First stop the speed of upper axis and lower axle, and slowly reduces power.Wherein, the reduction rate of power can be set to every 5s
The isometrical power of decline 0.5%.Lower axle decline is controlled when monocrystalline solid-liquid interface has the sign to be received.Become to monocrystalline ending waist
Upper axis decline is opened when thin, and continues to reduce power.Execute aforesaid operations repeatedly to guarantee that waist meticulous not cause to solidify.Monocrystalline
When ending diameter is contracted to 50mm or so, axis rises in control.When the diameter of equal monocrystalline solid-liquid interface is contracted to 20mm or so,
Quickly polycrystal raw material is separated with monocrystalline.
Finally, execute stop the supple of gas or steam, blowing out and the operation for tearing furnace open: that is, closing impurity gas, mixing in the operator control panel of single crystal growing furnace
Gas, mixing argon gas.Melting zone carries out slow cooling process after breaking.After monocrystalline blackening, generator is closed.After monocrystalline is cooling
It opens fire door and takes out monocrystalline.
The zone-melted silicon single crystal drawing method of the embodiment of the present disclosure, by using any area in front in epilog
Silicon crystal ending method allows every monocrystalline to shorten ending the time 10 minutes or more.Also, polycrystal raw material can achieve
Peak use rate, every monocrystalline ending can reduce by 2/3rds or more raw material, this also just effectively improves terminal velocity, together
When also save production cost.
The presently disclosed embodiments is described above, above description is exemplary, and non-exclusive, and
It is not limited to disclosed each embodiment.Without departing from the scope and spirit of illustrated each embodiment, for this skill
Many modifications and changes are obvious for the those of ordinary skill in art field.The selection of term used herein, purport
In the principle, practical application or technological improvement to the technology in market for best explaining each embodiment, or lead this technology
Other those of ordinary skill in domain can understand each embodiment disclosed herein.
Claims (10)
- A kind of method 1. zone-melted silicon single crystal finishes up characterized by comprisingS100 is closed described etc. when the technique of current growing single crystals, which reaches, to be terminated isodiametric growth and open the condition of ending Diameter growth operation, control draws the upper axis of the zone melting single-crystal furnace of the monocrystal and lower axle stops decline, and reduces power;S200 controls the lower axle and opens decline, and start to become in monocrystalline ending waist when monocrystalline solid-liquid interface starts to shrink When thin, control the upper axis and open decline, and continue to reduce the power preset time;S100 and S200 is executed repeatedly, until controlling the upper axis after reaching preset condition and beginning to ramp up, and is solid in the monocrystalline When the diameter of liquid interface is contracted to the first default value, polycrystal raw material is separated with monocrystal.
- 2. the method according to claim 1, wherein the condition for terminating isodiametric growth and opening ending is based on Current set monocrystal size determines.
- 3. according to the method described in claim 2, it is characterized in that, based on current set monocrystal size, determination terminates Isodiametric growth and the condition for opening ending, comprising:When between the current set monocrystal is having a size of 4 inches -6 inches, determines the end isodiametric growth and open Open the condition of ending are as follows: the residue length of polycrystal raw material is 5mm -10mm;When the current set monocrystal is having a size of 3 inches or less, determines the end isodiametric growth and open ending Condition are as follows: the upper axis of the zone melting single-crystal furnace drops to lower limit.
- 4. the method according to claim 1, wherein between the monocrystal is having a size of 4 inches -6 inches When, the preset condition is that monocrystalline ending diameter is contracted between 40mm -60mm;When the monocrystal is having a size of 3 inches or less, the preset condition is that the diameter of the monocrystalline solid-liquid interface is institute State the one third of the diameter of monocrystal.
- 5. according to the method described in claim 4, it is characterized in that, between the monocrystal is having a size of 4 inches -6 inches When, the preset condition is that monocrystalline ending diameter is contracted to 50mm.
- 6. method according to any one of claims 1 to 5, which is characterized in that the value range of first default value For 10mm -30mm.
- 7. according to the method described in claim 6, it is characterized in that, the value of first default value is 20mm.
- 8. method according to any one of claims 1 to 5, which is characterized in that the reduction rate of the power are as follows: under every 5s The isometrical power of 0.5%* drops.
- 9. method according to any one of claims 1 to 5, which is characterized in that the upper axis fall off rate are as follows: isodiametric growth When on axis decrease speed;The lower axle fall off rate are as follows: the lower axle decrease speed when monocrystal isodiametric growth;The upper axis Climbing speed are as follows: 1mm/min.
- 10. a kind of zone-melted silicon single crystal drawing method, which is characterized in that including the described in any item zone melting and refining silicon lists of claim 1 to 9 Brilliant ending method.
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