CN111139520A - Seeding method by Czochralski method - Google Patents
Seeding method by Czochralski method Download PDFInfo
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- CN111139520A CN111139520A CN201811308065.7A CN201811308065A CN111139520A CN 111139520 A CN111139520 A CN 111139520A CN 201811308065 A CN201811308065 A CN 201811308065A CN 111139520 A CN111139520 A CN 111139520A
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- liquid level
- silicon melt
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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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
- 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
Abstract
The invention provides a seeding method by a Czochralski method, which comprises the following steps: providing a silicon melt and a seed crystal, wherein the liquid level of the silicon melt is at a first liquid level position; dipping the seed crystal into the silicon melt and pulling the seed crystal upward and rotating to extract fine crystals from the liquid surface of the silicon melt; and in the process of leading out the fine crystals, when the length of the fine crystals reaches a preset value, lifting the liquid level of the silicon melt to a second liquid level position, wherein the second liquid level position is higher than the first liquid level position. The seeding method of the czochralski method has the advantages of reducing the temperature difference of the seed crystal in the seeding process and reducing dislocation caused by the temperature difference, thereby improving the seeding success rate and saving the crystal growth cost.
Description
Technical Field
The invention belongs to the field of semiconductor material preparation, and particularly relates to a seeding method by a Czochralski method.
Background
The method mainly comprises four key steps of material melting, seeding, shouldering, crystal waiting and ending in the process of preparing the large-size silicon single crystal. Polycrystalline silicon contained in a quartz crucible is melted by resistance heating while maintaining a temperature slightly higher than the melting point of silicon, a seed crystal is immersed in the melt, and then the seed crystal is pulled up at a certain speed while being rotated to draw out the crystal.
During seeding, the contact between the seed crystal and the melt can generate dislocation at the contact surface due to temperature difference, and a long and thin seed crystal needs to be drawn in order to eliminate the dislocation. In the process of preparing large-size and large-dosage crystals, in order to enable the fine crystals to bear the weight of 250kg-400kg, the diameter of the fine crystals needs to be kept above 4.0mm, and the weight of the crystals is increased, so that the diameter of the fine crystals is thicker.
At present, the seeding method is mainly adopted, namely the liquid level position is directly placed at the position of the equal diameter stage in the seeding stage to start seeding. As the fine grain diameter reaches the target diameter for a length of more than 120mm, a complete seeding process is considered.
Meanwhile, in order to meet the control of the crystal quality, the distance between the liquid level of the silicon melt and the bottom of the heat shield is controlled in a small range. But the axial temperature difference of fine grains is large in the seeding process, so that dislocation is not easy to discharge, and the seeding success rate is influenced.
Based on the above, the invention aims to provide a seeding method of a czochralski method, which is used for reducing the temperature difference of seed crystals in the seeding process and reducing dislocation caused by the temperature difference, thereby improving the seeding success rate and saving the crystal growth cost.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a seeding method of a Czochralski method, which is used for reducing the temperature difference of a seed crystal in the seeding process and reducing dislocation caused by the temperature difference, thereby improving the seeding success rate and saving the crystal growth cost.
To achieve the above and other related objects, the present invention provides a seeding method by the Czochralski method, comprising the steps of:
providing a silicon melt and a seed crystal, wherein the liquid level of the silicon melt is at a first liquid level position;
dipping the seed crystal into the silicon melt and pulling the seed crystal upward and rotating to extract fine crystals from the liquid surface of the silicon melt;
and in the process of leading out the fine crystals, when the length of the fine crystals reaches a preset value for removing dislocation, lifting the liquid level of the silicon melt to a second liquid level position, wherein the second liquid level position is higher than the first liquid level position.
Optionally, the distance between the first liquid surface position and the heat shield is 60 mm-70 mm, and the distance between the second liquid surface position and the heat shield is 35 mm-70 mm.
Optionally, the speed of raising the liquid level of the silicon melt to the second liquid level position is between 0.1mm/min and 2 mm/min.
Optionally, the fine crystals have a length between 200mm and 400mm to exclude dislocations.
Optionally, the fine crystals have a diameter between 4mm and 6 mm.
Optionally, the seed crystal is pulled upward at a rate of 1mm/min to 5mm/min relative to the liquid level of the silicon melt.
Optionally, the temperature change of the heater in the seeding process is between-6 ℃ and +10 ℃.
Optionally, the rotation speed of the seed crystal when being pulled upwards is between 6rpm and 15 rpm.
As described above, the invention provides a seeding method by a Czochralski method, and the invention has the following effects:
the invention divides seeding into two stages, in the first stage, the first liquid level position where the fine crystal is positioned and the heat shield are protected by a larger distance, the fine crystal enters the second stage after dislocation is eliminated, and then the second liquid level position where the fine crystal is positioned is lifted to the position with the equal diameter requirement, so that the fine crystal in the first stage is subjected to more heat radiated by the heater, the temperature difference of the whole fine crystal is kept to be reduced, and the dislocation of the fine crystal is reduced.
The seeding method of the czochralski method has the advantages of reducing the temperature difference of the seed crystal in the seeding process and reducing dislocation caused by the temperature difference, thereby improving the seeding success rate and saving the crystal growth cost.
Drawings
FIG. 1 shows a schematic structural diagram of step 1 of a seeding method of the Czochralski method of the present invention.
FIGS. 2 to 3 show the structure of step 2 of the seeding method of the Czochralski method according to the invention.
FIG. 4 is a schematic diagram showing the structure of step 3 of the seeding method of the Czochralski method of the present invention.
Description of the element reference numerals
101 silicon melt
102 seed crystal
103 fine crystal
104 fine crystal
105 first liquid level position
106 heat shield
107 heater
108 second liquid level position
109 melt crucible
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Please refer to fig. 1 to 4. It should be noted that the drawings provided in the present embodiment are only for illustrating the basic idea of the present invention, and the components related to the present invention are only shown in the drawings rather than drawn according to the number, shape and size of the components in actual implementation, and the type, quantity and proportion of the components in actual implementation may be changed freely, and the layout of the components may be more complicated.
Example 1
The embodiment provides a seeding method of a Czochralski method, which adopts a seeding apparatus as shown in FIG. 1, the seeding apparatus comprises a melt crucible 109, a heater 107 and a heat shield 106, the heater 107 is arranged around the melt crucible 109, the melt crucible 109 carries a silicon melt 101, and the heat shield 106 is arranged above the silicon melt 101 and is used for reflecting heat radiation to the surface of the silicon melt 101 so as to prevent the heat radiation of the silicon melt 101 from diffusing to a crystal bar.
As shown in fig. 1 to 4, the seeding method by the czochralski method comprises the following steps:
as shown in fig. 1, step 1) is performed first, providing a silicon melt 101 and a seed crystal 102, wherein a heat shield 106 is disposed above the silicon melt 101, and the liquid level of the silicon melt 101 is at a first liquid level position 105 relative to the heat shield 106.
By way of example, the distance between the first liquid surface position 105 and the heat shield 106 is between 60mm and 70 mm.
In this embodiment, the distance between the first fluid level position 105 and the heat shield 106 may be 63 mm. At this time, the temperature in the melt is stable, and the diameter of the fine crystal 103 is easily controlled, so that the diameter of the fine crystal 103 is more uniform, and further the generation of dislocation is prevented.
In the present embodiment, the seed crystal 102 has a diameter of 0.4cm to 0.6cm and a length of 8cm to 12cm, for example, the seed crystal 102 may have a diameter of 0.4cm, 0.45cm, 0.5cm, 0.55cm, 0.6cm, etc., and a length of 8cm, 9cm, 10cm, 11cm, 12cm, etc.
As shown in fig. 2 to 3, step 2) is then performed, the seed crystal 102 is immersed in the silicon melt 101, and the seed crystal 102 is pulled up and rotated to extract fine crystals 103 from the liquid surface of the silicon melt 101.
Illustratively, the seed crystal 102 is pulled up at a rate of 1mm/min to 5mm/min with respect to the liquid level of the silicon melt 101, for example, the seed crystal 102 may be pulled up at a rate of 1mm/min, 2mm/min, 3mm/min, 4mm/min, 5mm/min, or the like.
For example, the temperature change of the heater 107 during the seeding process is between-6 ℃ and +10 ℃, for example, the temperature change of the heater 107 during the seeding process can be 5 ℃ lower, 3 ℃ lower, 1 ℃ lower, 3 ℃ higher, 6 ℃ higher, 9 ℃ higher, etc.
Illustratively, the rotation speed of the seed crystal 102 when it is pulled up with respect to the liquid surface is between 6rpm and 15rpm, and for example, the rotation speed of the seed crystal 102 when it is pulled up with respect to the liquid surface may be 10rpm, 11rpm, 12rpm, 13rpm, or the like.
As shown in fig. 4, step 3) is finally performed, and in the process of extracting fine crystals, when the length of the fine crystals 103 reaches a predetermined value for dislocation exclusion, the liquid level of the silicon melt 101 is raised to a second liquid level position 108 toward the heat shield 106, and the second liquid level position 108 is higher than the first liquid level position 105.
By way of example, the distance between the location of the second liquid level 108 and the heat shield 106 is between 35mm and 70 mm.
In this embodiment, the distance between the second liquid level 108 and the heat shield 106 may be 45 mm. At this time, the shouldering speed of the fine grains 104 is stable, the temperature is easy to control, and broken edges are not easy to appear.
Illustratively, the speed of raising the surface of the silicon melt 101 to the second surface position 108 is between 0.1mm/min and 2 mm/min.
As an example, the length of the fine crystals 104 is between 200mm and 400mm to exclude dislocations, for example, the length of the fine crystals 104 may be 210mm, 280mm, 320mm, 370mm, etc.
When the seed crystal 102 is immersed in the silicon melt 101, dislocations are generated due to the thermal stress and the surface tension caused by the temperature difference between the seed crystal 102 and the silicon melt 101, and thus, the dislocations can disappear and a dislocation-free growth state can be established by applying a taper neck process, i.e., Dash technique, after the fusion. Dislocations extend along the slip plane and slip, and thus the dislocations disappear to extend and slip to the crystal surface.
By way of example, the fine crystals 104 have a diameter between 4mm and 6mm, for example, the fine crystals 104 may have a diameter of 4.2mm, 4.6mm, 5.2mm, 5.7mm, and the like.
Example 2
The embodiment provides a seeding method of a Czochralski method, which adopts a seeding apparatus as shown in FIG. 1, the seeding apparatus comprises a melt crucible 109, a heater 107 and a heat shield 106, the heater 107 is arranged around the melt crucible 109, the melt crucible 109 carries a silicon melt 101, and the heat shield 106 is arranged above the silicon melt 101 and is used for reflecting heat radiation to the surface of the silicon melt 101 so as to prevent the heat radiation of the silicon melt 101 from diffusing to a crystal bar.
As shown in fig. 1 to 4, the seeding method by the czochralski method comprises the following steps:
as shown in fig. 1, step 1) is performed first, providing a silicon melt 101 and a seed crystal 102, wherein a heat shield 106 is disposed above the silicon melt 101, and the liquid level of the silicon melt 101 is at a first liquid level position 105 relative to the heat shield 106.
By way of example, the distance between the first liquid surface position 105 and the heat shield 106 is between 60mm and 70 mm.
In this embodiment, the distance between the first fluid level position 105 and the heat shield 106 may be 66 mm. At this time, the temperature in the melt is stable, and the diameter of the fine crystal 103 is easily controlled, so that the diameter of the fine crystal 103 is more uniform, and further the generation of dislocation is prevented.
In the present embodiment, the seed crystal 102 has a diameter of 0.4cm to 0.6cm and a length of 8cm to 12cm, for example, the seed crystal 102 may have a diameter of 0.4cm, 0.45cm, 0.5cm, 0.55cm, 0.6cm, etc., and a length of 8cm, 9cm, 10cm, 11cm, 12cm, etc.
As shown in fig. 2 to 3, step 2) is then performed, the seed crystal 102 is immersed in the silicon melt 101, and the seed crystal 102 is pulled up and rotated to extract fine crystals 103 from the liquid surface of the silicon melt 101.
Illustratively, the seed crystal 102 is pulled up at a rate of 1mm/min to 5mm/min with respect to the liquid level of the silicon melt 101, for example, the seed crystal 102 may be pulled up at a rate of 1mm/min, 2mm/min, 3mm/min, 4mm/min, 5mm/min, or the like.
For example, the temperature change of the heater 107 during the seeding process is between-6 ℃ and +10 ℃, for example, the temperature change of the heater 107 during the seeding process can be 5 ℃ lower, 3 ℃ lower, 1 ℃ lower, 3 ℃ higher, 6 ℃ higher, 9 ℃ higher, etc.
Illustratively, the rotation speed of the seed crystal 102 when it is pulled up with respect to the liquid surface is between 6rpm and 15rpm, and for example, the rotation speed of the seed crystal 102 when it is pulled up with respect to the liquid surface may be 10rpm, 11rpm, 12rpm, 13rpm, or the like.
As shown in fig. 4, step 3) is finally performed, and in the process of extracting fine crystals, when the length of the fine crystals 103 reaches a predetermined value for dislocation exclusion, the liquid level of the silicon melt 101 is raised to a second liquid level position 108 toward the heat shield 106, and the second liquid level position 108 is higher than the first liquid level position 105.
By way of example, the distance between the location of the second liquid level 108 and the heat shield 106 is between 35mm and 70 mm.
In this embodiment, the distance between the second liquid level 108 and the heat shield 106 may be 40 mm. At this time, the shouldering speed of the fine grains 104 is stable, the temperature is easy to control, and broken edges are not easy to appear.
Illustratively, the speed of raising the surface of the silicon melt 101 to the second surface position 108 is between 0.1mm/min and 2 mm/min.
As an example, the length of the fine crystals 104 is between 200mm and 400mm to exclude dislocations, for example, the length of the fine crystals 104 may be 210mm, 280mm, 320mm, 370mm, etc.
When the seed crystal 102 is immersed in the silicon melt 101, dislocations are generated due to the thermal stress and the surface tension caused by the temperature difference between the seed crystal 102 and the silicon melt 101, and thus, the dislocations can disappear and a dislocation-free growth state can be established by applying a taper neck process, i.e., Dash technique, after the fusion. Dislocations extend along the slip plane and slip, and thus the dislocations disappear to extend and slip to the crystal surface.
By way of example, the fine crystals 104 have a diameter between 4mm and 6mm, for example, the fine crystals 104 may have a diameter of 4.2mm, 4.6mm, 5.2mm, 5.7mm, and the like.
Example 3
The embodiment provides a seeding method of a Czochralski method, which adopts a seeding apparatus as shown in FIG. 1, the seeding apparatus comprises a melt crucible 109, a heater 107 and a heat shield 106, the heater 107 is arranged around the melt crucible 109, the melt crucible 109 carries a silicon melt 101, and the heat shield 106 is arranged above the silicon melt 101 and is used for reflecting heat radiation to the surface of the silicon melt 101 so as to prevent the heat radiation of the silicon melt 101 from diffusing to a crystal bar.
As shown in fig. 1 to 4, the seeding method by the czochralski method comprises the following steps:
as shown in fig. 1, step 1) is performed first, providing a silicon melt 101 and a seed crystal 102, wherein a heat shield 106 is disposed above the silicon melt 101, and the liquid level of the silicon melt 101 is at a first liquid level position 105 relative to the heat shield 106.
By way of example, the distance between the first liquid surface position 105 and the heat shield 106 is between 60mm and 70 mm.
In this embodiment, the distance between the first fluid level position 105 and the heat shield 106 may be 69 mm. At this time, the temperature in the melt is stable, and the diameter of the fine crystal 103 is easily controlled, so that the diameter of the fine crystal 103 is more uniform, and further the generation of dislocation is prevented.
In the present embodiment, the seed crystal 102 has a diameter of 0.4cm to 0.6cm and a length of 8cm to 12cm, for example, the seed crystal 102 may have a diameter of 0.4cm, 0.45cm, 0.5cm, 0.55cm, 0.6cm, etc., and a length of 8cm, 9cm, 10cm, 11cm, 12cm, etc.
As shown in fig. 2 to 3, step 2) is then performed, the seed crystal 102 is immersed in the silicon melt 101, and the seed crystal 102 is pulled up and rotated to extract fine crystals 103 from the liquid surface of the silicon melt 101.
Illustratively, the seed crystal 102 is pulled up at a rate of 1mm/min to 5mm/min with respect to the liquid level of the silicon melt 101, for example, the seed crystal 102 may be pulled up at a rate of 1mm/min, 2mm/min, 3mm/min, 4mm/min, 5mm/min, or the like.
For example, the temperature change of the heater 107 during the seeding process is between-6 ℃ and +10 ℃, for example, the temperature change of the heater 107 during the seeding process can be 5 ℃ lower, 3 ℃ lower, 1 ℃ lower, 3 ℃ higher, 6 ℃ higher, 9 ℃ higher, etc.
Illustratively, the rotation speed of the seed crystal 102 when it is pulled up with respect to the liquid surface is between 6rpm and 15rpm, and for example, the rotation speed of the seed crystal 102 when it is pulled up with respect to the liquid surface may be 10rpm, 11rpm, 12rpm, 13rpm, or the like.
As shown in fig. 4, step 3) is finally performed, and in the process of extracting fine crystals, when the length of the fine crystals 103 reaches a predetermined value for dislocation exclusion, the liquid level of the silicon melt 101 is raised to a second liquid level position 108 toward the heat shield 106, and the second liquid level position 108 is higher than the first liquid level position 105.
By way of example, the distance between the location of the second liquid level 108 and the heat shield 106 is between 35mm and 70 mm.
In this embodiment, the distance between the second liquid level 108 and the heat shield 106 may be 50 mm. At this time, the shouldering speed of the fine grains 104 is stable, the temperature is easy to control, and broken edges are not easy to appear.
Illustratively, the speed of raising the surface of the silicon melt 101 to the second surface position 108 is between 0.1mm/min and 2 mm/min.
As an example, the length of the fine crystals 104 is between 200mm and 400mm to exclude dislocations, for example, the length of the fine crystals 104 may be 210mm, 280mm, 320mm, 370mm, etc.
When the seed crystal 102 is immersed in the silicon melt 101, dislocations are generated due to the thermal stress and the surface tension caused by the temperature difference between the seed crystal 102 and the silicon melt 101, and thus, the dislocations can disappear and a dislocation-free growth state can be established by applying a taper neck process, i.e., Dash technique, after the fusion. Dislocations extend along the slip plane and slip, and thus the dislocations disappear to extend and slip to the crystal surface.
By way of example, the fine crystals 104 have a diameter between 4mm and 6mm, for example, the fine crystals 104 may have a diameter of 4.2mm, 4.6mm, 5.2mm, 5.7mm, and the like.
In conclusion, the invention provides a seeding method by a Czochralski method, which has the following effects:
the invention divides seeding into two stages, in the first stage, the first liquid level position where the fine crystal is positioned and the heat shield are protected by a larger distance, the fine crystal enters the second stage after dislocation is eliminated, and then the second liquid level position where the fine crystal is positioned is lifted to the position with the equal diameter requirement, so that the fine crystal in the first stage is subjected to more heat radiated by the heater, the temperature difference of the whole fine crystal is kept to be reduced, and the dislocation of the fine crystal is reduced.
The seeding method of the czochralski method has the advantages of reducing the temperature difference of the seed crystal in the seeding process and reducing dislocation caused by the temperature difference, thereby improving the seeding success rate and saving the crystal growth cost. Therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (8)
1. A seeding method by a czochralski method, which is characterized by comprising the following steps:
providing a silicon melt and a seed crystal, wherein the liquid level of the silicon melt is at a first liquid level position;
dipping the seed crystal into the silicon melt and pulling the seed crystal upward and rotating to extract fine crystals from the liquid surface of the silicon melt;
and in the process of leading out the fine crystals, when the length of the fine crystals reaches a preset value for removing dislocation, lifting the liquid level of the silicon melt to a second liquid level position, wherein the second liquid level position is higher than the first liquid level position.
2. A czochralski seeding method as claimed in claim 1, wherein: the distance between the first liquid surface position and the heat shield is 60-70 mm, and the distance between the second liquid surface position and the heat shield is 35-70 mm.
3. A czochralski seeding method as claimed in claim 1, wherein: and the speed of lifting the liquid level of the silicon melt to the second liquid level position is between 0.1mm/min and 2 mm/min.
4. A czochralski seeding method as claimed in claim 1, wherein: the length of the fine crystals is between 200mm and 400mm to exclude dislocations.
5. A czochralski seeding method as claimed in claim 1, wherein: the diameter of the fine crystals is between 4mm and 6 mm.
6. A czochralski seeding method as claimed in claim 1, wherein: the seed crystal is pulled upwards relative to the liquid level of the silicon melt at a speed of 1mm/min to 5 mm/min.
7. A czochralski seeding method as claimed in claim 1, wherein: the temperature change of the heater in the seeding process is between-6 ℃ and +10 ℃.
8. A czochralski seeding method as claimed in claim 1, wherein: the rotating speed of the seed crystal when being lifted upwards is between 6rpm and 15 rpm.
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Cited By (3)
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| CN111647940A (en) * | 2020-08-04 | 2020-09-11 | 浙江晶科能源有限公司 | Monocrystalline silicon preparation method and device |
| CN112359412A (en) * | 2020-11-03 | 2021-02-12 | 上海新昇半导体科技有限公司 | Seeding method for crystal growth |
| CN115110146A (en) * | 2022-06-30 | 2022-09-27 | 西安奕斯伟材料科技有限公司 | Seed crystal and crystal pulling method and device |
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| US11708643B2 (en) | 2020-08-04 | 2023-07-25 | Shangrao Jinko Solar Technology Development Co., Ltd | Method and apparatus for manufacturing monocrystalline silicon |
| CN112359412A (en) * | 2020-11-03 | 2021-02-12 | 上海新昇半导体科技有限公司 | Seeding method for crystal growth |
| CN115110146A (en) * | 2022-06-30 | 2022-09-27 | 西安奕斯伟材料科技有限公司 | Seed crystal and crystal pulling method and device |
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