WO2024051241A1 - Monocrystalline silicon shouldering method - Google Patents

Monocrystalline silicon shouldering method Download PDF

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Publication number
WO2024051241A1
WO2024051241A1 PCT/CN2023/099725 CN2023099725W WO2024051241A1 WO 2024051241 A1 WO2024051241 A1 WO 2024051241A1 CN 2023099725 W CN2023099725 W CN 2023099725W WO 2024051241 A1 WO2024051241 A1 WO 2024051241A1
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WIPO (PCT)
Prior art keywords
shoulder
range
crystal
interval
speed
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PCT/CN2023/099725
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French (fr)
Chinese (zh)
Inventor
武刚
成路
杜婷婷
王正远
丁彪
马少林
Original Assignee
隆基绿能科技股份有限公司
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Publication of WO2024051241A1 publication Critical patent/WO2024051241A1/en

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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
    • 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
    • C30B15/20—Controlling or regulating
    • 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

Definitions

  • the embodiments of the present application relate to the field of photovoltaic technology, and in particular, to a single crystal silicon shoulder placement method.
  • the Czochralski method (Cz method) is one of the commonly used crystal growth methods.
  • the raw silicon is heated and melted in a single crystal furnace, and then the rod-shaped seed crystal is immersed in the melt, so that the silicon atoms in the melt grow along the seeds.
  • the arrangement structure of silicon atoms on the crystal forms regular crystals at the solid-liquid interface, thereby forming a single crystal.
  • the Czochralski method usually includes: temperature adjustment, seeding, shoulder placement, shoulder rotation, equal diameter, finishing, feeding, etc. Process steps.
  • the crystal diameter is gradually grown to the target diameter by reducing the pulling speed and temperature.
  • the top angle of the shoulder is usually an obtuse angle and the pulling speed of the crystal ingot is slow. Perform shoulder-resting maneuvers.
  • the above method can easily lead to dislocations in the crystal, failure of shoulder placement, and a small amount of cooling, resulting in high oxygen content in the head of the crystal, affecting the quality of the crystal.
  • This application provides a single crystal silicon shoulder placement method, aiming to reduce the possibility of dislocations during shoulder placement and improve the success rate of shoulder placement.
  • the embodiment of the present application provides a single crystal silicon shoulder placement method.
  • the method may include:
  • the cooling rate of the thermal field in the single crystal furnace is set to the first rate range, and the pulling speed of the crystal rod is set to the first speed range;
  • the cooling rate of the thermal field in the single crystal furnace is increased from the second rate range to the third rate range, and at the same time, the crystal rod is pulled The speed is increased from the first speed range to the third speed range; wherein the value of the shoulder length of the first interval is less than the value of the shoulder length of the second interval, and the value of the shoulder length of the second interval A value less than the shoulder length of the third interval;
  • the method also includes:
  • the first interval is that the shoulder length is greater than or equal to 1 mm and less than or equal to 60 mm, and the first rate range is that the cooling rate is greater than or equal to 2kw/h and less than or equal to 12kw/h,
  • the first speed range is that the pulling speed of the crystal ingot is greater than or equal to 25mm/h and less than or equal to 160mm/h;
  • the second interval is that the shoulder length is greater than 60mm and less than or equal to 150mm
  • the second speed range is that the cooling rate is greater than or equal to 3kw/h and less than or equal to 15kw/h
  • the second speed range The pulling speed of the crystal rod is greater than or equal to 45mm/h and less than or equal to 190mm/h;
  • the third interval is when the shoulder length is greater than 150mm
  • the third rate range is when the cooling rate is greater than or equal to 1kw/h and less than or equal to 10kw/h
  • the third speed range is when the crystal rod
  • the lifting speed is greater than or equal to 60mm/h and less than or equal to 200mm/h.
  • the method also includes:
  • the liquid opening distance is set to 15-20 mm.
  • the cooling amount of the thermal field in the single crystal furnace is 0-6.5kw;
  • the cooling amount of the thermal field in the single crystal furnace is 6.5-14kw;
  • the cooling amount of the thermal field in the single crystal furnace is 14-15 kw.
  • the method also includes:
  • the liquid mouth distance is set to 35-45mm, and the pulling speed of the crystal rod is set to 25-150mm/h;
  • the liquid mouth distance is set to 30-40mm, and the pulling speed of the crystal rod is set to 35-160mm/h;
  • the liquid mouth distance is set to 28-35mm, and the pulling speed of the crystal rod is set to 45-170mm/h.
  • the method also includes:
  • the liquid mouth distance is set to 25-30mm, and the pulling speed of the crystal rod is set to 55-180mm/h;
  • the liquid mouth distance is set to 20-28mm, and the pulling speed of the crystal rod is set to 60-190mm/h.
  • the method also includes:
  • the liquid mouth distance is set to 15-25mm, and the pulling speed of the crystal ingot is set to 60-200mm/h.
  • the method also includes:
  • the liquid mouth distance is set to 15-20mm, and the pulling speed of the crystal rod is set to 60-200mm/h.
  • the method also includes:
  • the embodiment of the present application provides a single crystal silicon rod, which adopts the above-mentioned shoulder placing method of single crystal silicon.
  • the angle of the shoulder vertex of the single crystal silicon rod is 45°-70°.
  • the shoulder of the single crystal silicon rod is an isosceles triangle.
  • any section of the shoulder perpendicular to the axial direction of the single crystal silicon rod select the two farthest points and connect them with the endpoint of the top of the shoulder. Between the two lines The included angle is 45°-70°.
  • this application provides a single crystal silicon shouldering method.
  • the shouldering length is obtained according to the target crystal rod diameter.
  • the cooling rate of the thermal field in the single crystal furnace is set to 2-12kw/h.
  • the pulling speed of the crystal rod is 25-160mm/h.
  • the shoulder length is 60-150mm
  • set the cooling rate of the thermal field in the single crystal furnace to 3-15kw/h
  • the pulling speed of the crystal rod to 45-190mm/h.
  • the shoulder length is greater than 150mm, set the single crystal furnace
  • the cooling rate of the internal thermal field is 1-10kw/h
  • the pulling speed of the crystal ingot is 60-200mm/h.
  • the shoulder placing process is carried out through the above process parameters, so that when the shoulder is placed, the shoulder top angle can be maintained at 45°-70 °, which reduces the probability of facets appearing during shoulder placement, further reduces the probability of dislocation, and improves the success rate of shoulder placement.
  • Figure 1 is a flow chart of a shoulder-resting method provided by an embodiment of the present application.
  • Figure 2 is a view of the top angle of the shoulder when the shoulder is placed according to an embodiment of the present application
  • Figure 3 is a flow chart of another shoulder-resting method provided by an embodiment of the present application.
  • Dislocation is a kind of line defect in the crystal. It is formed by the boundary between the slipped and unslipped regions in the crystal, or it is a defect characterized by the destruction of Burgers loop closure.
  • the original dislocations in the seed crystal and the dislocations introduced when the seed crystal is welded to the melt will continue to extend in the growing crystal.
  • Figure 1 is a step flow chart of a single crystal silicon shoulder placement method provided by an embodiment of the present application, including:
  • Step 101 Perform a shoulder setting operation on the crystal ingot according to the target crystal ingot diameter.
  • the temperature of the thermal field in the single crystal furnace needs to be lowered so that the crystal diameter gradually increases to the target size, which is the shoulder releasing operation. .
  • Step 102 When the shoulder length of the crystal ingot is in the first interval of the target range, set the cooling rate of the thermal field in the single crystal furnace to the first rate range, and at the same time set the pulling speed of the crystal ingot to the first speed range. .
  • the shoulder length is the vertical distance between the end of the seed crystal and the lower surface of the crystal during the shoulder placement process. "h” in Figure 2 is the shoulder length. , the longer the shoulder length, the larger the diameter of the target crystal rod obtained.
  • a in Figure 2 is the top angle of the shoulder. Since the angle between the ⁇ 111 ⁇ planes is 35.2°, if the top angle of the shoulder is greater than 70 degrees, ⁇ 111 ⁇ facets will appear during the shoulder placement process, and it is easy to cause positioning. Mistaken, leading to failure in shoulder placement. Therefore, during the shoulder placement process, different shoulder lengths are correspondingly set with different cooling rates and crystal rod pulling rates, so that when the shoulders are placed, the shoulder vertex angle is maintained at 45°-70° to avoid the formation of facets.
  • the first interval is that the shoulder length is greater than or equal to 1mm and less than or equal to 60mm
  • the corresponding first rate range can be that the cooling rate is greater than or equal to 2kw/h and less than or equal to 12kw/h.
  • the first cooling rate can be 3kw/h, 4kw/h, 5kw/h, 6kw/h, 7kw/h, 8kw/h, 9kw/h, 10kw/h, 11kw/h and 12kw/h, etc.
  • the first speed range is that the pulling speed of the crystal rod is greater than or equal to 25mm/h and less than or equal to 160mm/h. Specifically, it can be 25mm/h, 45mm/h, 65mm/h, 85mm/h, 105mm/h, 125mm/h. h2, 145mm/h and 160mm/h, etc.
  • Step 103 When the shoulder length of the crystal rod is in the second interval of the target range, increase the cooling rate of the thermal field in the single crystal furnace from the first rate range to the second rate range, and at the same time, increase the cooling rate of the thermal field in the single crystal furnace.
  • the pulling speed of the rod is increased from the first speed range to the second speed range.
  • the second interval can be that the shoulder length is greater than 60mm and less than or equal to 150mm, and the second rate range is that the cooling rate is greater than or equal to 3kw/h and less than or equal to 15kw/h.
  • the second rate range is that the cooling rate is greater than or equal to 3kw/h and less than or equal to 15kw/h.
  • it can be 3kw/ h, 4kw/h, 5kw/h, 6kw/h, 7kw/h, 8kw/h, 9kw/h, 10kw/h, 12kw/h and 15kw/h, etc.
  • the second speed range is the pulling speed of the crystal rod Greater than or equal to 45mm/h and less than or equal to 190mm/h, the pulling speed of the crystal rod can be 45mm/h, 65mm/h, 85mm/h, 105mm/h, 125mm/h, 145mm/h, 165mm/h, 185mm/h and 190mm/h, etc.
  • the cooling rate can be adjusted from the first speed range to the second speed range
  • the pulling speed of the crystal rod can be adjusted from the first speed range It is the second speed range to continue to keep the shoulder apex angle between 45° and 70° to avoid the formation of facets.
  • Step 104 When the shoulder length of the crystal ingot is in the third interval of the target range, increase the cooling rate of the thermal field in the single crystal furnace from the second rate range to the third rate range, and simultaneously move the crystal ingot The lifting speed is increased from the second speed range to the third speed range; wherein, the value of the shoulder length of the first interval is less than the value of the shoulder length of the second interval, and the value of the shoulder length of the second interval is The value of the length is smaller than the value of the shoulder length of the third interval.
  • the third interval can be that the shoulder length is greater than 150mm, and the third rate range is that the cooling rate is greater than or equal to 1kw/h and less than or equal to 10kw/h, for example, it can be 1kw/h or 2kw/h. , 3kw/h, 4kw/h, 5kw/h, 6kw/h, 7kw/h, 8kw/h, 9kw/h and 10kw/h, etc.
  • the third speed range is that the pulling speed of the crystal rod is greater than or equal to 60mm/ h and less than or equal to 200mm/h, for example, it can be: 60mm/h, 80mm/h, 100mm/h, 120mm/h, 140mm/h, 160mm/h, 180mm/h and 200mm/h. This is to ensure that when the shoulder length reaches the third interval, the shoulder apex angle continues to remain between 45° and 70° during the shouldering process to avoid defects such as facets and dislocations that affect the growth of the crystal ingot.
  • Step 105 When the crystal ingot diameter of the crystal ingot is the target crystal ingot diameter, end the shoulder releasing operation.
  • the shouldering operation when the shouldering operation is carried out until the diameter of the obtained crystal has reached close to the target crystal rod diameter, the shouldering operation can be ended, and the next step of shouldering and equal-diameter growth is entered to complete the single crystal pulling. After the manufacturing process, the crystal rod with the target diameter is obtained.
  • This application gradually increases the cooling rate of the thermal field in the single crystal furnace and the pulling speed of the crystal rod according to the length of the shoulder during the shoulder placing process, so that the shoulder apex angle is always maintained at 45°-70° during the shoulder placing process.
  • this application controls the cooling amount, pulling speed, etc., so that the edge lines of the vertical cross-section of the shoulder change approximately linearly.
  • the shoulder top angle is between 45° and 70°, it can avoid or reduce the position of the facets caused by placing the shoulders. Wrong, the success rate of shoulder placement has been improved.
  • the shoulder-resting operation is usually carried out by placing the shoulders flat. The top angle of the shoulder is about 120°. When performing the shoulder-resting operation at this angle, dislocation and dislocation multiplication may occur. It may even become polycrystalline, causing the shoulder placement to fail. Compared with the prior art solution, this application improves the success rate of the shoulder-resting operation.
  • this application provides a single crystal silicon shouldering method.
  • the shouldering length is obtained according to the target crystal rod diameter.
  • the cooling rate of the thermal field in the single crystal furnace is set to 2-12kw/h.
  • the pulling speed of the crystal rod is 25-160mm/h.
  • the shoulder length is 60-150mm
  • set the cooling rate of the thermal field in the single crystal furnace to 3-15kw/h
  • the pulling speed of the crystal rod to 45-190mm/h.
  • the shoulder length is greater than 150mm, set the single crystal furnace
  • the cooling rate of the internal thermal field is 1-10kw/h
  • the pulling speed of the crystal ingot is 60-200mm/h.
  • the shoulder placing process is carried out through the above process parameters, so that when the shoulder is placed, the shoulder top angle can be maintained at 45°-70 °, which reduces the probability of facets appearing during shoulder placement, further reduces the probability of dislocation, and improves the success rate of shoulder placement.
  • Figure 3 is a step flow chart of yet another single crystal silicon shoulder placement method provided by an embodiment of the present application, including:
  • Step 201 According to the target diameter of the crystal ingot, perform a shoulder setting operation on the crystal ingot.
  • step 101 For details of this step, please refer to step 101 and will not be described again here.
  • Step 202 When the shoulder length of the crystal ingot is in the first interval of the target range, set the cooling rate of the thermal field in the single crystal furnace to the first rate range, and at the same time set the pulling speed of the crystal ingot to the first speed range. , and set the liquid port distance to 30-45mm.
  • the first speed range and the first speed range are set with reference to step 102.
  • the distance between the liquid openings is adjusted synchronously.
  • the liquid mouth distance is in the range of 30-45mm, for example, it can be 30mm, 33mm, 35mm, 37mm, 39mm, 41mm, 43mm and 45mm, etc.
  • One speed range ensures the largest cooling amount in the first speed range and improves the success rate of shoulder release.
  • Step 203 When the shoulder length of the crystal ingot is in the second interval of the target range, increase the cooling rate of the thermal field in the single crystal furnace from the first rate range to the second rate range, and simultaneously move the crystal ingot The lifting speed is increased from the first speed range to the second speed range, and the liquid port distance is set to 20-35mm.
  • the second speed range and the second speed range are set with reference to step 103.
  • the distance between the liquid openings is adjusted synchronously,
  • the range of the liquid mouth distance is 20-35mm.
  • it can be 20mm, 22mm, 24mm, 26mm, 28mm, 31mm, 33mm, 35mm, etc.
  • the speed can reach the second speed range, ensuring a large cooling amount in the second speed range and improving the success rate of shoulder release.
  • Step 204 When the shoulder length of the crystal ingot is in the third interval of the target range, increase the cooling rate of the thermal field in the single crystal furnace from the second rate range to the third rate range, and simultaneously move the crystal ingot The lifting speed is increased from the second speed range to the third speed range, and the liquid mouth distance is set to 15-20mm; wherein the value of the shoulder length of the first interval is less than the shoulder length of the second interval value, the value of the shoulder length of the second interval is smaller than the value of the shoulder length of the third interval.
  • the third speed range and the third speed range are set with reference to step 104.
  • the distance between the liquid ports is adjusted synchronously.
  • the range of the liquid port distance is 15-20mm, for example, it can be 15mm, 16mm, 17mm, 18mm, 19mm and 20mm, etc.
  • Step 205 When the crystal rod diameter of the crystal rod is the target crystal rod diameter, end the shoulder releasing operation.
  • step 105 For details of this step, please refer to step 105 and will not be described again here.
  • the method also includes:
  • Step 206 During the shoulder placing operation, control the top angle of the shoulder to 45°-70°.
  • the shoulder apex angle can be controlled to be maintained at 45°-70°. This is to reduce and avoid the appearance of ⁇ 111 ⁇ facets during shoulder placement and improve the success rate of shoulder placement.
  • the cooling amount of the thermal field in the single crystal furnace is 0-6.5kw; when the shoulder length of the crystal rod is in the target range When the second interval of the single crystal furnace, the cooling amount of the thermal field in the single crystal furnace is 6.5-14kw; when the shoulder length of the crystal rod is in the third interval of the target range, the cooling amount of the thermal field in the single crystal furnace is 14-15kw.
  • the achievable cooling amount is 0-6.5kw under the first rate range.
  • the faster the cooling rate the faster the growth of the shoulder length, for example , when the cooling rate is 4kw/h, the shoulder length grows to 60mm, which takes 1 hour; when the cooling rate is 8kw/h, the shoulder length grows to 60mm, which only takes about 0.8 hours.
  • the shoulder length of the crystal rod When it is in the second interval of the target range, under the second rate range, the cooling amount that can be achieved is 6.5-14kw.
  • the shoulder length of the crystal ingot is in the third interval of the target range, under the third rate range, it can be achieved
  • the cooling capacity is 14-15kw.
  • the amount of cooling during the shoulder placement process in this application is greater than that of the prior art, so that the temperature of the equal diameter head is relatively different. Lower than the original process, the oxygen content in the head of the single crystal grown with this new process is reduced, improving the crystal quality.
  • the method also includes:
  • Step 207 When the shoulder length is 1-30mm, set the liquid mouth distance to 35-45mm, and set the pulling speed of the crystal rod to 25-150mm/h.
  • the cooling rate in the single crystal furnace can be set with reference to step 102.
  • the liquid mouth distance can be set to 35-45mm, for example, it can be set to 35mm, 37mm, 39mm, 41mm, 42mm, 43mm, 44mm and 45mm, etc.
  • the pulling speed of the crystal rod can be set to 25-150mm/h, for example Can be 25mm/h, 35mm/h, 45mm/h, 55mm/h, 65mm/h, 75mm/h, 85mm/h, 95mm/h, 105mm/h, 115mm/h, 125mm/h, 135mm/h, 145mm/h and 150mm/h, etc.
  • the cooling rate, lifting speed and liquid mouth distance within the above range can further ensure that the shoulder top angle is between 45°-70°.
  • Step 208 When the shoulder length is 30-60mm, set the liquid mouth distance to 30-40mm, and set the pulling speed of the crystal rod to 35-160mm/h.
  • the cooling rate in the single crystal furnace can be set with reference to step 102.
  • the liquid port distance can be set to 30-40mm, for example, it can be set to 30mm, 32mm, 34mm, 35mm, 36mm, 37mm, 38mm, 39mm and 40mm, etc.
  • the pulling speed of the crystal rod can be set to 35-160mm/h, for example, it can be 35mm/h, 45mm/h, 55mm/h, 65mm/h, 75mm/h, 85mm/h, 95mm/h, 105mm/h, 115mm/h, 125mm/h, 135mm/h, 150mm/h and 160mm/h, etc., within the above range, the cooling rate, pulling speed and liquid
  • the mouth distance can further ensure that the shoulder top angle is between 45° and 70°.
  • Step 209 When the shoulder length is 60-90mm, set the liquid mouth distance to 28-35mm, and set the pulling speed of the crystal rod to 45-170mm/h.
  • the cooling rate in the single crystal furnace can be referred to step 102.
  • setting, and also set the liquid mouth distance to 28-35mm for example, it can be set to 28mm, 29mm, 30mm, 31mm, 32mm, 33mm, 34mm and 35mm, etc.
  • the pulling speed of the crystal rod can be set to 45-170mm/h, for example Can be 45mm/h, 55mm/h, 65mm/h, 75mm/h, 85mm/h, 95mm/h, 105mm/h, 115mm/h, 125mm/h, 135mm/h, 145mm/h, 160mm/h and 170mm/h, etc.
  • the cooling rate, lifting speed and liquid mouth distance within the above range can further ensure that the shoulder top angle is between 45°-70°.
  • Step 210 When the shoulder length is 90-120 mm, set the liquid mouth distance to 25-30 mm, and set the pulling speed of the crystal rod to 55-190 mm/h.
  • the cooling rate in the single crystal furnace can refer to the steps 103 setting
  • the liquid mouth distance can be set to 25-30mm at the same time, for example, it can be set to 25mm, 26mm, 27mm, 28mm, 28.5mm, 29mm, 29.5mm and 30mm, etc.
  • the pulling speed of the crystal rod can be set to 55-30mm.
  • 190mm/h for example, it can be 55mm/h, 65mm/h, 75mm/h, 85mm/h, 95mm/h, 105mm/h, 115mm/h, 125mm/h, 135mm/h, 145mm/h, 155mm/h , 170mm/h and 190mm/h, etc.
  • the cooling rate, pulling speed and liquid port distance in the single crystal furnace within the above range can further ensure that the shoulder apex angle is 45°-70°.
  • Step 211 When the shoulder length is 120-150 mm, set the liquid mouth distance to 20-28 mm, and set the pulling speed of the crystal rod to 60-190 mm/h.
  • the cooling rate in the single crystal furnace can be set with reference to step 103.
  • the liquid mouth distance can be set to 20-28mm, for example, it can be set to 20mm, 21mm, 22mm, 23mm, 24mm, 25mm, 26mm, 27mm, and 28mm, etc.
  • the pulling speed of the crystal rod can be set to 60-190mm/h.
  • it can be 60mm/h, 70mm/h, 80mm/h, 90mm/h, 100mm/h, 110mm/h, 120mm/h, 130mm/h, 140mm/h, 150mm/h, 160mm/h, 170mm/h , 180mm/h and 190mm/h, etc.
  • the cooling rate, lifting speed and liquid mouth distance within the above range can further ensure that the shoulder top angle is 45°-70°.
  • Step 212 When the shoulder length is 150-180 mm, set the liquid mouth distance to 15-25 mm, and set the pulling speed of the crystal rod to 60-200 mm/h.
  • the shoulder length when the shoulder length is 150-180mm, for example, it is 150mm, 155mm, 160mm, 165mm, 170mm, 175mm, and 180mm, etc.
  • the cooling rate in the single crystal furnace can be set by referring to step 103.
  • set the liquid port distance to 15-25mm. For example, it can be set to 15mm, 17mm, 19mm, 20mm, 21mm, 22mm. , 23mm, 24mm and 25mm, etc.
  • the pulling speed of the crystal rod can be set to 60-200mm/h, for example, 60mm/h, 70mm/h, 80mm/h, 90mm/h, 100mm/h, 110mm/h, 120mm/h, 130mm/h, 140mm/h, 150mm/h, 160mm/h, 170mm/h, 180mm/h, 190mm/h and 200mm/h, etc., within the above range, the cooling rate, pulling speed and liquid The mouth distance can further ensure that the shoulder top angle is between 45° and 70°.
  • Step 213 When the shoulder length is 180 mm, set the liquid mouth distance to 15-20 mm, and set the pulling speed of the crystal rod to 60-200 mm/h.
  • the cooling rate in the single crystal furnace can be set with reference to step 104.
  • the liquid port distance is set to 15-20mm, for example, it can be set to 15mm, 16mm, 17mm, 18mm, 19mm and 20mm, etc.
  • the pulling speed of the crystal rod can be set to 60-200mm/h, for example, it can be 60mm/h, 70mm/h, 80mm/h, 90mm/h, 100mm/h, 110mm/h, 120mm/ h, 130mm/h, 140mm/h, 150mm/h, 160mm/h, 170mm/h, 180mm/h, 190mm and 200mm/h, etc.
  • the cooling rate, pulling speed and liquid mouth distance within the above range can be further Make sure the top angle of the shoulders is between 45° and 70°.
  • the method also includes:
  • Step 214 during the shoulder releasing process, set the crystal rotation to 8-12 r/min, the crucible rotation to 5-9 r/min, and the crucible rotation direction is opposite to the crystal rotation direction.
  • the crystal rotation refers to the rotation speed of the crystal
  • the crucible rotation refers to the rotation speed of the crucible in the single crystal furnace.
  • the purpose of the crystal rotation and crucible rotation is to suppress the thermal convection of the melt and provide a stable thermal system for single crystal growth.
  • the rotation of the crystal rotation and crucible is conducive to the uniform distribution of impurities.
  • the crystal rotation and crucible are set in opposite directions to ensure that single crystals can be drawn. crystal.
  • Table 1 is an improved shoulder placing process parameter table provided by the embodiment of the present application.
  • the shoulder length is the vertical distance between the end of the seed crystal and the lower surface of the crystal when the shoulder is placed during the shoulder placement process.
  • “h” in Figure 2 is the shoulder length. The longer the shoulder length The longer, the larger the diameter of the target crystal rod obtained.
  • the cooling amount is the difference between the current power of the single crystal furnace and the power at the beginning of shouldering during the shouldering process.
  • the liquid mouth distance is between the heat conduction cylinder in the single crystal furnace and the liquid level of the melt in the single crystal furnace.
  • the vertical distance of , the pulling speed is the speed when pulling the crystal rod
  • the crystal rotation is the rotation speed of the crystal
  • the crucible rotation is the rotation speed of the crucible in the single crystal furnace.
  • the crucible can be a graphite crucible or a quartz crucible, used to hold polysilicon raw materials.
  • the liquid level of the melt can be controlled at a position through the crucible lifting system, and the liquid mouth distance can be adjusted by adjusting the position of the crucible.
  • the guide tube is used to separate the inside and outside of the thermal field, thereby speeding up the single crystal pulling speed, and also plays a role in guiding the flow (internal argon gas).
  • Table 2 is a shoulder-resting parameter table in the prior art. The definitions of the parameters in the table are the same as those in Table 1.
  • Table 4 shows the comparison of the success rate of shoulder placement between the improved process of this application and the original process.
  • the comparison shoulder apex angle is 90°-120°
  • the shoulder apex angle is 45°-70°. It can be seen that compared with the original process, the shoulder placing method of the present application is better The success rate of shoulder placement has been improved.
  • this application provides a single crystal silicon shouldering method.
  • the shouldering length is obtained according to the target crystal rod diameter.
  • the cooling rate of the thermal field in the single crystal furnace is set to 2-12kw/h.
  • the pulling speed of the crystal rod is 25-160mm/h.
  • the shoulder length is 60-150mm
  • set the cooling rate of the thermal field in the single crystal furnace to 3-15kw/h
  • the pulling speed of the crystal rod to 45-190mm/h.
  • the shoulder length is greater than 150mm
  • set the single crystal furnace The cooling rate of the internal thermal field is 1-10kw/h, and the pulling speed of the crystal ingot is 60-200mm/h.
  • the shoulder is placed through the above process parameters, so that the shoulder top angle can be maintained at 45°-70° when the shoulder is placed. , reducing the probability of facets appearing during shoulder placement, further reducing the probability of dislocation, and improving the success rate of shoulder placement.
  • the embodiment of the present application provides a single crystal silicon rod, which adopts the above-mentioned shoulder placing method of single crystal silicon.
  • the angle of the shoulder vertex of the single crystal silicon rod is 45°-70°.
  • the shoulder of the single crystal silicon rod is an isosceles triangle.
  • the shoulder angle of the single crystal silicon rod produced by the single crystal silicon shoulder placing method of the present application is between 45° and 70°.
  • any section of the shoulder perpendicular to the axial direction of the crystal rod select the two farthest points and connect them with the endpoints of the top of the shoulder.
  • the angle between the two lines is 45-70 degrees.
  • the cross-section of the shoulder perpendicular to the axial direction of the crystal rod is a circular surface, and the angle between the two endpoints in the diameter direction of the circular surface and the top endpoint is 45-70 degrees.
  • a certain instantaneous cross-section may not be circular, and the angle between the two farthest endpoints on the cross-section and the top endpoint may not be within this range. Therefore, the present invention is limited to any selected cross-section.
  • the two farthest points on the selected cross-section are connected with the end point of the top of the shoulder.
  • the angle between the two lines is 45°- 70°, which is within the protection scope of the present invention.
  • the extension line of the longitudinal section of the shoulder of the single crystal silicon rod forms an isosceles triangle, but in some other cases, such as fluctuations in process parameters, etc.
  • the hypotenuse where the shoulder is located is not a standard straight line, but may be a gently connected fold line forming the shoulder, that is, the cross-sectional edge in the axial direction of the shoulder may show some fold lines. Select a point on the fold line and connect it to the vertex of the shoulder.
  • the angle between the connecting line and the vertical line in the axial direction of the crystal rod is 22.5°-35°, which is half of the angle 45°-70°. , reducing the probability of facets appearing and further reducing the probability of dislocations.

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Abstract

The present application provides a monocrystalline silicon shouldering method, comprising: acquiring a shouldering length according to a target ingot diameter, and when the shouldering length of an ingot is in a first interval of a target range, setting the cooling rate of a thermal field in a mono-crystal furnace to be a first rate range, and setting the pulling speed of the ingot to be a first speed range; when the shouldering length of the ingot is in a second interval of the target range, increasing the cooling rate from the first rate range to a second rate range, and increasing the pulling speed from the first speed range to a second speed range; and when the shouldering length is in a third interval of the target range, increasing the cooling rate from the second rate range to a third rate range, and increasing the pulling speed from the second speed range to a third speed range. Shouldering is performed by means of the method, so that a shoulder vertex angle can be kept at 45°-70° during shouldering, thereby reducing the probability of {111} facets appearing in a shouldering process, further reducing the probability of dislocation, and improving the success rate of shouldering.

Description

一种单晶硅放肩方法A shoulder-laying method for single crystal silicon
相关申请的交叉引用Cross-references to related applications
本公开要求在2022年9月5日提交中国专利局、申请号为202211083122.2、名称为“一种单晶硅放肩方法”的中国专利申请的优先权，其全部内容通过引用结合在本公开中。This disclosure claims priority to the Chinese patent application filed with the China Patent Office on September 5, 2022, with application number 202211083122.2 and titled "A method for shoulder placement of single crystal silicon", the entire content of which is incorporated into this disclosure by reference. .
技术领域Technical field
本申请实施例涉及光伏技术领域，尤其涉及一种单晶硅放肩方法。The embodiments of the present application relate to the field of photovoltaic technology, and in particular, to a single crystal silicon shoulder placement method.
背景技术Background technique
直拉法(Czochralski，Cz法)是常用的晶体生长方法之一，通过将原料硅在单晶炉中加热融化，再将棒状的籽晶浸入融液中，使得融液中的硅原子沿籽晶上硅原子的排列结构在固液交界面上形成规则的结晶，从而形成单晶体，具体的，直拉法通常包括：调温、引晶、放肩、转肩、等径、收尾、加料等工艺步骤。The Czochralski method (Cz method) is one of the commonly used crystal growth methods. The raw silicon is heated and melted in a single crystal furnace, and then the rod-shaped seed crystal is immersed in the melt, so that the silicon atoms in the melt grow along the seeds. The arrangement structure of silicon atoms on the crystal forms regular crystals at the solid-liquid interface, thereby forming a single crystal. Specifically, the Czochralski method usually includes: temperature adjustment, seeding, shoulder placement, shoulder rotation, equal diameter, finishing, feeding, etc. Process steps.
放肩是指在引晶完成后通过降低拉速和降低温度使晶体直径逐渐长大至目标直径，目前在放肩时通常以肩部顶角为钝角且晶棒的提拉速度较慢的方式进行放肩操作。Shoulder placement means that after seeding is completed, the crystal diameter is gradually grown to the target diameter by reducing the pulling speed and temperature. Currently, when shoulder placement is performed, the top angle of the shoulder is usually an obtuse angle and the pulling speed of the crystal ingot is slow. Perform shoulder-resting maneuvers.
上述方式容易导致晶体出现位错，放肩失败，并且降温量较小，导致晶体头部的氧含量高，影响晶体品质。The above method can easily lead to dislocations in the crystal, failure of shoulder placement, and a small amount of cooling, resulting in high oxygen content in the head of the crystal, affecting the quality of the crystal.
发明内容Contents of the invention
本申请提供一种单晶硅放肩方法，旨在减少放肩时发生位错的可能，提高放肩成功率。This application provides a single crystal silicon shoulder placement method, aiming to reduce the possibility of dislocations during shoulder placement and improve the success rate of shoulder placement.
本申请实施例提供了一种单晶硅放肩方法，该方法可以包括：The embodiment of the present application provides a single crystal silicon shoulder placement method. The method may include:
根据目标晶棒直径，对晶棒进行放肩操作；According to the target crystal rod diameter, carry out the shoulder setting operation on the crystal rod;
在所述晶棒的放肩长度处于目标范围的第一区间时，设定单晶炉内热场的降温速率为第一速率范围，同时设置晶棒的提拉速度为第一速度范围；When the shoulder length of the crystal rod is in the first interval of the target range, the cooling rate of the thermal field in the single crystal furnace is set to the first rate range, and the pulling speed of the crystal rod is set to the first speed range;
在所述晶棒的放肩长度处于目标范围的第二区间时，将所述单晶炉内热 场的降温速率由所述第一速率范围提升至第二速率范围，同时将晶棒的提拉速度由第一速度范围提升至第二速度范围；When the shoulder length of the crystal rod is in the second interval of the target range, heat the single crystal furnace The cooling rate of the field is increased from the first rate range to the second rate range, and the pulling speed of the crystal rod is increased from the first speed range to the second speed range;
在所述晶棒的放肩长度处于目标范围的第三区间时，将所述单晶炉内热场的降温速率由所述第二速率范围提升至第三速率范围，同时将晶棒的提拉速度由第一速度范围提升至第三速度范围；其中，所述第一区间的放肩长度的值小于所述第二区间的放肩长度的值，所述第二区间的放肩长度的值小于所述第三区间的放肩长度的值；When the shoulder length of the crystal rod is in the third interval of the target range, the cooling rate of the thermal field in the single crystal furnace is increased from the second rate range to the third rate range, and at the same time, the crystal rod is pulled The speed is increased from the first speed range to the third speed range; wherein the value of the shoulder length of the first interval is less than the value of the shoulder length of the second interval, and the value of the shoulder length of the second interval A value less than the shoulder length of the third interval;
在所述晶棒的晶棒直径为所述目标晶棒直径时，结束放肩操作。When the crystal rod diameter of the crystal rod is the target crystal rod diameter, the shoulder releasing operation ends.
可选地，所述方法还包括：Optionally, the method also includes:
在放肩操作的过程中，控制肩部顶角的角度为45°-70°。During the shoulder-resting operation, control the top angle of the shoulder to 45°-70°.
可选地，所述第一区间为所述放肩长度大于或等于1mm且小于或等于60mm，所述第一速率范围为所述降温速率大于或等于2kw/h且小于或等于12kw/h，所述第一速度范围为所述晶棒的提拉速度大于或等于25mm/h且小于或等于160mm/h；Optionally, the first interval is that the shoulder length is greater than or equal to 1 mm and less than or equal to 60 mm, and the first rate range is that the cooling rate is greater than or equal to 2kw/h and less than or equal to 12kw/h, The first speed range is that the pulling speed of the crystal ingot is greater than or equal to 25mm/h and less than or equal to 160mm/h;
所述第二区间为所述放肩长度大于60mm且小于或等于150mm，所述第二速率范围为所述降温速率大于或等于3kw/h且小于或等于15kw/h，所述第二速度范围为所述晶棒的提拉速度大于或等于45mm/h且小于或等于190mm/h；The second interval is that the shoulder length is greater than 60mm and less than or equal to 150mm, the second speed range is that the cooling rate is greater than or equal to 3kw/h and less than or equal to 15kw/h, the second speed range The pulling speed of the crystal rod is greater than or equal to 45mm/h and less than or equal to 190mm/h;
所述第三区间为所述放肩长度大于150mm，所述第三速率范围为所述降温速率大于或等于1kw/h且小于或等于10kw/h，所述第三速度范围为所述晶棒的提拉速度大于或等于60mm/h且小于或等于200mm/h。The third interval is when the shoulder length is greater than 150mm, the third rate range is when the cooling rate is greater than or equal to 1kw/h and less than or equal to 10kw/h, and the third speed range is when the crystal rod The lifting speed is greater than or equal to 60mm/h and less than or equal to 200mm/h.
可选地，所述方法还包括：Optionally, the method also includes:
在所述晶棒的放肩长度处于目标范围的第一区间时，设置液口距为30-45mm；When the shoulder length of the crystal rod is in the first interval of the target range, set the liquid mouth distance to 30-45mm;
在所述晶棒的放肩长度处于目标范围的第二区间时，设置液口距为20-35mm；When the shoulder length of the crystal rod is in the second interval of the target range, set the liquid mouth distance to 20-35mm;
在所述晶棒的放肩长度处于目标范围的第三区间时，设置液口距为15-20mm。When the shoulder length of the crystal rod is in the third interval of the target range, the liquid opening distance is set to 15-20 mm.
可选地，在所述晶棒的放肩长度处于目标范围的第一区间时，所述单晶炉内热场的降温量为0-6.5kw； Optionally, when the shoulder length of the crystal rod is in the first interval of the target range, the cooling amount of the thermal field in the single crystal furnace is 0-6.5kw;
在所述晶棒的放肩长度处于目标范围的第二区间时，所述单晶炉内热场的降温量为6.5-14kw；When the shoulder length of the crystal rod is in the second interval of the target range, the cooling amount of the thermal field in the single crystal furnace is 6.5-14kw;
在所述晶棒的放肩长度处于目标范围的第三区间时，所述单晶炉内热场的降温量为14-15kw。When the shoulder length of the crystal rod is in the third interval of the target range, the cooling amount of the thermal field in the single crystal furnace is 14-15 kw.
可选地，所述方法还包括：Optionally, the method also includes:
在所述放肩长度为1-30mm时，设置液口距为35-45mm，同时设置晶棒的提拉速度为25-150mm/h；When the shoulder length is 1-30mm, the liquid mouth distance is set to 35-45mm, and the pulling speed of the crystal rod is set to 25-150mm/h;
在所述放肩长度为30-60mm时，设置液口距为30-40mm，同时设置晶棒的提拉速度为35-160mm/h；When the shoulder length is 30-60mm, the liquid mouth distance is set to 30-40mm, and the pulling speed of the crystal rod is set to 35-160mm/h;
在所述放肩长度为60-90mm时，设置液口距为28-35mm，同时设置晶棒的提拉速度为45-170mm/h。When the shoulder length is 60-90mm, the liquid mouth distance is set to 28-35mm, and the pulling speed of the crystal rod is set to 45-170mm/h.
可选地，所述方法还包括：Optionally, the method also includes:
在所述放肩长度为90-120mm时，设置液口距为25-30mm，同时设置晶棒的提拉速度为55-180mm/h；When the shoulder length is 90-120mm, the liquid mouth distance is set to 25-30mm, and the pulling speed of the crystal rod is set to 55-180mm/h;
在所述放肩长度为120-150mm时，设置液口距为20-28mm，同时设置晶棒的提拉速度为60-190mm/h。When the shoulder length is 120-150mm, the liquid mouth distance is set to 20-28mm, and the pulling speed of the crystal rod is set to 60-190mm/h.
可选地，所述方法还包括：Optionally, the method also includes:
在所述放肩长度为150-180mm时，设置液口距为15-25mm，同时设置晶棒的提拉速度为60-200mm/h。When the shoulder length is 150-180mm, the liquid mouth distance is set to 15-25mm, and the pulling speed of the crystal ingot is set to 60-200mm/h.
可选地，所述方法还包括：Optionally, the method also includes:
在所述放肩长度为180mm时，设置液口距为15-20mm，同时设置晶棒的提拉速度为60-200mm/h。When the shoulder length is 180mm, the liquid mouth distance is set to 15-20mm, and the pulling speed of the crystal rod is set to 60-200mm/h.
可选地，所述方法还包括：Optionally, the method also includes:
在放肩过程中，设定晶转为8-12r/min，埚转5-9r/min，且所述埚转的方向与所述晶转的方向相反。During the shoulder releasing process, set the crystal rotation to 8-12 r/min, the crucible rotation to 5-9 r/min, and the crucible rotation direction is opposite to the crystal rotation direction.
本申请实施例提供了一种单晶硅棒，采用上述的单晶硅放肩方法，所述单晶硅棒的肩部顶角的角度为45°-70°。The embodiment of the present application provides a single crystal silicon rod, which adopts the above-mentioned shoulder placing method of single crystal silicon. The angle of the shoulder vertex of the single crystal silicon rod is 45°-70°.
可选地，所述单晶硅棒肩部为等腰三角形。Optionally, the shoulder of the single crystal silicon rod is an isosceles triangle.
可选地，在垂直于所述单晶硅棒的轴向方向的肩部的任一截面上，选取距离最远的两个点，与肩部顶部的端点进行连线，两条线之间的夹角为45°-70°。 Optionally, on any section of the shoulder perpendicular to the axial direction of the single crystal silicon rod, select the two farthest points and connect them with the endpoint of the top of the shoulder. Between the two lines The included angle is 45°-70°.
综上，本申请提供一种单晶硅放肩方法，根据目标晶棒直径获取放肩长度，当放肩长度处于1-60mm时，设置单晶炉内热场的降温速率为2-12kw/h，晶棒的提拉速度为25-160mm/h。当放肩长度处于60-150mm，设置单晶炉内热场的降温速率为3-15kw/h，晶棒的提拉速度为45-190mm/h，当放肩长度大于150mm时，设置单晶炉内热场的降温速率为1-10kw/h，晶棒的提拉速度为60-200mm/h，通过上述工艺参数进行放肩过程，使得放肩时，肩部顶角可以保持在45°-70°，减小了放肩过程中小面出现的概率，进一步降低发生位错的概率，提高了放肩成功率。In summary, this application provides a single crystal silicon shouldering method. The shouldering length is obtained according to the target crystal rod diameter. When the shouldering length is 1-60mm, the cooling rate of the thermal field in the single crystal furnace is set to 2-12kw/h. , the pulling speed of the crystal rod is 25-160mm/h. When the shoulder length is 60-150mm, set the cooling rate of the thermal field in the single crystal furnace to 3-15kw/h, and the pulling speed of the crystal rod to 45-190mm/h. When the shoulder length is greater than 150mm, set the single crystal furnace The cooling rate of the internal thermal field is 1-10kw/h, and the pulling speed of the crystal ingot is 60-200mm/h. The shoulder placing process is carried out through the above process parameters, so that when the shoulder is placed, the shoulder top angle can be maintained at 45°-70 °, which reduces the probability of facets appearing during shoulder placement, further reduces the probability of dislocation, and improves the success rate of shoulder placement.
上述说明仅是本公开技术方案的概述，为了能够更清楚了解本公开的技术手段，而可依照说明书的内容予以实施，并且为了让本公开的上述和其它目的、特征和优点能够更明显易懂，以下特举本公开的具体实施方式。The above description is only an overview of the technical solutions of the present disclosure. In order to have a clearer understanding of the technical means of the present disclosure, they can be implemented according to the content of the description, and in order to make the above and other objects, features and advantages of the present disclosure more obvious and understandable. , the specific implementation modes of the present disclosure are specifically listed below.
附图说明Description of the drawings
为了更清楚地说明本公开实施例或相关技术中的技术方案，下面将对实施例或相关技术描述中所需要使用的附图作一简单地介绍，显而易见地，下面描述中的附图是本公开的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。In order to more clearly illustrate the technical solutions in the embodiments of the present disclosure or related technologies, a brief introduction will be made below to the drawings that need to be used in the description of the embodiments or related technologies. Obviously, the drawings in the following description are of the present invention. For some disclosed embodiments, those of ordinary skill in the art can also obtain other drawings based on these drawings without exerting creative efforts.
附图用于更好地理解本申请，不构成对本申请的不当限定。其中：The accompanying drawings are used for a better understanding of the present application and do not constitute an undue limitation of the present application. in:
图1是本申请实施例提供的一种放肩方法流程图；Figure 1 is a flow chart of a shoulder-resting method provided by an embodiment of the present application;
图2是本申请实施例提供的一种放肩时肩部顶角图；Figure 2 is a view of the top angle of the shoulder when the shoulder is placed according to an embodiment of the present application;
图3是本申请实施例提供的另一种放肩方法流程图。Figure 3 is a flow chart of another shoulder-resting method provided by an embodiment of the present application.
具体实施例Specific embodiments
为使本公开实施例的目的、技术方案和优点更加清楚，下面将结合本公开实施例中的附图，对本公开实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例是本公开一部分实施例，而不是全部的实施例。基于本公开中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本公开保护的范围。In order to make the purpose, technical solutions and advantages of the embodiments of the present disclosure clearer, the technical solutions in the embodiments of the present disclosure will be clearly and completely described below in conjunction with the drawings in the embodiments of the present disclosure. Obviously, the described embodiments These are some embodiments of the present disclosure, but not all embodiments. Based on the embodiments in this disclosure, all other embodiments obtained by those of ordinary skill in the art without making creative efforts fall within the scope of protection of this disclosure.
下面对本申请实施例提供的方案中涉及的一些概念和/或术语做一下解释说明。 Some concepts and/or terms involved in the solutions provided by the embodiments of this application are explained below.
位错，位错是晶体中的一种线缺陷，它是晶体中已滑移与未滑移区之间的边界构成，或是以伯格斯回路闭合性破坏来表征的缺陷。在硅单晶生长的开始阶段，籽晶中原有的位错和籽晶与熔体熔接时引入的位错，在生长的晶体中会继续延伸，在晶体生长过程中，固液界面附近存在不熔固态颗粒，也易引入位错，尤其当热场温度梯度较大，在晶体中产生较大的热应力时，更易产生位错并使其增殖。Dislocation is a kind of line defect in the crystal. It is formed by the boundary between the slipped and unslipped regions in the crystal, or it is a defect characterized by the destruction of Burgers loop closure. At the beginning of the growth of silicon single crystal, the original dislocations in the seed crystal and the dislocations introduced when the seed crystal is welded to the melt will continue to extend in the growing crystal. During the crystal growth process, there are inconsistencies near the solid-liquid interface. Molten solid particles are also prone to introduce dislocations, especially when the thermal field temperature gradient is large and large thermal stress is generated in the crystal, dislocations are more likely to be generated and multiplied.
图1是本申请实施例提供的一种单晶硅放肩方法的步骤流程图，包括：Figure 1 is a step flow chart of a single crystal silicon shoulder placement method provided by an embodiment of the present application, including:
步骤101，根据目标晶棒直径，对晶棒进行放肩操作。Step 101: Perform a shoulder setting operation on the crystal ingot according to the target crystal ingot diameter.
在本申请实施例中，在拉晶过程中，当引晶生长完成后，需要降低单晶炉内的热场的温度，使晶体直径渐渐增大到目标所需的大小，即为放肩操作。所需的目标晶棒的直径越大，放肩操作的过程越长。In the embodiment of the present application, during the crystal pulling process, after the seed growth is completed, the temperature of the thermal field in the single crystal furnace needs to be lowered so that the crystal diameter gradually increases to the target size, which is the shoulder releasing operation. . The larger the diameter of the target ingot required, the longer the shoulder setting operation will be.
步骤102，在所述晶棒的放肩长度处于目标范围的第一区间时，设定单晶炉内热场的降温速率为第一速率范围，同时设置晶棒的提拉速度为第一速度范围。Step 102: When the shoulder length of the crystal ingot is in the first interval of the target range, set the cooling rate of the thermal field in the single crystal furnace to the first rate range, and at the same time set the pulling speed of the crystal ingot to the first speed range. .
在本申请实施例中，参考图2，放肩长度为放肩过程中，籽晶的末端与放肩时的晶体的下表面之间的垂直距离，图2中“h”即为放肩长度，放肩长度越长，得到的目标晶棒的直径越大。In the embodiment of the present application, with reference to Figure 2, the shoulder length is the vertical distance between the end of the seed crystal and the lower surface of the crystal during the shoulder placement process. "h" in Figure 2 is the shoulder length. , the longer the shoulder length, the larger the diameter of the target crystal rod obtained.
图2中“a”为肩部顶角，由于{111}面的夹角是35.2°，如果肩部顶角大于70度，在放肩过程中会出现{111}小面，则容易发生位错化，导致放肩失败。因此在放肩的过程中，不同放肩长度对应设置不同的降温速率和晶棒的提拉速率，使得放肩时，肩部顶角保持在45°-70°，避免产生小面。"a" in Figure 2 is the top angle of the shoulder. Since the angle between the {111} planes is 35.2°, if the top angle of the shoulder is greater than 70 degrees, {111} facets will appear during the shoulder placement process, and it is easy to cause positioning. Mistaken, leading to failure in shoulder placement. Therefore, during the shoulder placement process, different shoulder lengths are correspondingly set with different cooling rates and crystal rod pulling rates, so that when the shoulders are placed, the shoulder vertex angle is maintained at 45°-70° to avoid the formation of facets.
具体地，第一区间为放肩长度大于或等于1mm且小于或等于60mm，对应的第一速率范围可以为降温速率大于或等于2kw/h且小于或等于12kw/h，具体地，在第一区间内，第一降温速率可以为3kw/h、4kw/h、5kw/h、6kw/h、7kw/h、8kw/h、9kw/h、10kw/h、11kw/h以及12kw/h等，第一速度范围为晶棒的提拉速度大于或等于25mm/h且小于或等于160mm/h，具体可以为25mm/h、45mm/h、65mm/h、85mm/h、105mm/h、125mm/h2、145mm/h以及160mm/h等。Specifically, the first interval is that the shoulder length is greater than or equal to 1mm and less than or equal to 60mm, and the corresponding first rate range can be that the cooling rate is greater than or equal to 2kw/h and less than or equal to 12kw/h. Specifically, in the first Within the interval, the first cooling rate can be 3kw/h, 4kw/h, 5kw/h, 6kw/h, 7kw/h, 8kw/h, 9kw/h, 10kw/h, 11kw/h and 12kw/h, etc. The first speed range is that the pulling speed of the crystal rod is greater than or equal to 25mm/h and less than or equal to 160mm/h. Specifically, it can be 25mm/h, 45mm/h, 65mm/h, 85mm/h, 105mm/h, 125mm/h. h2, 145mm/h and 160mm/h, etc.
步骤103，在所述晶棒的放肩长度处于目标范围的第二区间时，将所述单晶炉内热场的降温速率由所述第一速率范围提升至第二速率范围，同时将晶 棒的提拉速度由第一速度范围提升至第二速度范围。Step 103: When the shoulder length of the crystal rod is in the second interval of the target range, increase the cooling rate of the thermal field in the single crystal furnace from the first rate range to the second rate range, and at the same time, increase the cooling rate of the thermal field in the single crystal furnace. The pulling speed of the rod is increased from the first speed range to the second speed range.
在本申请实施例中，第二区间可以为放肩长度大于60mm且小于或等于150mm，第二速率范围为降温速率大于或等于3kw/h且小于或等于15kw/h，例如，可以为3kw/h、4kw/h、5kw/h、6kw/h、7kw/h、8kw/h、9kw/h、10kw/h、12kw/h以及15kw/h等，第二速度范围为晶棒的提拉速度大于或等于45mm/h且小于或等于190mm/h，晶棒的提拉速度可以为45mm/h、65mm/h、85mm/h、105mm/h、125mm/h、145mm/h、165mm/h、185mm/h以及190mm/h等，当放肩长度进入第二区间范围时，可以将降温速率由第一速率范围调整为第二速率范围，同时将晶棒的提拉速度由第一速度范围调整为第二速度范围，以继续使得肩部顶角处于45°-70°之间，避免产生小面。In the embodiment of the present application, the second interval can be that the shoulder length is greater than 60mm and less than or equal to 150mm, and the second rate range is that the cooling rate is greater than or equal to 3kw/h and less than or equal to 15kw/h. For example, it can be 3kw/ h, 4kw/h, 5kw/h, 6kw/h, 7kw/h, 8kw/h, 9kw/h, 10kw/h, 12kw/h and 15kw/h, etc. The second speed range is the pulling speed of the crystal rod Greater than or equal to 45mm/h and less than or equal to 190mm/h, the pulling speed of the crystal rod can be 45mm/h, 65mm/h, 85mm/h, 105mm/h, 125mm/h, 145mm/h, 165mm/h, 185mm/h and 190mm/h, etc., when the shoulder length enters the second range, the cooling rate can be adjusted from the first speed range to the second speed range, and at the same time, the pulling speed of the crystal rod can be adjusted from the first speed range It is the second speed range to continue to keep the shoulder apex angle between 45° and 70° to avoid the formation of facets.
步骤104，在所述晶棒的放肩长度处于目标范围的第三区间时，将所述单晶炉内热场的降温速率由所述第二速率范围提升至第三速率范围，同时将晶棒的提拉速度由第二速度范围提升至第三速度范围；其中，所述第一区间的放肩长度的值小于所述第二区间的放肩长度的值，所述第二区间的放肩长度的值小于所述第三区间的放肩长度的值。Step 104: When the shoulder length of the crystal ingot is in the third interval of the target range, increase the cooling rate of the thermal field in the single crystal furnace from the second rate range to the third rate range, and simultaneously move the crystal ingot The lifting speed is increased from the second speed range to the third speed range; wherein, the value of the shoulder length of the first interval is less than the value of the shoulder length of the second interval, and the value of the shoulder length of the second interval is The value of the length is smaller than the value of the shoulder length of the third interval.
在本申请实施例中，第三区间可以为放肩长度大于150mm，第三速率范围为降温速率大于或等于1kw/h且小于或等于10kw/h，例如，可以为1kw/h、2kw/h、3kw/h、4kw/h、5kw/h、6kw/h、7kw/h、8kw/h、9kw/h以及10kw/h等，第三速度范围为晶棒的提拉速度大于或等于60mm/h且小于或等于200mm/h，例如可以为：60mm/h、80mm/h、100mm/h、120mm/h、140mm/h、160mm/h、180mm/h以及200mm/h。以保证当放肩长度达到第三区间时，放肩过程中肩部顶角继续保持在45°-70°之间，避免产生小面、位错等影响晶棒生长的缺陷。In the embodiment of the present application, the third interval can be that the shoulder length is greater than 150mm, and the third rate range is that the cooling rate is greater than or equal to 1kw/h and less than or equal to 10kw/h, for example, it can be 1kw/h or 2kw/h. , 3kw/h, 4kw/h, 5kw/h, 6kw/h, 7kw/h, 8kw/h, 9kw/h and 10kw/h, etc. The third speed range is that the pulling speed of the crystal rod is greater than or equal to 60mm/ h and less than or equal to 200mm/h, for example, it can be: 60mm/h, 80mm/h, 100mm/h, 120mm/h, 140mm/h, 160mm/h, 180mm/h and 200mm/h. This is to ensure that when the shoulder length reaches the third interval, the shoulder apex angle continues to remain between 45° and 70° during the shouldering process to avoid defects such as facets and dislocations that affect the growth of the crystal ingot.
步骤105，在所述晶棒的晶棒直径为所述目标晶棒直径时，结束放肩操作。Step 105: When the crystal ingot diameter of the crystal ingot is the target crystal ingot diameter, end the shoulder releasing operation.
在本申请实施例中，当放肩操作进行到得到的晶体的直径已经达到接近目标晶棒直径时，放肩操作即可结束，进入下一步转肩、等径生长的步骤，完成单晶拉制过程后，得到目标直径的晶棒。In the embodiment of the present application, when the shouldering operation is carried out until the diameter of the obtained crystal has reached close to the target crystal rod diameter, the shouldering operation can be ended, and the next step of shouldering and equal-diameter growth is entered to complete the single crystal pulling. After the manufacturing process, the crystal rod with the target diameter is obtained.
本申请通过在放肩过程中，根据放肩长度，逐步提升单晶炉内热场的降温速率和晶棒的提拉速度，使得放肩过程中肩部顶角始终保持在45°-70°，且本申请通过对降温量、拉速等进行控制，使得肩部竖直截面的边缘线条近似线性变化。当肩部顶角在45°-70°，可以避免或减少放肩产生小面导致产生位 错，提升了放肩成功率。现有技术中，通常采用平放肩的方法进行放肩操作，平放肩操作肩部顶角在120°左右，在这个角度下进行放肩操作时，可能会产生位错和位错增殖，甚至变为多晶，导致放肩失败。本申请相比现有技术的方案，提高了放肩操作的成功率。This application gradually increases the cooling rate of the thermal field in the single crystal furnace and the pulling speed of the crystal rod according to the length of the shoulder during the shoulder placing process, so that the shoulder apex angle is always maintained at 45°-70° during the shoulder placing process. In addition, this application controls the cooling amount, pulling speed, etc., so that the edge lines of the vertical cross-section of the shoulder change approximately linearly. When the shoulder top angle is between 45° and 70°, it can avoid or reduce the position of the facets caused by placing the shoulders. Wrong, the success rate of shoulder placement has been improved. In the prior art, the shoulder-resting operation is usually carried out by placing the shoulders flat. The top angle of the shoulder is about 120°. When performing the shoulder-resting operation at this angle, dislocation and dislocation multiplication may occur. It may even become polycrystalline, causing the shoulder placement to fail. Compared with the prior art solution, this application improves the success rate of the shoulder-resting operation.
综上，本申请提供一种单晶硅放肩方法，根据目标晶棒直径获取放肩长度，当放肩长度处于1-60mm时，设置单晶炉内热场的降温速率为2-12kw/h，晶棒的提拉速度为25-160mm/h。当放肩长度处于60-150mm，设置单晶炉内热场的降温速率为3-15kw/h，晶棒的提拉速度为45-190mm/h，当放肩长度大于150mm时，设置单晶炉内热场的降温速率为1-10kw/h，晶棒的提拉速度为60-200mm/h，通过上述工艺参数进行放肩过程，使得放肩时，肩部顶角可以保持在45°-70°，减小了放肩过程中小面出现的概率，进一步降低发生位错的概率，提高了放肩成功率。In summary, this application provides a single crystal silicon shouldering method. The shouldering length is obtained according to the target crystal rod diameter. When the shouldering length is 1-60mm, the cooling rate of the thermal field in the single crystal furnace is set to 2-12kw/h. , the pulling speed of the crystal rod is 25-160mm/h. When the shoulder length is 60-150mm, set the cooling rate of the thermal field in the single crystal furnace to 3-15kw/h, and the pulling speed of the crystal rod to 45-190mm/h. When the shoulder length is greater than 150mm, set the single crystal furnace The cooling rate of the internal thermal field is 1-10kw/h, and the pulling speed of the crystal ingot is 60-200mm/h. The shoulder placing process is carried out through the above process parameters, so that when the shoulder is placed, the shoulder top angle can be maintained at 45°-70 °, which reduces the probability of facets appearing during shoulder placement, further reduces the probability of dislocation, and improves the success rate of shoulder placement.
图3是本申请实施例提供的又一种单晶硅放肩方法的步骤流程图，包括：Figure 3 is a step flow chart of yet another single crystal silicon shoulder placement method provided by an embodiment of the present application, including:
步骤201、根据目标晶棒直径，对晶棒进行放肩操作。Step 201: According to the target diameter of the crystal ingot, perform a shoulder setting operation on the crystal ingot.
此步骤具体可参考步骤101，此处不再赘述。For details of this step, please refer to step 101 and will not be described again here.
步骤202、在所述晶棒的放肩长度处于目标范围的第一区间时，设定单晶炉内热场的降温速率为第一速率范围，同时设置晶棒的提拉速度为第一速度范围，并设置液口距为30-45mm。Step 202: When the shoulder length of the crystal ingot is in the first interval of the target range, set the cooling rate of the thermal field in the single crystal furnace to the first rate range, and at the same time set the pulling speed of the crystal ingot to the first speed range. , and set the liquid port distance to 30-45mm.
在本申请实施例中，晶棒的放肩长度处于目标范围的第一区间时，第一速率范围与第一速度范围参考步骤102设置，此时同步调整液口距的距离，在第一区间时，液口距的范围为30-45mm，例如，可以为30mm、33mm、35mm、37mm、39mm、41mm、43mm以及45mm等，通过调整液口距的范围，可以辅助使得降温的速率可以达到第一速率范围，保证第一速率范围下的降温量大的大小，提升放肩成功率。In the embodiment of the present application, when the shoulder length of the crystal ingot is in the first interval of the target range, the first speed range and the first speed range are set with reference to step 102. At this time, the distance between the liquid openings is adjusted synchronously. When the liquid mouth distance is in the range of 30-45mm, for example, it can be 30mm, 33mm, 35mm, 37mm, 39mm, 41mm, 43mm and 45mm, etc. By adjusting the range of the liquid mouth distance, it can help to achieve the cooling rate. One speed range ensures the largest cooling amount in the first speed range and improves the success rate of shoulder release.
步骤203、在所述晶棒的放肩长度处于目标范围的第二区间时，将所述单晶炉内热场的降温速率由所述第一速率范围提升至第二速率范围，同时将晶棒的提拉速度由第一速度范围提升至第二速度范围，并设置液口距为20-35mm。Step 203: When the shoulder length of the crystal ingot is in the second interval of the target range, increase the cooling rate of the thermal field in the single crystal furnace from the first rate range to the second rate range, and simultaneously move the crystal ingot The lifting speed is increased from the first speed range to the second speed range, and the liquid port distance is set to 20-35mm.
在本申请实施例中，晶棒的放肩长度处于目标范围的第二区间时，第二速率范围与第二速度范围参考步骤103设置，此时同步调整液口距的距离， 在第二区间时，液口距的范围为20-35mm，例如，可以为20mm、22mm、24mm、26mm、28mm、31mm、33mm以及35mm等，通过调整液口距的范围，可以辅助使得降温的速率可以达到第二速率范围，保证第二速率范围下的降温量大的大小，提升放肩成功率。In the embodiment of the present application, when the shoulder length of the crystal ingot is in the second interval of the target range, the second speed range and the second speed range are set with reference to step 103. At this time, the distance between the liquid openings is adjusted synchronously, In the second interval, the range of the liquid mouth distance is 20-35mm. For example, it can be 20mm, 22mm, 24mm, 26mm, 28mm, 31mm, 33mm, 35mm, etc. By adjusting the range of the liquid mouth distance, it can assist in cooling. The speed can reach the second speed range, ensuring a large cooling amount in the second speed range and improving the success rate of shoulder release.
步骤204、在所述晶棒的放肩长度处于目标范围的第三区间时，将所述单晶炉内热场的降温速率由所述第二速率范围提升至第三速率范围，同时将晶棒的提拉速度由第二速度范围提升至第三速度范围，并设置液口距为15-20mm；其中，所述第一区间的放肩长度的值小于所述第二区间的放肩长度的值，所述第二区间的放肩长度的值小于所述第三区间的放肩长度的值。Step 204: When the shoulder length of the crystal ingot is in the third interval of the target range, increase the cooling rate of the thermal field in the single crystal furnace from the second rate range to the third rate range, and simultaneously move the crystal ingot The lifting speed is increased from the second speed range to the third speed range, and the liquid mouth distance is set to 15-20mm; wherein the value of the shoulder length of the first interval is less than the shoulder length of the second interval value, the value of the shoulder length of the second interval is smaller than the value of the shoulder length of the third interval.
在本申请实施例中，晶棒的放肩长度处于目标范围的第三区间时，第三速率范围与第三速度范围的设置参考步骤104设置，此时同步调整液口距的距离，在第二区间时，液口距的范围为15-20mm，例如，可以为15mm、16mm、17mm、18mm、19mm以及20mm等，通过调整液口距的范围，可以辅助使得降温的速率可以达到第三速率范围，保证第二速率范围下的降温量的大小，提升放肩成功率。In the embodiment of the present application, when the shoulder length of the crystal ingot is in the third interval of the target range, the third speed range and the third speed range are set with reference to step 104. At this time, the distance between the liquid ports is adjusted synchronously. In the second interval, the range of the liquid port distance is 15-20mm, for example, it can be 15mm, 16mm, 17mm, 18mm, 19mm and 20mm, etc. By adjusting the range of the liquid port distance, it can assist in making the cooling rate reach the third rate. range to ensure the cooling amount in the second speed range and improve the success rate of shoulder release.
步骤205，在所述晶棒的晶棒直径为所述目标晶棒直径时，结束放肩操作。Step 205: When the crystal rod diameter of the crystal rod is the target crystal rod diameter, end the shoulder releasing operation.
此步骤具体可参考步骤105，此处不再赘述。For details of this step, please refer to step 105 and will not be described again here.
可选地，所述方法还包括：Optionally, the method also includes:
步骤206，在放肩操作的过程中，控制肩部顶角的角度为45°-70°。Step 206: During the shoulder placing operation, control the top angle of the shoulder to 45°-70°.
在本申请实施例中，在放肩过程中，通过调整单晶炉内的降温速率，晶棒提拉的速度以及液口距的距离，控制肩部顶角可以保持在45°-70°，以减少和避免放肩过程中出现{111}小面，提高放肩成功率。In the embodiment of this application, during the shoulder placing process, by adjusting the cooling rate in the single crystal furnace, the speed of pulling the crystal ingot and the distance between the liquid ports, the shoulder apex angle can be controlled to be maintained at 45°-70°. This is to reduce and avoid the appearance of {111} facets during shoulder placement and improve the success rate of shoulder placement.
可选地，在所述晶棒的放肩长度处于目标范围的第一区间时，所述单晶炉内热场的降温量为0-6.5kw；在所述晶棒的放肩长度处于目标范围的第二区间时，所述单晶炉内热场的降温量为6.5-14kw；在所述晶棒的放肩长度处于目标范围的第三区间时，所述单晶炉内热场的降温量为14-15kw。Optionally, when the shoulder length of the crystal rod is in the first interval of the target range, the cooling amount of the thermal field in the single crystal furnace is 0-6.5kw; when the shoulder length of the crystal rod is in the target range When the second interval of the single crystal furnace, the cooling amount of the thermal field in the single crystal furnace is 6.5-14kw; when the shoulder length of the crystal rod is in the third interval of the target range, the cooling amount of the thermal field in the single crystal furnace is 14-15kw.
具体地，晶棒的放肩长度处于目标范围的第一区间时，在第一速率范围下，可以达到的降温量为0-6.5kw，降温速率越快，放肩长度的成长越快，例如，当降温速率为4kw/h时，放肩长度成长为60mm，需要1小时；当降温速率为8kw/h时，放肩长度成长为60mm，仅需要约0.8小时。晶棒的放肩长度 处于目标范围的第二区间时，在第二速率范围下，可以达到的降温量为6.5-14kw，晶棒的放肩长度处于目标范围的第三区间时，在第三速率范围下，可以达到的降温量为14-15kw。由于晶棒的提拉速度增快，降温速率增高，所以相比现有技术，本申请放肩结束后，放肩过程中的降温量相比现有技术更大，使得等径头部温度相比原有工艺低，用此新工艺生长的单晶头部氧含量降低，提升了晶体品质。Specifically, when the shoulder length of the crystal rod is in the first interval of the target range, the achievable cooling amount is 0-6.5kw under the first rate range. The faster the cooling rate, the faster the growth of the shoulder length, for example , when the cooling rate is 4kw/h, the shoulder length grows to 60mm, which takes 1 hour; when the cooling rate is 8kw/h, the shoulder length grows to 60mm, which only takes about 0.8 hours. The shoulder length of the crystal rod When it is in the second interval of the target range, under the second rate range, the cooling amount that can be achieved is 6.5-14kw. When the shoulder length of the crystal ingot is in the third interval of the target range, under the third rate range, it can be achieved The cooling capacity is 14-15kw. Since the pulling speed of the crystal rod is increased and the cooling rate is increased, compared with the prior art, the amount of cooling during the shoulder placement process in this application is greater than that of the prior art, so that the temperature of the equal diameter head is relatively different. Lower than the original process, the oxygen content in the head of the single crystal grown with this new process is reduced, improving the crystal quality.
可选地，所述方法还包括：Optionally, the method also includes:
步骤207，在所述放肩长度为1-30mm时，设置液口距为35-45mm，同时设置晶棒的提拉速度为25-150mm/h。Step 207: When the shoulder length is 1-30mm, set the liquid mouth distance to 35-45mm, and set the pulling speed of the crystal rod to 25-150mm/h.
在本申请实施例中，当放肩长度为1-30mm时，如放肩长度为1mm、5mm、10mm、15mm、20mm、25mm以及30mm等长度，单晶炉内的降温速率可以参考步骤102设置，另外可以设置液口距为35-45mm，例如可以设置为35mm、37mm、39mm、41mm、42mm、43mm、44mm以及45mm等，同时可以设置晶棒的提拉速度为25-150mm/h，例如可以为25mm/h、35mm/h、45mm/h、55mm/h、65mm/h、75mm/h、85mm/h、95mm/h、105mm/h、115mm/h、125mm/h、135mm/h、145mm/h以及150mm/h等，在上述范围内的降温速率、提拉速度以及液口距可以进一步保证肩部顶角处于45°-70°。In the embodiment of this application, when the shoulder length is 1-30mm, for example, the shoulder length is 1mm, 5mm, 10mm, 15mm, 20mm, 25mm and 30mm, the cooling rate in the single crystal furnace can be set with reference to step 102. , in addition, the liquid mouth distance can be set to 35-45mm, for example, it can be set to 35mm, 37mm, 39mm, 41mm, 42mm, 43mm, 44mm and 45mm, etc., and the pulling speed of the crystal rod can be set to 25-150mm/h, for example Can be 25mm/h, 35mm/h, 45mm/h, 55mm/h, 65mm/h, 75mm/h, 85mm/h, 95mm/h, 105mm/h, 115mm/h, 125mm/h, 135mm/h, 145mm/h and 150mm/h, etc. The cooling rate, lifting speed and liquid mouth distance within the above range can further ensure that the shoulder top angle is between 45°-70°.
步骤208，在所述放肩长度为30-60mm时，设置液口距为30-40mm，同时设置晶棒的提拉速度为35-160mm/h。Step 208: When the shoulder length is 30-60mm, set the liquid mouth distance to 30-40mm, and set the pulling speed of the crystal rod to 35-160mm/h.
在本申请实施例中，当放肩长度为30-60mm时，单晶炉内的降温速率可以参考步骤102设置，另外同时可以设置液口距为30-40mm，例如可以设置为30mm、32mm、34mm、35mm、36mm、37mm、38mm、39mm以及40mm等，同时可以设置晶棒的提拉速度为35-160mm/h，例如可以为35mm/h、45mm/h、55mm/h、65mm/h、75mm/h、85mm/h、95mm/h、105mm/h、115mm/h、125mm/h、135mm/h、150mm/h以及160mm/h等，在上述范围内的降温速率、提拉速度以及液口距可以进一步保证肩部顶角处于45°-70°。In the embodiment of this application, when the shoulder length is 30-60mm, the cooling rate in the single crystal furnace can be set with reference to step 102. In addition, the liquid port distance can be set to 30-40mm, for example, it can be set to 30mm, 32mm, 34mm, 35mm, 36mm, 37mm, 38mm, 39mm and 40mm, etc. At the same time, the pulling speed of the crystal rod can be set to 35-160mm/h, for example, it can be 35mm/h, 45mm/h, 55mm/h, 65mm/h, 75mm/h, 85mm/h, 95mm/h, 105mm/h, 115mm/h, 125mm/h, 135mm/h, 150mm/h and 160mm/h, etc., within the above range, the cooling rate, pulling speed and liquid The mouth distance can further ensure that the shoulder top angle is between 45° and 70°.
步骤209，在所述放肩长度为60-90mm时，设置液口距为28-35mm，同时设置晶棒的提拉速度为45-170mm/h。Step 209: When the shoulder length is 60-90mm, set the liquid mouth distance to 28-35mm, and set the pulling speed of the crystal rod to 45-170mm/h.
在本申请实施例中，当放肩长度为60-90mm时，例如为：60mm、65mm、70mm、75mm、80mm以及85mm等时单晶炉内的降温速率可以参考步骤102 设置，另外设置液口距为28-35mm，例如可以设置为28mm、29mm、30mm、31mm、32mm、33mm、34mm以及35mm等，同时可以设置晶棒的提拉速度为45-170mm/h，例如可以为45mm/h、55mm/h、65mm/h、75mm/h、85mm/h、95mm/h、105mm/h、115mm/h、125mm/h、135mm/h、145mm/h、160mm/h以及170mm/h等，在上述范围内的降温速率、提拉速度以及液口距可以进一步保证肩部顶角处于45°-70°。In the embodiment of this application, when the shoulder length is 60-90mm, for example: 60mm, 65mm, 70mm, 75mm, 80mm and 85mm, the cooling rate in the single crystal furnace can be referred to step 102. setting, and also set the liquid mouth distance to 28-35mm, for example, it can be set to 28mm, 29mm, 30mm, 31mm, 32mm, 33mm, 34mm and 35mm, etc., and the pulling speed of the crystal rod can be set to 45-170mm/h, for example Can be 45mm/h, 55mm/h, 65mm/h, 75mm/h, 85mm/h, 95mm/h, 105mm/h, 115mm/h, 125mm/h, 135mm/h, 145mm/h, 160mm/h and 170mm/h, etc. The cooling rate, lifting speed and liquid mouth distance within the above range can further ensure that the shoulder top angle is between 45°-70°.
步骤210，在所述放肩长度为90-120mm时，设置液口距为25-30mm，同时设置晶棒的提拉速度为55-190mm/h。Step 210: When the shoulder length is 90-120 mm, set the liquid mouth distance to 25-30 mm, and set the pulling speed of the crystal rod to 55-190 mm/h.
在本申请实施例中，当放肩长度为90-120mm时，例如为：90mm、94mm、98mm、102mm、106mm、110mm、114mm、116mm以及120mm等时，单晶炉内的降温速率可以参考步骤103设置，另外可以同时设置液口距为25-30mm，例如可以设置为25mm、26mm、27mm、28mm、28.5mm、29mm、29.5mm以及30mm等，同时可以设置晶棒的提拉速度为55-190mm/h，例如可以为55mm/h、65mm/h、75mm/h、85mm/h、95mm/h、105mm/h、115mm/h、125mm/h、135mm/h、145mm/h、155mm/h、170mm/h以及190mm/h等，在上述范围内的单晶炉内的降温速率、提拉速度以及液口距可以进一步保证肩部顶角处于45°-70°。In the embodiment of the present application, when the shoulder length is 90-120mm, for example: 90mm, 94mm, 98mm, 102mm, 106mm, 110mm, 114mm, 116mm and 120mm, etc., the cooling rate in the single crystal furnace can refer to the steps 103 setting, in addition, the liquid mouth distance can be set to 25-30mm at the same time, for example, it can be set to 25mm, 26mm, 27mm, 28mm, 28.5mm, 29mm, 29.5mm and 30mm, etc., and the pulling speed of the crystal rod can be set to 55-30mm. 190mm/h, for example, it can be 55mm/h, 65mm/h, 75mm/h, 85mm/h, 95mm/h, 105mm/h, 115mm/h, 125mm/h, 135mm/h, 145mm/h, 155mm/h , 170mm/h and 190mm/h, etc. The cooling rate, pulling speed and liquid port distance in the single crystal furnace within the above range can further ensure that the shoulder apex angle is 45°-70°.
步骤211，在所述放肩长度为120-150mm时，设置液口距为20-28mm，同时设置晶棒的提拉速度为60-190mm/h。Step 211: When the shoulder length is 120-150 mm, set the liquid mouth distance to 20-28 mm, and set the pulling speed of the crystal rod to 60-190 mm/h.
在本申请实施例中，当放肩长度为120-150mm时，例如为120mm、125mm、130mm、135mm、140mm、145mm以及150mm等时，单晶炉内的降温速率可以参考步骤103设置，另外可以同时设置液口距为20-28mm，例如可以设置为20mm、21mm、22mm、23mm、24mm、25mm、26mm、27mm、以及28mm等，同时可以设置晶棒的提拉速度为60-190mm/h，例如可以为60mm/h、70mm/h、80mm/h、90mm/h、100mm/h、110mm/h、120mm/h、130mm/h、140mm/h、150mm/h、160mm/h、170mm/h、180mm/h以及190mm/h等，在上述范围内的降温速率、提拉速度以及液口距可以进一步保证肩部顶角处于45°-70°。In the embodiment of the present application, when the shoulder length is 120-150mm, such as 120mm, 125mm, 130mm, 135mm, 140mm, 145mm and 150mm, etc., the cooling rate in the single crystal furnace can be set with reference to step 103. In addition, it can be set At the same time, set the liquid mouth distance to 20-28mm, for example, it can be set to 20mm, 21mm, 22mm, 23mm, 24mm, 25mm, 26mm, 27mm, and 28mm, etc., and the pulling speed of the crystal rod can be set to 60-190mm/h. For example, it can be 60mm/h, 70mm/h, 80mm/h, 90mm/h, 100mm/h, 110mm/h, 120mm/h, 130mm/h, 140mm/h, 150mm/h, 160mm/h, 170mm/h , 180mm/h and 190mm/h, etc. The cooling rate, lifting speed and liquid mouth distance within the above range can further ensure that the shoulder top angle is 45°-70°.
步骤212，在所述放肩长度为150-180mm时，设置液口距为15-25mm，同时设置晶棒的提拉速度为60-200mm/h。Step 212: When the shoulder length is 150-180 mm, set the liquid mouth distance to 15-25 mm, and set the pulling speed of the crystal rod to 60-200 mm/h.
在本申请实施例中，当放肩长度为150-180mm时，例如为150mm、155mm、 160mm、165mm、170mm、175mm、以及180mm等，单晶炉内的降温速率可以参考步骤103设置，另外设置液口距为15-25mm，例如可以设置为15mm、17mm、19mm、20mm、21mm、22mm、23mm、24mm以及25mm等，同时可以设置晶棒的提拉速度为60-200mm/h，例如可以60mm/h、70mm/h、80mm/h、90mm/h、100mm/h、110mm/h、120mm/h、130mm/h、140mm/h、150mm/h、160mm/h、170mm/h、180mm/h、190mm/h以及200mm/h等，在上述范围内的降温速率、提拉速度以及液口距可以进一步保证肩部顶角处于45°-70°。In the embodiment of the present application, when the shoulder length is 150-180mm, for example, it is 150mm, 155mm, 160mm, 165mm, 170mm, 175mm, and 180mm, etc. The cooling rate in the single crystal furnace can be set by referring to step 103. In addition, set the liquid port distance to 15-25mm. For example, it can be set to 15mm, 17mm, 19mm, 20mm, 21mm, 22mm. , 23mm, 24mm and 25mm, etc. At the same time, the pulling speed of the crystal rod can be set to 60-200mm/h, for example, 60mm/h, 70mm/h, 80mm/h, 90mm/h, 100mm/h, 110mm/h, 120mm/h, 130mm/h, 140mm/h, 150mm/h, 160mm/h, 170mm/h, 180mm/h, 190mm/h and 200mm/h, etc., within the above range, the cooling rate, pulling speed and liquid The mouth distance can further ensure that the shoulder top angle is between 45° and 70°.
步骤213，在所述放肩长度为180mm时，设置液口距为15-20mm，同时设置晶棒的提拉速度为60-200mm/h。Step 213: When the shoulder length is 180 mm, set the liquid mouth distance to 15-20 mm, and set the pulling speed of the crystal rod to 60-200 mm/h.
在本申请实施例中，当放肩长度为180mm时，单晶炉内的降温速率可以参考步骤104设置，另外设置液口距为15-20mm，例如可以设置为15mm、16mm、17mm、18mm、19mm以及20mm等，同时可以设置晶棒的提拉速度为60-200mm/h，例如可以为60mm/h、70mm/h、80mm/h、90mm/h、100mm/h、110mm/h、120mm/h、130mm/h、140mm/h、150mm/h、160mm/h、170mm/h、180mm/h、190mm以及200mm/h等，在上述范围内的降温速率、提拉速度以及液口距可以进一步保证肩部顶角处于45°-70°。In the embodiment of this application, when the shoulder length is 180mm, the cooling rate in the single crystal furnace can be set with reference to step 104. In addition, the liquid port distance is set to 15-20mm, for example, it can be set to 15mm, 16mm, 17mm, 18mm, 19mm and 20mm, etc. At the same time, the pulling speed of the crystal rod can be set to 60-200mm/h, for example, it can be 60mm/h, 70mm/h, 80mm/h, 90mm/h, 100mm/h, 110mm/h, 120mm/ h, 130mm/h, 140mm/h, 150mm/h, 160mm/h, 170mm/h, 180mm/h, 190mm and 200mm/h, etc. The cooling rate, pulling speed and liquid mouth distance within the above range can be further Make sure the top angle of the shoulders is between 45° and 70°.
可选地，所述方法还包括：Optionally, the method also includes:
步骤214，在放肩过程中，设定晶转为8-12r/min，埚转5-9r/min，且所述埚转的方向与所述晶转的方向相反。Step 214, during the shoulder releasing process, set the crystal rotation to 8-12 r/min, the crucible rotation to 5-9 r/min, and the crucible rotation direction is opposite to the crystal rotation direction.
在本申请实施例中，晶转为晶体转动的速度，埚转为单晶炉内坩埚的转动速度。晶转和埚转目的为抑制熔液的热对流，为单晶生长提供稳定热***，晶转和坩埚的转动有利于杂质的均匀分布，晶转和坩埚方向相反设置，保证可以拉制出单晶。In the embodiment of the present application, the crystal rotation refers to the rotation speed of the crystal, and the crucible rotation refers to the rotation speed of the crucible in the single crystal furnace. The purpose of the crystal rotation and crucible rotation is to suppress the thermal convection of the melt and provide a stable thermal system for single crystal growth. The rotation of the crystal rotation and crucible is conducive to the uniform distribution of impurities. The crystal rotation and crucible are set in opposite directions to ensure that single crystals can be drawn. crystal.
表1为本申请实施例提供的改进的放肩工艺参数表。其中，参考图2，放肩长度为放肩过程中，籽晶的末端与放肩时的晶体的下表面之间的垂直距离，图2中“h”即为放肩长度，放肩长度越长，得到的目标晶棒的直径越大。降温量为在放肩过程中，当前单晶炉功率与开始放肩时功率之间的差值，液口距为单晶炉内的导热筒与单晶炉内的熔液的液面之间的垂直距离，拉速为提拉晶棒时的速度，晶转为晶体转动的速度，埚转为单晶炉内坩埚的转动速度。 Table 1 is an improved shoulder placing process parameter table provided by the embodiment of the present application. Among them, referring to Figure 2, the shoulder length is the vertical distance between the end of the seed crystal and the lower surface of the crystal when the shoulder is placed during the shoulder placement process. "h" in Figure 2 is the shoulder length. The longer the shoulder length The longer, the larger the diameter of the target crystal rod obtained. The cooling amount is the difference between the current power of the single crystal furnace and the power at the beginning of shouldering during the shouldering process. The liquid mouth distance is between the heat conduction cylinder in the single crystal furnace and the liquid level of the melt in the single crystal furnace. The vertical distance of , the pulling speed is the speed when pulling the crystal rod, the crystal rotation is the rotation speed of the crystal, and the crucible rotation is the rotation speed of the crucible in the single crystal furnace.
进一步地，坩埚可以为石墨坩埚或石英坩埚，用于盛放多晶硅原料，可以通过坩埚升降***，把熔液的液面控制在一个位置，通过调整坩埚的位置调整液口距。导流筒用来隔断热场内部和外部，从而起到加快单晶拉速的作用，同时也起到导流(内部氩气)的作用。
Further, the crucible can be a graphite crucible or a quartz crucible, used to hold polysilicon raw materials. The liquid level of the melt can be controlled at a position through the crucible lifting system, and the liquid mouth distance can be adjusted by adjusting the position of the crucible. The guide tube is used to separate the inside and outside of the thermal field, thereby speeding up the single crystal pulling speed, and also plays a role in guiding the flow (internal argon gas).
表1Table 1
表2为现有技术中的放肩参数表，表中参数的定义与表1相同。
Table 2 is a shoulder-resting parameter table in the prior art. The definitions of the parameters in the table are the same as those in Table 1.
表2Table 2
对比表1与表2的数据可以看出，在达到相同的放肩长度如120mm时，原有工艺的降温量为9kw，本申请在放肩长度达到120mm时，降温量为10.0-13.0kw，相比原有工艺，本申请的降温量更多，也就使得等径头部温度相比原有工艺更低，使得本申请最终得到的单晶头部氧含量相比原有工艺更低，提升了晶体的品质，参考表3，表3为使用本申请方法制备单晶时得到的晶体头部氧含量，相比原有工艺，氧含量降低约1-2ppma。
Comparing the data in Table 1 and Table 2, it can be seen that when the shoulder length reaches the same length of 120mm, the cooling amount of the original process is 9kw. In this application, when the shoulder length reaches 120mm, the cooling amount is 10.0-13.0kw. Compared with the original process, the amount of cooling in this application is greater, which makes the temperature of the equal-diameter head lower than that of the original process, so that the oxygen content of the single crystal head finally obtained by this application is lower than that of the original process. The quality of the crystal is improved. Please refer to Table 3. Table 3 shows the oxygen content in the head of the crystal obtained when using the method of this application to prepare a single crystal. Compared with the original process, the oxygen content is reduced by about 1-2 ppma.
表3 table 3
表4为本申请改进后的工艺与原有工艺放肩成功率的比较。原有工艺中对照肩部顶角为90°-120°，本申请改进的工艺肩部顶角为45°-70°°，可以看出，相比原有工艺，本申请的放肩方法的放肩成功率得到了提升。
Table 4 shows the comparison of the success rate of shoulder placement between the improved process of this application and the original process. In the original process, the comparison shoulder apex angle is 90°-120°, while in the improved process of the present application, the shoulder apex angle is 45°-70°. It can be seen that compared with the original process, the shoulder placing method of the present application is better The success rate of shoulder placement has been improved.
表4Table 4
综上，本申请提供一种单晶硅放肩方法，根据目标晶棒直径获取放肩长度，当放肩长度处于1-60mm时，设置单晶炉内热场的降温速率为2-12kw/h，晶棒的提拉速度为25-160mm/h。当放肩长度处于60-150mm，设置单晶炉内热场的降温速率为3-15kw/h，晶棒的提拉速度为45-190mm/h，当放肩长度大于150mm时，设置单晶炉内热场的降温速率为1-10kw/h，晶棒的提拉速度为60-200mm/h，通过上述工艺参数进行放肩，使得放肩时，肩部顶角可以保持在45°-70°，减小了放肩过程中小面出现的概率，进一步降低发生位错的概率，提高了放肩成功率。In summary, this application provides a single crystal silicon shouldering method. The shouldering length is obtained according to the target crystal rod diameter. When the shouldering length is 1-60mm, the cooling rate of the thermal field in the single crystal furnace is set to 2-12kw/h. , the pulling speed of the crystal rod is 25-160mm/h. When the shoulder length is 60-150mm, set the cooling rate of the thermal field in the single crystal furnace to 3-15kw/h, and the pulling speed of the crystal rod to 45-190mm/h. When the shoulder length is greater than 150mm, set the single crystal furnace The cooling rate of the internal thermal field is 1-10kw/h, and the pulling speed of the crystal ingot is 60-200mm/h. The shoulder is placed through the above process parameters, so that the shoulder top angle can be maintained at 45°-70° when the shoulder is placed. , reducing the probability of facets appearing during shoulder placement, further reducing the probability of dislocation, and improving the success rate of shoulder placement.
本申请实施例提供了一种单晶硅棒，采用上述的单晶硅放肩方法，所述单晶硅棒的肩部顶角的角度为45°-70°。The embodiment of the present application provides a single crystal silicon rod, which adopts the above-mentioned shoulder placing method of single crystal silicon. The angle of the shoulder vertex of the single crystal silicon rod is 45°-70°.
可选地，所述单晶硅棒肩部为等腰三角形。Optionally, the shoulder of the single crystal silicon rod is an isosceles triangle.
在本申请实施例中，采用本申请的单晶硅放肩方法生成的单晶硅棒的放肩角度在45°-70°。In the embodiment of the present application, the shoulder angle of the single crystal silicon rod produced by the single crystal silicon shoulder placing method of the present application is between 45° and 70°.
在垂直于晶棒轴向方向的肩部的任一截面上，选取距离最远的两个点，与肩部顶部的端点进行连线，两条线之间的夹角为45-70度。通常情况下，在垂直于晶棒轴向方向的肩部的截面为圆面，圆面直径方向上的两个端点与顶部端点的连线之间的夹角为45-70度。但在一些特殊情况下，如功率、拉速等工艺参数波动，某一瞬时截面可能不是圆面，截面上距离最远的两个端点与顶部端点连线的夹角可能不在该范围内。因此，本发明是限定，任一选取一个截面，所选取的某一截面上距离最远的两个点，与肩部顶部的端点进行连线，两条线之间的夹角为45°-70°，即在本发明的保护范围内。On any section of the shoulder perpendicular to the axial direction of the crystal rod, select the two farthest points and connect them with the endpoints of the top of the shoulder. The angle between the two lines is 45-70 degrees. Normally, the cross-section of the shoulder perpendicular to the axial direction of the crystal rod is a circular surface, and the angle between the two endpoints in the diameter direction of the circular surface and the top endpoint is 45-70 degrees. However, in some special circumstances, such as fluctuations in process parameters such as power and drawing speed, a certain instantaneous cross-section may not be circular, and the angle between the two farthest endpoints on the cross-section and the top endpoint may not be within this range. Therefore, the present invention is limited to any selected cross-section. The two farthest points on the selected cross-section are connected with the end point of the top of the shoulder. The angle between the two lines is 45°- 70°, which is within the protection scope of the present invention.
作为一种具体实施方案而言，通常情况下，单晶硅棒肩部纵向截面的延长线构成等腰三角形，但在一些其他情况下，如工艺参数的波动等情况下， 肩部所在的斜边并非一条标准直线，可能为一条平缓连接的折线形成肩部，即肩部轴向方向的截面边缘可能呈现一些折线。选取折线上的某一点，并与肩部的顶点进行连线，该连线与晶棒轴向方向的竖直线的夹角在22.5°-35°，即为角度45°-70°的一半，减小了小面出现的概率，进一步降低发生位错的概率。As a specific implementation, usually, the extension line of the longitudinal section of the shoulder of the single crystal silicon rod forms an isosceles triangle, but in some other cases, such as fluctuations in process parameters, etc. The hypotenuse where the shoulder is located is not a standard straight line, but may be a gently connected fold line forming the shoulder, that is, the cross-sectional edge in the axial direction of the shoulder may show some fold lines. Select a point on the fold line and connect it to the vertex of the shoulder. The angle between the connecting line and the vertical line in the axial direction of the crystal rod is 22.5°-35°, which is half of the angle 45°-70°. , reducing the probability of facets appearing and further reducing the probability of dislocations.
需要说明的是，对于方法实施例，为了简单描述，故将其都表述为一系列的动作组合，但是本领域技术人员应该知悉，本申请实施例并不受所描述的动作顺序的限制，因为依据本申请实施例，某些步骤可以采用其他顺序或者同时进行。其次，本领域技术人员也应该知悉，说明书中所描述的实施例均属于优选实施例，所涉及的动作并不一定都是本申请实施例所必须的。It should be noted that for the sake of simple description, the method embodiments are expressed as a series of action combinations. However, those skilled in the art should know that the embodiments of the present application are not limited by the described action sequence, because According to the embodiments of the present application, certain steps may be performed in other orders or simultaneously. Secondly, those skilled in the art should also know that the embodiments described in the specification are all preferred embodiments, and the actions involved are not necessarily necessary for the embodiments of the present application.
需要说明的是，在本文中，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程、方法、物品或者装置不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者装置所固有的要素。在没有更多限制的情况下，由语句“包括一个……”限定的要素，并不排除在包括该要素的过程、方法、物品或者装置中还存在另外的相同要素。It should be noted that, in this document, the terms "comprising", "comprises" or any other variations thereof are intended to cover a non-exclusive inclusion, such that a process, method, article or device that includes a series of elements not only includes those elements, It also includes other elements not expressly listed or inherent in the process, method, article or apparatus. Without further limitation, an element defined by the statement "comprises a..." does not exclude the presence of additional identical elements in a process, method, article or apparatus that includes that element.
上面结合附图对本申请的实施例进行了描述，但是本申请并不局限于上述的具体实施方式，上述的具体实施方式仅仅是示意性的，而不是限制性的，本领域的普通技术人员在本申请的启示下，在不脱离本申请宗旨和权利要求所保护的范围情况下，还可做出很多形式，这些均属于本申请的保护之内。 The embodiments of the present application have been described above in conjunction with the accompanying drawings. However, the present application is not limited to the above-mentioned specific implementations. The above-mentioned specific implementations are only illustrative and not restrictive. Those of ordinary skill in the art will Inspired by this application, many forms can be made without departing from the purpose of this application and the scope protected by the claims, and these all fall within the protection of this application.

Claims (13)

  1. 一种单晶硅放肩方法，其特征在于，所述方法包括：A method for shoulder placement of single crystal silicon, characterized in that the method includes:
    根据目标晶棒直径，对晶棒进行放肩操作；According to the target crystal rod diameter, carry out the shoulder setting operation on the crystal rod;
    在所述晶棒的放肩长度处于目标范围的第一区间时，设定单晶炉内热场的降温速率为第一速率范围，同时设置晶棒的提拉速度为第一速度范围；When the shoulder length of the crystal rod is in the first interval of the target range, the cooling rate of the thermal field in the single crystal furnace is set to the first rate range, and the pulling speed of the crystal rod is set to the first speed range;
    在所述晶棒的放肩长度处于目标范围的第二区间时，将所述单晶炉内热场的降温速率由所述第一速率范围提升至第二速率范围，同时将晶棒的提拉速度由第一速度范围提升至第二速度范围；When the shoulder length of the crystal rod is in the second interval of the target range, the cooling rate of the thermal field in the single crystal furnace is increased from the first rate range to the second rate range, and at the same time, the crystal rod is pulled The speed is increased from the first speed range to the second speed range;
    在所述晶棒的放肩长度处于目标范围的第三区间时，将所述单晶炉内热场的降温速率由所述第二速率范围提升至第三速率范围，同时将晶棒的提拉速度由第二速度范围提升至第三速度范围；其中，所述第一区间的放肩长度的值小于所述第二区间的放肩长度的值，所述第二区间的放肩长度的值小于所述第三区间的放肩长度的值；When the shoulder length of the crystal rod is in the third interval of the target range, the cooling rate of the thermal field in the single crystal furnace is increased from the second rate range to the third rate range, and at the same time, the crystal rod is pulled The speed is increased from the second speed range to the third speed range; wherein the value of the shoulder length of the first interval is less than the value of the shoulder length of the second interval, and the value of the shoulder length of the second interval A value less than the shoulder length of the third interval;
    在所述晶棒的晶棒直径为所述目标晶棒直径时，结束放肩操作。When the crystal rod diameter of the crystal rod is the target crystal rod diameter, the shoulder releasing operation ends.
  2. 根据权利要求1所述的方法，其特征在于，所述方法还包括：The method of claim 1, further comprising:
    在放肩操作的过程中，控制肩部顶角的角度为45°-70°。During the shoulder-resting operation, control the top angle of the shoulder to 45°-70°.
  3. 根据权利要求1所述的方法，其特征在于，所述第一区间为所述放肩长度大于或等于1mm且小于或等于60mm，所述第一速率范围为所述降温速率大于或等于2kw/h且小于或等于12kw/h，所述第一速度范围为所述晶棒的提拉速度大于或等于25mm/h且小于或等于160mm/h；The method according to claim 1, wherein the first interval is that the shoulder length is greater than or equal to 1 mm and less than or equal to 60 mm, and the first rate range is that the cooling rate is greater than or equal to 2kw/ h and less than or equal to 12kw/h, and the first speed range is that the pulling speed of the crystal ingot is greater than or equal to 25mm/h and less than or equal to 160mm/h;
    所述第二区间为所述放肩长度大于60mm且小于或等于150mm，所述第二速率范围为所述降温速率大于或等于3kw/h且小于或等于15kw/h，所述第二速度范围为所述晶棒的提拉速度大于或等于45mm/h且小于或等于190mm/h；The second interval is that the shoulder length is greater than 60mm and less than or equal to 150mm, the second speed range is that the cooling rate is greater than or equal to 3kw/h and less than or equal to 15kw/h, the second speed range The pulling speed of the crystal rod is greater than or equal to 45mm/h and less than or equal to 190mm/h;
    所述第三区间为所述放肩长度大于150mm，所述第三速率范围为所述降温速率大于或等于1kw/h且小于或等于10kw/h，所述第三速度范围为所述晶棒的提拉速度大于或等于60mm/h且小于或等于200mm/h。The third interval is when the shoulder length is greater than 150mm, the third rate range is when the cooling rate is greater than or equal to 1kw/h and less than or equal to 10kw/h, and the third speed range is when the crystal rod The lifting speed is greater than or equal to 60mm/h and less than or equal to 200mm/h.
  4. 根据权利要求3所述的方法，其特征在于，所述方法还包括：The method of claim 3, further comprising:
    在所述晶棒的放肩长度处于目标范围的第一区间时，设置液口距为30-45mm； When the shoulder length of the crystal rod is in the first interval of the target range, set the liquid mouth distance to 30-45mm;
    在所述晶棒的放肩长度处于目标范围的第二区间时，设置液口距为20-35mm；When the shoulder length of the crystal rod is in the second interval of the target range, set the liquid mouth distance to 20-35mm;
    在所述晶棒的放肩长度处于目标范围的第三区间时，设置液口距为15-20mm。When the shoulder length of the crystal rod is in the third interval of the target range, the liquid opening distance is set to 15-20 mm.
  5. 根据权利要求3所述的方法，其特征在于，在所述晶棒的放肩长度处于目标范围的第一区间时，所述单晶炉内热场的降温量为0-6.5kw；The method according to claim 3, characterized in that when the shoulder length of the crystal rod is in the first interval of the target range, the cooling amount of the thermal field in the single crystal furnace is 0-6.5kw;
    在所述晶棒的放肩长度处于目标范围的第二区间时，所述单晶炉内热场的降温量为6.5-14kw；When the shoulder length of the crystal rod is in the second interval of the target range, the cooling amount of the thermal field in the single crystal furnace is 6.5-14kw;
    在所述晶棒的放肩长度处于目标范围的第三区间时，所述单晶炉内热场的降温量为14-15kw。When the shoulder length of the crystal rod is in the third interval of the target range, the cooling amount of the thermal field in the single crystal furnace is 14-15 kw.
  6. 根据权利要求3所述的方法，其特征在于，所述方法还包括：The method of claim 3, further comprising:
    在所述放肩长度为1-30mm时，设置液口距为35-45mm，同时设置晶棒的提拉速度为25-150mm/h；When the shoulder length is 1-30mm, the liquid mouth distance is set to 35-45mm, and the pulling speed of the crystal rod is set to 25-150mm/h;
    在所述放肩长度为30-60mm时，设置液口距为30-40mm，同时设置晶棒的提拉速度为35-160mm/h；When the shoulder length is 30-60mm, the liquid mouth distance is set to 30-40mm, and the pulling speed of the crystal rod is set to 35-160mm/h;
    在所述放肩长度为60-90mm时，设置液口距为28-35mm，同时设置晶棒的提拉速度为45-170mm/h。When the shoulder length is 60-90mm, the liquid mouth distance is set to 28-35mm, and the pulling speed of the crystal rod is set to 45-170mm/h.
  7. 据权利要求3所述的方法，其特征在于，所述方法还包括：The method of claim 3, further comprising:
    在所述放肩长度为90-120mm时，设置液口距为25-30mm，同时设置晶棒的提拉速度为55-180mm/h；When the shoulder length is 90-120mm, the liquid mouth distance is set to 25-30mm, and the pulling speed of the crystal rod is set to 55-180mm/h;
    在所述放肩长度为120-150mm时，设置液口距为20-28mm，同时设置晶棒的提拉速度为60-190mm/h。When the shoulder length is 120-150mm, the liquid mouth distance is set to 20-28mm, and the pulling speed of the crystal rod is set to 60-190mm/h.
  8. 据权利要求3所述的方法，其特征在于，所述方法还包括：The method of claim 3, further comprising:
    在所述放肩长度为150-180mm时，设置液口距为15-25mm，同时设置晶棒的提拉速度为60-200mm/h。When the shoulder length is 150-180mm, the liquid mouth distance is set to 15-25mm, and the pulling speed of the crystal ingot is set to 60-200mm/h.
  9. 根据权利要求3所述的方法，其特征在于，所述方法还包括：The method of claim 3, further comprising:
    在所述放肩长度为180mm时，设置液口距为15-20mm，同时设置晶棒的提拉速度为60-200mm/h。When the shoulder length is 180mm, the liquid mouth distance is set to 15-20mm, and the pulling speed of the crystal rod is set to 60-200mm/h.
  10. 根据权利要求1所述的方法，其特征在于，所述方法还包括：The method of claim 1, further comprising:
    在放肩过程中，设定晶转为8-12r/min，埚转5-9r/min，且所述埚转的方 向与所述晶转的方向相反。During the shoulder releasing process, the crystal rotation is set to 8-12r/min, the crucible rotation is 5-9r/min, and the direction of the crucible rotation is In the opposite direction to the crystal rotation.
  11. 一种单晶硅棒，采用如权利要求1至10任一项所述的方法，其特征在于，所述单晶硅棒的肩部顶角的角度为45°-70°。A single crystal silicon rod using the method according to any one of claims 1 to 10, characterized in that the shoulder vertex angle of the single crystal silicon rod is 45°-70°.
  12. 根据权利要求11所述的单晶硅棒，其特征在于，所述单晶硅棒肩部为等腰三角形。The single crystal silicon rod according to claim 11, characterized in that the shoulder of the single crystal silicon rod is an isosceles triangle.
  13. 根据权利要求11所述的单晶硅棒，其特征在于，在垂直于所述单晶硅棒的轴向方向的肩部的任一截面上，选取距离最远的两个点，与肩部顶部的端点进行连线，两条线之间的夹角为45°-70°。 The single crystal silicon rod according to claim 11, characterized in that on any cross section of the shoulder perpendicular to the axial direction of the single crystal silicon rod, select the two points furthest apart from the shoulder. Connect the top endpoints with a line, and the angle between the two lines is 45°-70°.
PCT/CN2023/099725 2022-09-05 2023-06-12 Monocrystalline silicon shouldering method WO2024051241A1 (en)

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CN112048761A (en) * 2020-08-24 2020-12-08 有研半导体材料有限公司 Large-diameter monocrystalline silicon shouldering growth process
CN113564694A (en) * 2021-07-22 2021-10-29 东莞晶驰光电科技有限公司 Sapphire crystal growth process
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CN103556216A (en) * 2013-11-18 2014-02-05 内蒙古中环光伏材料有限公司 Czochralski single-crystal production process capable of reducing swirl defect at head of single crystal and detection method
CN112048761A (en) * 2020-08-24 2020-12-08 有研半导体材料有限公司 Large-diameter monocrystalline silicon shouldering growth process
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