CN211367812U - Novel seed crystal for pulling single crystal - Google Patents
Novel seed crystal for pulling single crystal Download PDFInfo
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- CN211367812U CN211367812U CN201921976748.XU CN201921976748U CN211367812U CN 211367812 U CN211367812 U CN 211367812U CN 201921976748 U CN201921976748 U CN 201921976748U CN 211367812 U CN211367812 U CN 211367812U
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Abstract
The utility model provides a novel seed crystal is used to czochralski crystal, including coaxial coupling's one-level crystalline segment, second grade crystalline segment and tertiary crystalline segment in proper order, its characterized in that still includes the extension crystalline segment, the extension crystalline segment is arranged in tertiary crystalline segment is kept away from second grade crystalline segment one side, the extension crystalline segment is followed tertiary crystalline segment axis direction outwards and with tertiary crystalline segment body coupling sets up, the extension crystalline segment is the toper structure, the major diameter terminal surface of extension crystalline segment with tertiary crystalline segment external diameter is the same. The utility model provides a pair of novel seed crystal is used to czochralski single crystal is particularly useful for the single crystal drawing of at least once butt fusion, has solved the seed crystal among the prior art and has leaded to expanding the technical problem of shoulder or isometric disconnected bud in earlier stage easily, is favorable to reducing the thermal shock to single crystal growth when the butt fusion, and dislocation's production when reducing single crystal growth improves the single crystal one-time crystallization rate, reduction in production cost, improvement single crystal productivity.
Description
Technical Field
The utility model belongs to the technical field of the used accessory of solar energy czochralski silicon single crystal stove, especially, relate to a novel seed crystal for czochralski single crystal.
Background
The growth process of the czochralski single crystal mainly comprises the steps of clearing, melting, welding, temperature stabilization, seeding, shoulder expanding, shoulder rotating, constant diameter, ending and furnace stopping. When in welding, the seed crystal needs to be lowered to the liquid level to be contacted with the silicon melt, at the moment, because the thermal stress can generate a plurality of dislocations, the factors for generating the dislocations mainly comprise: the temperature difference between the seed crystal and the liquid level of the silicon melt during the contact and the sectional area of the seed crystal during the contact, but the thin seed crystal has the risk of breaking during the single crystal pulling process.
Chinese patent publication No. CN109338462A, which provides a diameter-variable seed crystal for pulling a single crystal and a seeding method, wherein the lower end face of the seed crystal structure contacting with silicon liquid is a circular structure, which is a common seed crystal structure, the diameter of the lower end face of the seed crystal is more than 10mm, but the structure is easy to form dislocation during the fusion process, and if the dislocation is not completely removed during the seeding process, the shoulder expansion or the bud breaking at the earlier stage with equal diameter is easy to cause.
SUMMERY OF THE UTILITY MODEL
The utility model provides a novel seed crystal for czochralski single crystal, which is especially suitable for single crystal pulling with at least one welding, and solves the technical problem that the seed crystal in the prior art easily leads to shoulder expanding or isometric early bract breaking.
In order to solve the technical problem, the utility model discloses a technical scheme is:
the utility model provides a novel seed crystal is used to czochralski crystal, includes coaxial coupling's one-level crystalline segment, second grade crystalline segment and tertiary crystalline segment in proper order, still includes the extension crystalline segment, the extension crystalline segment is arranged in tertiary crystalline segment is kept away from second grade crystalline segment one side, the extension crystalline segment is followed tertiary crystalline segment axis direction outwards and with tertiary crystalline segment body coupling sets up, the extension crystalline segment is the toper structure, the major diameter terminal surface of extension crystalline segment with tertiary crystalline segment external diameter is the same.
Further, the taper angle of the elongated segment is 30-90 °.
Further, the taper angle of the elongated segment is 63 ° 26'.
Further, the extension crystal segment and the third-stage crystal segment are coaxially arranged.
Further, the vertex angle of the extended crystal segment is in a circular arc structure.
Further, the length of the extended crystal segment is smaller than the diameter of the third-level crystal segment.
Further, the length of the extended segment is equal to 1/10-1/15 of the length of the tertiary segment.
Further, the diameter of the third-stage crystal section is 3-5 mm.
Furthermore, the diameter of the first-level crystal section is 5-7 mm.
Further, the length of the third-stage crystal section is 50-80 mm.
Compared with the prior art, the utility model provides a pair of novel seed crystal is used to czochralski single crystal is particularly useful for the single crystal drawing of at least one butt fusion, has solved the seed crystal among the prior art and has leaded to expanding the technical problem of shoulder or constant diameter break bract earlier stage easily, is favorable to reducing the thermal shock to single crystal growth when the butt fusion, dislocation's production when reducing single crystal growth, improves the single crystal one-time crystallization rate, reduction in production cost improves the single crystal productivity.
Drawings
FIG. 1 is a schematic view showing the structure of a novel seed crystal for pulling a single crystal according to an embodiment of the present invention;
fig. 2 is a schematic view of the positions of the seed crystal and the crucible during fusion according to an embodiment of the present invention.
In the figure:
10. seed crystal 11, primary crystal section 12 and secondary crystal section
13. Three-stage crystal segment 14, extended crystal segment 20 and seed crystal chuck
30. Weight 40, seed crystal rope 50 and guide cylinder
60. Crucible pot
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The utility model provides a novel seed crystal is used to czochralski crystal, as shown in figure 1, seed crystal 10 from the top down includes one-level crystalline segment 11, second grade crystalline segment 12 and tertiary crystalline segment 13 that coaxial coupling set up in proper order, still includes extension crystalline segment 14, and extension crystalline segment 14 sets up the one side of keeping away from second grade crystalline segment 12 at tertiary crystalline segment 13, and extension crystalline segment 14 outwards sets up along the axis direction of tertiary crystalline segment 13, and extension crystalline segment 14 is formed with tertiary crystalline segment 13, second grade crystalline segment 12 and 11 integrated into one piece of one-level crystalline segment.
Specifically, the first-level crystal segment 11 is a cylinder structure, the diameter d1 is 5-7mm, the first-level crystal segment 11 is adapted to the seed chuck 20 and is used for being fixedly connected with the seed chuck 20, so that the seed crystal 10 is clamped and fixed on a lifting device arranged in an auxiliary chamber of the single crystal furnace, as shown in fig. 2, the weight of the seed chuck 20 is driven by the weight 30 along with the seed crystal rope 40, the seed crystal 10 is driven to vertically move up and down, the seed crystal 10 is positioned right above the crucible 60, the seed crystal 10 and the seed chuck 20 are both positioned in the guide cylinder 50, and the guide cylinder 50 is positioned right above the silicon melt in the crucible 60. The second-stage crystal segment 12 is a transition segment and is of an inverted frustum structure and is used for connecting the first-stage crystal segment 11 and the third-stage crystal segment 13, namely, the large-diameter end face of the second-stage crystal segment 12 is connected with the same end face of the first-stage crystal segment 11, the small-diameter end face of the second-stage crystal segment 12 is connected with the same end face of the third-stage crystal segment 13, and the second-stage crystal segment 12 is arranged to obtain a standard small diameter, namely the diameter of the third-stage crystal segment 13, and meanwhile, the connection strength of the seed. The diameter d2 of the third-stage ingot 13, which is the diameter of the small diameter of the ingot in contact with the silicon material solution during the pulling of the single crystal, must be 3-5mm, and the length L1 of the third-stage ingot must be 50-80 mm.
Further, extended crystal segment 14 is a conical structure, as shown in fig. 1, extended crystal segment 14 and third-level crystal segment 13 are coaxially arranged, a large-diameter end face of extended crystal segment 14 is the same as the outer diameter of third-level crystal segment 13, the length of extended crystal segment 14 is not greater than the diameter of third-level crystal segment 13, and preferably, the length of extended crystal segment 14 is smaller than the diameter of third-level crystal segment 13 and the length of extended crystal segment 14 is equal to 1/10-1/15 of the length of third-level crystal segment 13. The taper angle theta of elongated segment 14 is 30-90 deg., preferably the taper angle theta of elongated segment 14 is 63 deg. 26'. The apex angle of the extension crystal section 14 is of a circular arc structure, so that the sharp end is prevented from pricking personnel when the seed crystal 10 is installed or moved, and dangerous accidents are prevented.
After the silicon raw material is charged, the seed crystal 10 is installed, the seed crystal 10 is fixed on a seed crystal chuck 20, evacuation, leakage detection, argon filling and power rise are sequentially carried out, the silicon raw material is melted, and after the melting is finished, temperature stabilization is carried out on the silicon liquid, so that the temperature of the silicon liquid and a thermal field is controlled to be adjusted to be suitable for the process temperature during fusion welding, the liquid level temperature is 1450 ℃, and the gap between the liquid level of the molten silicon in the crucible 60 and the guide cylinder 50 is ensured to be 15-30mm during temperature stabilization. The purpose of temperature stabilization is to place the molten silicon at uneven temperature, if the temperature is too low, the seed crystal 10 will solidify along the liquid surface during welding, if the temperature is too low, the welding will be insufficient, and qualified single crystals will be difficult to grow after necking down; if the temperature is too high, the seed crystal 10 will be melted. After the temperature is stabilized, the seed crystal 10 begins to slowly descend and the lower end surface of the extended crystal section 14 is enabled to reach the position 3-5mm from the liquid level of the molten silicon in the crucible 60, and the seed crystal 10 begins to be preheated so as to reduce the temperature difference between the seed crystal 10 and the molten silicon and further reduce the thermal stress generated in the seed crystal 10 when the seed crystal 10 is contacted with the molten silicon. After preheating, slowly descending the seed crystal 10 to the liquid level of the molten silicon, and fully contacting the extension crystal section 14 in the seed crystal 10 with the molten silicon. In the fusion process, when the seed crystal is contacted with the high-temperature melt, a large amount of dislocation can be generated on the surface of the seed crystal 10 contacted with the liquid surface due to thermal shock, the number of the dislocation is in direct proportion to the contact area, the larger the dislocation amount, the smaller the area, the smaller the dislocation amount, the extended crystal section 14 is of an inverted cone structure, the extended crystal section is firstly contacted with the molten silicon, and the area is smaller, so that the dislocation on the extended crystal section 14 is reduced; meanwhile, the extension crystal section 14 with the conical structure can dissipate heat more easily, and can further reduce internal thermal stress, thereby reducing the number of dislocations. When the taper angle θ of the extended segment 14 is greater than 90 °, the reduction of thermal stress is not facilitated, and when the taper angle θ of the extended segment 14 is less than 30 °, the thermal impact force of the extended segment 14 is increased, which is not suitable for the reduction of dislocations. Preferably, when the taper angle θ of the extension segment 14 is 63 ° 26', the number of dislocations on the surface of the seed crystal 10 is minimized, and the thermal impact on the surface of the seed crystal 10 during the fusion process is reduced, so that the rate of formation of the single crystal can be increased, and the yield of the single crystal can be improved. When the seed crystal 10 is first welded, care is taken to set a minimum position value of the seed crystal 10 to prevent the seed crystal 10 from being completely melted due to the continuous melting of the seed crystal caused by too high temperature and even to immerse the seed holder 20 in the silicon liquid. The seed crystal 10 is sufficiently fused with the silicon liquid and is maintained in a state where it is not grown and is not melted for a long time, and the seeding stage of the single crystal growth process can be started after this state is reached.
Furthermore, for the same seed crystal 10, the multiple use can be realized, at least one welding is generated, and when the second welding is performed, in order to ensure the stability of the welding process, the sizes of the guide cylinder 50, the seed crystal 10, the seed chuck 20 and the weight 30 must be ensured to be the same from front to back, so that the position of the seed crystal 10 is still consistent with the first welding position when the welding is performed again. Furthermore, in order to ensure that the position of the seed crystal 10 is consistent when the secondary fusion is carried out, after the extended crystal section 14 in the seed crystal 10 is contacted with the molten silicon liquid level, the positions of the seed crystal 10, the seed holder 20, the weight 30 and the seed crystal rope 40 in the auxiliary chamber of the single crystal furnace are relatively consistent, so that the heat emitted by the heat conduction in the seed crystal 10 and the seed holder 20 is the same as the first fusion, the consistency of the influence on the molten silicon liquid level temperature when the seed crystal 10 is fused can be ensured, and the fusion process is more stable. The positions of the seed crystals 10 are consistent during multiple times of welding, so that the seed crystals 10 can be repeatedly used, the use cost of the seed crystals is reduced, the number of times of melting back is reduced, the single crystal yield can be increased, and the single crystal yield can be improved.
After welding, the seeding process can be started, the seed crystal 10 slowly descends, the crucible rotation speed descends first and then ascends, the crucible rotation speed descends from 10rpm to 5rpm first and then ascends from 5rpm to 10rpm, and the dislocation generated by initial seeding can be removed. The dislocation is grown to the surface of the seed crystal and stopped during seeding, so that dislocation-free crystal nucleus is obtained and the dislocation generated during welding is eliminated. In the seeding process, the seeding diameter and length are based on effective elimination of dislocation, the diameter is required to be 4.5-5.5mm usually, the effective length of the thin neck is not less than one diameter of the pulled single crystal, and the proper increase of the seeding length is not only beneficial to elimination of dislocation, but also beneficial to the stability of liquid level temperature, thereby improving the success rate of shouldering.
The extension crystal section 14 is added on the basis of the existing seed crystal structure, so that thermal impact on single crystal growth is reduced during welding, dislocation generation during single crystal growth is reduced, the one-time crystallization rate of the single crystal is improved, the production cost is reduced, and the single crystal production capacity is improved.
A fusion process of a novel seed crystal for Czochralski single crystal, which employs the novel seed crystal as described in any one of the above items, comprises:
after the silicon raw material is charged, the seed crystal 10 is installed, the seed crystal 10 is fixed on a seed crystal chuck 20, evacuation, leakage detection, argon filling and power rise are sequentially carried out, the silicon raw material is melted, and after the melting is finished, temperature stabilization is carried out on the silicon liquid, so that the temperature of the silicon liquid and a thermal field is controlled to be adjusted to be suitable for the process temperature during fusion welding, the liquid level temperature is 1450 ℃, and the gap between the liquid level of the molten silicon in the crucible 60 and the guide cylinder 50 is ensured to be 15-30mm during temperature stabilization. The purpose of temperature stabilization is to place the molten silicon at uneven temperature, if the temperature is too low, the seed crystal 10 will solidify along the liquid surface during welding, if the temperature is too low, the welding will be insufficient, and qualified single crystals will be difficult to grow after necking down; if the temperature is too high, the seed crystal 10 will be melted. After the temperature is stabilized, the seed crystal 10 begins to slowly descend and the lower end surface of the extended crystal section 14 is enabled to reach the position 3-5mm from the liquid level of the molten silicon in the crucible 60, and the seed crystal 10 begins to be preheated so as to reduce the temperature difference between the seed crystal 10 and the molten silicon and further reduce the thermal stress generated in the seed crystal 10 when the seed crystal 10 is contacted with the molten silicon. After preheating, slowly descending the seed crystal 10 to the liquid level of the molten silicon, and fully contacting the extension crystal section 14 in the seed crystal 10 with the molten silicon. In the fusion process, when the seed crystal is contacted with the high-temperature melt, a large amount of dislocation can be generated on the surface of the seed crystal 10 contacted with the liquid surface due to thermal shock, the number of the dislocation is in direct proportion to the contact area, the larger the dislocation amount, the smaller the area, the smaller the dislocation amount, the extended crystal section 14 is of an inverted cone structure, the extended crystal section is firstly contacted with the molten silicon, and the area is smaller, so that the dislocation on the extended crystal section 14 is reduced; meanwhile, the extension crystal section 14 with the conical structure can dissipate heat more easily, and can further reduce internal thermal stress, thereby reducing the number of dislocations. When the taper angle θ of the extended segment 14 is greater than 90 °, the reduction of thermal stress is not facilitated, and when the taper angle θ of the extended segment 14 is less than 30 °, the thermal impact force of the extended segment 14 is increased, which is not suitable for the reduction of dislocations. Preferably, when the taper angle θ of the extension segment 14 is 63 ° 26', the number of dislocations on the surface of the seed crystal 10 is minimized, and the thermal impact on the surface of the seed crystal 10 during the fusion process is reduced, so that the rate of formation of the single crystal can be increased, and the yield of the single crystal can be improved. When the seed crystal 10 is first welded, care is taken to set a minimum position value of the seed crystal 10 to prevent the seed crystal 10 from being completely melted due to the continuous melting of the seed crystal caused by too high temperature and even to immerse the seed holder 20 in the silicon liquid. The seed crystal 10 is sufficiently fused with the silicon liquid and is maintained in a state where it is not grown and is not melted for a long time, and the seeding stage of the single crystal growth process can be started after this state is reached.
Furthermore, for the same seed crystal 10, the multiple use can be realized, at least one welding is generated, and when the second welding is performed, in order to ensure the stability of the welding process, the sizes of the guide cylinder 50, the seed crystal 10, the seed chuck 20 and the weight 30 must be ensured to be the same from front to back, so that the position of the seed crystal 10 is still consistent with the first welding position when the welding is performed again. Furthermore, in order to ensure that the position of the seed crystal 10 is consistent when the secondary fusion is carried out, after the extended crystal section 14 in the seed crystal 10 is contacted with the molten silicon liquid level, the positions of the seed crystal 10, the seed holder 20, the weight 30 and the seed crystal rope 40 in the auxiliary chamber of the single crystal furnace are relatively consistent, so that the heat emitted by the heat conduction in the seed crystal 10 and the seed holder 20 is the same as the first fusion, the consistency of the influence on the molten silicon liquid level temperature when the seed crystal 10 is fused can be ensured, and the fusion process is more stable. The positions of the seed crystals 10 are consistent during multiple times of welding, so that the seed crystals 10 can be repeatedly used, the use cost of the seed crystals is reduced, the number of times of melting back is reduced, the single crystal yield can be increased, and the single crystal yield can be improved.
After welding, the seeding process can be started, the seed crystal 10 slowly descends, the crucible rotation speed descends first and then ascends, the crucible rotation speed descends from 10rpm to 5rpm first and then ascends from 5rpm to 10rpm, and the dislocation generated by initial seeding can be removed. The dislocation is grown to the surface of the seed crystal and stopped during seeding, so that dislocation-free crystal nucleus is obtained and the dislocation generated during welding is eliminated. In the seeding process, the seeding diameter and length are based on effective elimination of dislocation, the diameter is required to be 4.5-5.5mm usually, the effective length of the thin neck is not less than one diameter of the pulled single crystal, and the proper increase of the seeding length is not only beneficial to elimination of dislocation, but also beneficial to the stability of liquid level temperature, thereby improving the success rate of shouldering.
Compared with the prior art, adopt the utility model provides a pair of novel seed crystal is used to czochralski single crystal is particularly useful for the single crystal of at least one butt fusion and draws, has solved the seed crystal among the prior art and has leaded to expanding the technical problem of shoulder or constant diameter break bract earlier stage easily, is favorable to reducing the thermal shock to single crystal growth when the butt fusion, dislocation's production when reducing single crystal growth improves the single crystal and once becomes the crystal rate, reduction in production cost improves the single crystal productivity. The utility model also provides a fusion welding process of the novel seed crystal for the Czochralski single crystal, which not only reduces the number of meltback times, but also improves the crystallization rate of the single crystal.
The embodiments of the present invention have been described in detail, and the description is only for the preferred embodiments of the present invention, and should not be construed as limiting the scope of the present invention. All the equivalent changes and improvements made according to the application scope of the present invention should still fall within the patent coverage of the present invention.
Claims (10)
1. The utility model provides a novel seed crystal is used to czochralski crystal, includes coaxial coupling's one-level crystalline segment, second grade crystalline segment and tertiary crystalline segment in proper order, its characterized in that still includes the extension crystalline segment, the extension crystalline segment is arranged in tertiary crystalline segment is kept away from second grade crystalline segment one side, the extension crystalline segment is followed tertiary crystalline segment axis direction outwards and with tertiary crystalline segment body coupling sets up, the extension crystalline segment is the toper structure, the major diameter terminal surface of extension crystalline segment with tertiary crystalline segment external diameter is the same.
2. A novel seed crystal for pulling a single crystal as set forth in claim 1, wherein said elongated segment has a taper angle of 30 to 90 °.
3. A novel seed crystal for pulling a single crystal as set forth in claim 2, wherein said elongated segment has a taper angle of 63 ° 26'.
4. A novel seed crystal for Czochralski single crystal as set forth in any one of claims 1 to 3, wherein said elongated segment is coaxially disposed with said tertiary segment.
5. A novel seed crystal for pulling a single crystal as set forth in claim 4, wherein said apex angle of said elongated segment has a circular arc-shaped configuration.
6. A novel seed crystal for pulling a single crystal as set forth in claim 5, wherein said elongated segment has a length smaller than the diameter of said tertiary segment.
7. A novel seed crystal for pulling a Czochralski single crystal as set forth in claim 6, wherein the length of said elongated segment is equal to 1/10-1/15 of the length of said tertiary segment.
8. A novel seed crystal for Czochralski single crystal as claimed in any one of claims 1-3 and 5-7, wherein said tertiary segment has a diameter of 3-5 mm.
9. A novel seed crystal for Czochralski single crystal as set forth in claim 8, wherein said primary segment has a diameter of 5-7 mm.
10. A novel seed crystal for Czochralski single crystal as set forth in claim 9, wherein the length of said tertiary crystal segment is 50-80 mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110670122A (en) * | 2019-11-15 | 2020-01-10 | 内蒙古中环光伏材料有限公司 | Novel seed crystal for pulling single crystal and welding process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110670122A (en) * | 2019-11-15 | 2020-01-10 | 内蒙古中环光伏材料有限公司 | Novel seed crystal for pulling single crystal and welding process |
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