CN114481301B - Production process for reducing broken bracts of Czochralski single crystal - Google Patents
Production process for reducing broken bracts of Czochralski single crystal Download PDFInfo
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- CN114481301B CN114481301B CN202011259858.1A CN202011259858A CN114481301B CN 114481301 B CN114481301 B CN 114481301B CN 202011259858 A CN202011259858 A CN 202011259858A CN 114481301 B CN114481301 B CN 114481301B
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- 239000013078 crystal Substances 0.000 title claims abstract description 125
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000010453 quartz Substances 0.000 claims abstract description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 26
- 230000008569 process Effects 0.000 claims abstract description 26
- 230000007704 transition Effects 0.000 claims description 5
- 230000000087 stabilizing effect Effects 0.000 claims description 4
- 239000000155 melt Substances 0.000 abstract description 14
- 239000012535 impurity Substances 0.000 abstract description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 description 24
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- 238000009826 distribution Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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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
- C30B15/20—Controlling or regulating
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
In the production process for reducing the breaking bract of the Czochralski single crystal, in the initial drawing process of the constant diameter, the crystal growth height is divided into four stages, namely a first stage, a second stage, a third stage and a fourth stage; the crystal rotating speed, the quartz crucible rotating speed and the thermal field temperature for controlling the crystal growth are included in each stage; in the first stage to the fourth stage, the crystal rotation speed is firstly operated at an initial rotation speed and then slowly increased, and then is operated at a constant rotation speed; the rotation speed of the quartz crucible is stable and unchanged at the initial rotation speed from the shoulder to the initial constant diameter stage; the stable thermal field temperature is firstly stabilized at an initial temperature shifted to an initial constant diameter stage from the end of shoulder turning, then slowly reduced, and then continuously operated at a constant temperature. The invention reduces the friction between the quartz crucible and the melt, reduces the occurrence of impurities, avoids the enrichment of the impurities at the head section of the crystal, and reduces the probability of breaking the single crystal; meanwhile, the influence of the hot air flow of the melt on the crystal quality is improved, so that the oxygen content of the head part of the crystal is reduced, and the product quality is improved.
Description
Technical Field
The invention belongs to the technical field of Czochralski crystal manufacturing, and particularly relates to a production process for reducing breaking bracts of Czochralski crystals.
Background
In the process of pulling a single crystal, the breaking bud is one of the main problems of single crystal pulling failure, and the main factor of the breaking bud is caused by excessive impurities in a quartz crucible, especially in the initial drawing process of constant diameter after shoulder turning, once the crystal turning speed (crystal turning) and the crucible turning speed (crucible turning) are unreasonably set, friction between molten silicon liquid and the quartz crucible is increased, so that the impurities in the quartz crucible enter the silicon liquid, and the breaking bud is easy to cause. In addition, if the temperature setting of the thermal field is unreasonable in the drawing process, the aggregation of impurities at the head of the crystal is accelerated by the heat convection of the solution, so that the crystal without growth stripes is easy to grow, and the risk of breaking the bud is further accelerated. Once the bud is broken, not only is production interrupted, but also the waste of resources is caused, and the production cost is increased.
Disclosure of Invention
The invention provides a production process for reducing breaking bracts of a Czochralski single crystal, which is particularly suitable for a crystal with the diameter of 210-330mm in the drawing process of an equal-diameter initial stage after shoulder turning, and mainly solves the technical problem that breaking bracts are easy to occur in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
in the production process for reducing the breaking bract of the Czochralski single crystal, in the initial drawing process of constant diameter after shoulder turning, the crystal growth height is divided into four stages, namely an entering stage of a first stage, a transition stage of a second stage, an increasing stage of a third stage and a stabilizing stage of a fourth stage;
the crystal rotating speed, the quartz crucible rotating speed and the thermal field temperature for controlling the crystal growth are included in each stage; in the first stage to the fourth stage, the crystal rotation speed is firstly operated at an initial rotation speed and then slowly increased, and then is operated at a constant rotation speed; the rotating speed of the quartz crucible is stable and unchanged at an initial rotating speed from a shoulder to an initial constant diameter; the temperature of the stable thermal field is firstly reduced slowly after the stable operation is carried out at the initial temperature which is shifted to the initial stage of the constant diameter from the end of shoulder turning, and then the stable thermal field is continuously operated at the constant temperature.
Further, in the first stage, the crystal is stably operated at an initial rotational speed; and the initial rotation speed of the crystal is 10rpm which is the same as the rotation speed at the end of the shoulder rotation.
Further, the crystals slowly rise from the initial rotational speed to 12rpm in the second stage; and stably operated at 12rpm in the third and fourth stages.
Further, the rotational speed of the quartz crucible is always the same as the rotational speed thereof at the end of the shoulder, and is 10rpm.
Further, the thermal field temperature is stable in the first stage and the second stage and is the same as the initial temperature at which the shoulder turning is performed at the initial stage of the constant diameter.
Further, the thermal field temperature is reduced by 2-5Sp based on its initial temperature in the third stage.
Further, the thermal field temperature is lowered by 3Sp on the basis of the initial temperature thereof in the third stage, and the reduced thermal field temperature is stably operated to the end of the fourth stage.
Further, the height of the first stage is 0-150mm; the height of the second stage is 150-300mm.
Further, the height of the third stage is 300-500mm; the height of the fourth stage is 500-800mm.
Further, the diameter of the crystal with the same diameter is 210-330mm.
Compared with the prior art, by adopting the technical scheme, the friction between the quartz crucible and the molten silicon liquid is reduced, the occurrence of impurities is reduced, the enrichment of the impurities at the head section of the crystal is avoided, and the probability of breaking bracts of the single crystal is reduced; meanwhile, the influence of the hot air flow of the silicon liquid on the crystal quality in the thermal field can be improved, so that the oxygen content of the crystal head is reduced, the product quality is improved, and the production cost is reduced.
Drawings
FIG. 1 is a schematic diagram of a crystal isodiametric drawing structure according to an embodiment of the present invention;
FIG. 2 is a graph showing an exemplary distribution of isotherms in solution at different crystal speeds in accordance with one embodiment of the present invention.
In the figure:
10. crystal 20, quartz crucible 30, melt
40. Isotherm 50, minimum liquid level
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples.
The embodiment proposes a production process for reducing breaking bract of a Czochralski single crystal, as shown in FIG. 1, which is suitable for a constant diameter initial drawing process after shoulder turning, particularly suitable for a crystal with a constant diameter of 210-330mm, wherein the growth height of the crystal 10 in the drawing process is divided into four stages, namely an entering stage of a first stage, a transition stage of a second stage, an increasing stage of a third stage and a stabilizing stage of a fourth stage, wherein each stage comprises a crystal rotation speed, a quartz crucible rotation speed and a thermal field temperature for controlling the growth of the crystal 10. In the initial constant diameter stage after shoulder rotation, the crystal rotation speed is slowly increased after the crystal rotation speed is operated at the initial rotation speed from the entering stage of the first stage to the stabilizing stage of the fourth stage, and then the crystal rotation speed is operated at the constant rotation speed; the rotation speed of the quartz crucible is stable and unchanged at the initial rotation speed from the shoulder to the initial constant diameter stage; the stable thermal field temperature is firstly stabilized at an initial temperature shifted to an initial constant diameter stage from the end of shoulder turning, then slowly reduced, and then continuously operated at a constant temperature.
In this embodiment, the diameter of the selection crystal 10 is 210mm.
Specifically, the first stage has a height of 0-150mm, and the crystal 10 enters the entry section of the initial isodiametric process. After the shoulder of the crystal 10 is completed, the crystal enters an isodiametric stage in which not only is the diameter of the crystal 10 controlled, but it is also important to maintain dislocation-free growth of the crystal 10. The initial rotation speed of the crystal 10 was 10rpm which was the same as the rotation speed at the end of the shoulder, and the entire first stage was stably operated at the initial rotation speed of 10rpm. At this time, accordingly, the initial rotation speed of the quartz crucible 20 was 10rpm which was the same as the rotation speed at the end of the shoulder rotation. In this case, the temperature of the thermal field is the same as the temperature at the end of the shoulder rotation, that is, the variable of the thermal field is 0 in the first stage, in order to maintain crystal growth.
In the process of crystal constant diameter, if the rotation speed of the quartz crucible 20 is too high, the movement generated by the melt 30 is more severe, and then metal ions on the inner wall layer of the quartz crucible 20 react with molten silicon liquid to generate impurities which are unfavorable for crystal growth, and the impurities move more strongly along with the melt 30, so that once the impurities are too much, the crystal is liable to break. If the rotation speed of the quartz crucible 20 is too small, the temperature of the solid-liquid interface of the crystal is too low, and dislocation in the crystal is increased, which seriously affects the quality of the crystal. Therefore, the rotation speed of the quartz crucible 20 is kept constant throughout the initial constant diameter of the crystal, and the rotation speed at the end of the shoulder rotation is maintained until the end of the fourth stage.
The height in the second stage is 150-300mm, which is the transition section in the initial process of the equal diameter of the crystal 10. Since the thermal field environment is substantially unchanged, in addition to compensating for heat transfer loss caused by the reduction of silicon material during growth, a higher crystal rotation speed is required to keep the crystal diameter unchanged. In this stage, the crystal 10 is gradually slowly raised from the initial rotation speed of 10rpm to 12rpm; due to the increase of the rotation speed of the crystal 10, under the rotation of the crystal 10, the melt 30 below the solid-liquid interface flows upwards along the Z-axis under the rotation of the crystal 10, and heat enters the vicinity of the growth interface in a convection manner through the melt 30, so that the heat dissipation at the interface near the edge of the crystal 10 is faster than that at the center, the shape of the solid-liquid interface, i.e. the crystal growth interface, is concave to the melt 30 and continuously moves to one side of the crystal, as shown in fig. 2, at this time, the temperature variable of the thermal field is still 0, and the position of the lowest liquid level 50 is at the solid-liquid intersection position.
In order to reduce the tendency of the concave solid-liquid interface to the melt 30, the thermal field temperature is reduced to reduce the variation of the convex solid-liquid interface to the crystal side and the variation of the distance of the lowest liquid surface 50 from the convex solid-liquid interface to the crystal side. Therefore, the crystal 10 is stably operated at a rotation speed of 12rpm in the third stage and the fourth stage, and the thermal field temperature is reduced in the third stage, and the thermal field temperature after having been reduced in the fourth stage is stable and unchanged.
During the increase in crystal rotation speed, the melt 30 has viscosity due to the co-rotation of the solid-liquid interface with the crystals in the melt 30, and the melt 30 forms forced convection after being influenced by centrifugal force. As shown in fig. 2, an exemplary graph of the distribution of isotherms 40 in solution at different crystal speeds shows that the corresponding melt 30 convection data is different for different crystal revolutions and that the isotherms 40 in the crystal portion all intersect at the lowest level 50. When the crystal rotation speed reaches about 10rpm, the solid-liquid interface convection value is only 1, and when the crystal rotation speed reaches about 12rpm, forced convection occurs; from these data, it was found that the temperature of the melt 30 at the solid-liquid interface was continuously increased as the crystal transition was increased, and the trend of the isotherm at the solid-liquid interface was the same as that of fig. 1, i.e., convex toward the side of the crystal 10. The raising of the solid-liquid interface melt 30 can effectively reduce supercooling, improve the stability of crystal growth, and the melt temperature at the bottom of the quartz crucible is in a change trend of firstly decreasing and then increasing. As can be seen, the crucible bottom temperature is at its lowest at crystal speed of l 0rpm; when the crystal rotation speed is increased to 12rpm, the temperature at the bottom of the quartz crucible starts to rise, and when the crystal rotation speed is gradually increased to 14rpm, the temperature at the bottom of the crucible is obviously increased. Therefore, when the crystal grows in the initial stage of equal diameter, the crystal rotating speed is slowly increased to 12rpm, the quartz crucible rotating speed is kept at 10rpm, and the crystal pulling speed is correspondingly optimized, namely, the pulling speed can be slightly reduced in a high pulling speed interval in the crystal growth process, the pulling speed is increased after the interface is stable, and the original pulling speed is kept, so that the crystal 10 with stable diameter and good consistency can be obtained.
The third stage has a height of 300-500mm and is an increasing stage in the initial growth process of the crystal 10 with equal diameter, in which stage, in order to keep stable growth of the crystal 10 and reduce the influence of hot air flow of the melt 30 on a solid-liquid interface, the variable of the thermal field temperature is required to be 2-5Sp, namely, the thermal field temperature is reduced by 2-5Sp based on the initial temperature, so as to obtain a new thermal field temperature, preferably, the thermal field temperature is reduced by 3Sp based on the initial temperature in the stage, and the thermal field temperature is continuously and stably operated until the fourth stage is finished; at this time, the rotation speed of the quartz crucible 20 was always the same as that at the end of the shoulder, and was 10rpm; and the rotation speed of the crystal 10 is the same as that at the end of the second stage, i.e., 12rpm.
The fourth stage has a height of 500-800mm, and is a stable stage of the initial growth process of the crystal 10 in the equal diameter, and the crystal after the stage directly enters the long-time stable drawing in the equal diameter process. In this process, the rotation speed of the crystal 10 is the same as that of the third stage, namely, 12rpm, and the rotation speed of the quartz crucible 20 is still unchanged, namely, 10rpm; accordingly, the thermal field temperature continues unchanged at the end of the third phase.
In the initial drawing process of the crystal 10 with equal diameter, the rotation speed of the crystal 10 is increased, so that the silicon liquid funnel effect generated by the rotation of the quartz crucible can be counteracted, an impurity enrichment region is avoided, and the solution near the outer edge of the crystal 10 is downwards pressed to form stable reverse convection, thereby achieving the purpose of improving the single crystal breaking bud condition.
The above is still applicable to the pulling of the crystal 10 with the diameter of 210-330mm, and the single crystal breaking bud condition can be reduced.
By adopting the technical scheme, the friction between the quartz crucible and the molten silicon liquid can be reduced, the occurrence of impurities is reduced, the enrichment of the impurities at the head section of the crystal is avoided, and the probability of breaking bracts of the single crystal is reduced; meanwhile, the influence of the hot air flow of the silicon liquid on the crystal quality in the thermal field can be improved, so that the oxygen content of the crystal head is reduced, the product quality is improved, and the production cost is reduced.
The foregoing detailed description of the embodiments of the invention has been presented only to illustrate the preferred embodiments of the invention and should not be taken as limiting the scope of the invention. All equivalent changes and modifications within the scope of the present invention are intended to be covered by the present invention.
Claims (9)
1. The production process for reducing the breaking bract of the Czochralski single crystal is characterized in that in the initial drawing process of constant diameter after shoulder turning, the crystal growth height is divided into four stages, namely an entering stage of a first stage, a transition stage of a second stage, a growing stage of a third stage and a stabilizing stage of a fourth stage;
the crystal rotating speed, the quartz crucible rotating speed and the thermal field temperature for controlling the crystal growth are included in each stage; in the first stage to the fourth stage, the crystal rotation speed is firstly operated at an initial rotation speed and then slowly increased, and then is operated at a constant rotation speed; the rotating speed of the quartz crucible is stable and unchanged at an initial rotating speed from a shoulder to an initial constant diameter; the temperature of the thermal field is firstly reduced slowly after the initial temperature which is switched into the initial stage of the constant diameter from the end of shoulder turning is operated stably, and then the operation is continued at a constant temperature;
in the first stage, the initial rotation speed of the crystal is the same as the rotation speed of the crystal at the end of the shoulder rotation;
in the second stage, the crystal is slowly increased from an initial rotation speed and stably operated in the third and fourth stages;
the rotating speed of the quartz crucible is always the same as the rotating speed of the quartz crucible at the end of the shoulder rotation;
the temperature of the thermal field is stable and unchanged in the first stage and the second stage, and is the same as the initial temperature of the thermal field at the beginning of the equal diameter when the shoulder turning is finished.
2. The process for producing a reduced Czochralski single crystal breaking bud of claim 1, wherein in the first stage, the crystal is stably operated at an initial rotational speed; and the initial rotation speed of the crystal is 10rpm.
3. The process for producing a reduced Czochralski single crystal breaking bud of claim 2, wherein the crystal is slowly raised from an initial rotational speed to 12rpm in the second stage; and stably operated at 12rpm in the third and fourth stages.
4. The process for reducing the breaking bract of a Czochralski crystal according to any one of claims 1 to 3, wherein the rotation speed of the quartz crucible is always 10rpm which is the same as the rotation speed thereof at the end of shoulder turning.
5. The process of claim 1, wherein the thermal field temperature is reduced by 2-5Sp based on the initial temperature in the third stage.
6. The process according to claim 5, wherein the thermal field temperature is lowered by 3Sp based on the initial temperature thereof in the third stage, and the reduced thermal field temperature is stably operated to the end of the fourth stage.
7. The process for producing a reduced breaking bud of Czochralski crystal of any one of claims 1-3, 5-6, wherein the first stage height is 0-150mm; the height of the second stage is 150-300mm.
8. The process for reducing the breaking bract of a Czochralski crystal of claim 7, wherein the third stage height is 300-500mm; the height of the fourth stage is 500-800mm.
9. The process for producing a reduced Czochralski single crystal breaking bud according to any one of claims 1 to 3, 5 to 6, and 8, wherein the crystal has an isodiametric diameter of 210 to 330mm.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11278993A (en) * | 1998-03-31 | 1999-10-12 | Sumitomo Metal Ind Ltd | Growth of single crystal |
| CN102220632A (en) * | 2011-06-23 | 2011-10-19 | 英利能源（中国）有限公司 | Technical method of N-type Czochralski silicon monocrystal |
| CN108411360A (en) * | 2018-04-13 | 2018-08-17 | 内蒙古中环光伏材料有限公司 | A kind of method of full nitrogen growth czochralski silicon monocrystal |
| CN109097825A (en) * | 2018-08-29 | 2018-12-28 | 内蒙古中环协鑫光伏材料有限公司 | A kind of process for preventing pulling of crystals growth from shaking |
-
2020
- 2020-11-12 CN CN202011259858.1A patent/CN114481301B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11278993A (en) * | 1998-03-31 | 1999-10-12 | Sumitomo Metal Ind Ltd | Growth of single crystal |
| CN102220632A (en) * | 2011-06-23 | 2011-10-19 | 英利能源（中国）有限公司 | Technical method of N-type Czochralski silicon monocrystal |
| CN108411360A (en) * | 2018-04-13 | 2018-08-17 | 内蒙古中环光伏材料有限公司 | A kind of method of full nitrogen growth czochralski silicon monocrystal |
| CN109097825A (en) * | 2018-08-29 | 2018-12-28 | 内蒙古中环协鑫光伏材料有限公司 | A kind of process for preventing pulling of crystals growth from shaking |
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