CN114481301A - Production process for reducing Czochralski single crystal bract breaking - Google Patents
Production process for reducing Czochralski single crystal bract breaking Download PDFInfo
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- CN114481301A CN114481301A CN202011259858.1A CN202011259858A CN114481301A CN 114481301 A CN114481301 A CN 114481301A CN 202011259858 A CN202011259858 A CN 202011259858A CN 114481301 A CN114481301 A CN 114481301A
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- 239000013078 crystal Substances 0.000 title claims abstract description 131
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 239000010453 quartz Substances 0.000 claims abstract description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 25
- 230000008569 process Effects 0.000 claims abstract description 22
- 230000007704 transition Effects 0.000 claims description 5
- 230000006641 stabilisation Effects 0.000 claims description 3
- 238000011105 stabilization Methods 0.000 claims description 3
- 239000000155 melt Substances 0.000 abstract description 16
- 239000012535 impurity Substances 0.000 abstract description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 239000007789 gas Substances 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 description 25
- 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
- 230000008859 change Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial 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
- 238000005259 measurement Methods 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
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
According to the production process for reducing the broken bract of the Czochralski single crystal, in the equal-diameter initial drawing process, the crystal growth height is divided into four stages, namely a first stage, a second stage, a third stage and a fourth stage; the method comprises the steps of controlling the crystal rotating speed, the quartz crucible rotating speed and the thermal field temperature of crystal growth in each stage; in the first stage to the fourth stage, the crystal rotating speed is increased slowly after the crystal rotating speed is operated at the initial rotating speed, and then the crystal rotating speed is operated at a constant rotating speed; the rotating speed of the quartz crucible is stable and unchanged at the initial rotating speed from the rotating shoulder to the constant-diameter initial stage; the stable thermal field temperature is firstly stably operated at the initial temperature of the constant-diameter initial stage after the shoulder turning is finished, then slowly reduced, and then continuously operated at the constant temperature. The invention reduces the friction between the quartz crucible and the melt, reduces the appearance of impurities, avoids the impurities from being enriched in the head section of the crystal, and reduces the probability of breaking bracts of the single crystal; meanwhile, the influence of the hot gas flow of the melt on the quality of the crystal is improved, so that the oxygen content at the head of the crystal is reduced, and the product quality is improved.
Description
Technical Field
The invention belongs to the technical field of Czochralski single crystal manufacturing, and particularly relates to a production process for reducing bract breaking of Czochralski single crystals.
Background
In the Czochralski single crystal pulling process, bract breaking is one of the main problems of single crystal pulling failure, the main factor of bract breaking is caused by excessive impurities in the quartz crucible, and especially in the pulling process at the equal diameter initial stage after shoulder turning, once the crystal turning rotating speed (crystal turning) and the crucible rotating speed (crucible turning) are not reasonably set, the 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 bract breaking is easily caused. In addition, in the drawing process, if the temperature of the thermal field is set unreasonably, the heat convection of the solution accelerates the accumulation of impurities at the head of the crystal, the crystal without growth stripes is easy to grow, and the risk of bract breaking is further accelerated. Once the bract breaking occurs, not only the production is 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 breakage of Czochralski single crystal, which is particularly suitable for the pulling process of crystal with the diameter of 210-.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a production process for reducing Czochralski single crystal bract breaking comprises dividing the crystal growth height into four stages in the equal-diameter initial stage drawing process after shoulder rotation, wherein the four stages are respectively an entry stage of a first stage, a transition stage of a second stage, an increase stage of a third stage and a stabilization stage of a fourth stage;
the method comprises the steps of controlling the crystal rotating speed, the quartz crucible rotating speed and the thermal field temperature of crystal growth in each stage; in the first stage to the fourth stage, the crystal rotating speed is firstly operated at the initial rotating speed and then slowly increased, and then the crystal rotating speed is operated at the constant rotating speed; the rotating speed of the quartz crucible is stable and unchanged at the initial rotating speed from the rotating shoulder to the constant-diameter initial stage; the stable thermal field temperature is firstly stably operated at the initial temperature of the constant-diameter initial stage after the shoulder turning is finished, then slowly reduced, and then continuously operated at the constant temperature.
Further, in the first stage, the crystal stably runs at an initial rotating speed; and the initial rotation speed of the crystal is the same as the rotation speed of the crystal at the end of shoulder rotation, and is 10 rpm.
Further, the crystal is slowly increased to 12rpm from the initial rotating speed in the second stage; and stably operated at 12rpm in the third and fourth stages.
Further, the rotation speed of the quartz crucible is always the same as that of the quartz crucible at the end of the shoulder rotation, and is 10 rpm.
Further, the temperature of the thermal field is stable and constant in the first stage and the second stage, and is the same as the initial temperature of the thermal field when the thermal field is turned to the initial stage of constant diameter at the end of shoulder turning.
Further, the thermal field temperature is reduced by 2-5Sp in the third stage on the basis of its initial temperature.
Further, the temperature of the thermal field is reduced by 3Sp based on the initial temperature in the third stage, and the reduced temperature of the thermal field is stably operated until the fourth stage is finished.
Further, the height of the first stage is 0-150 mm; the second stage height is 150-300 mm.
Further, the height of the third stage is 300-500 mm; the height of the fourth stage is 500-800 mm.
Further, the diameter of the crystal is 210-330 mm.
Compared with the prior art, the technical scheme is adopted, so that the friction between the quartz crucible and the molten silicon liquid is reduced, the occurrence of impurities is reduced, the impurities are prevented from being enriched in the head section of the crystal, and the probability of single crystal bract breaking is reduced; meanwhile, the influence of hot gas flow of the silicon liquid in the thermal field on the quality of the crystal can be improved, so that the oxygen content at the head of the crystal is reduced, the product quality is improved, and the production cost is reduced.
Drawings
FIG. 1 is a schematic structural diagram of a crystal isodiametric drawing according to an embodiment of the present invention;
FIG. 2 is a graph illustrating the distribution of isotherms in a solution at various crystal rotation speeds in accordance with one embodiment of the present invention.
In the figure:
10. crystal 20, quartz crucible 30, melt
40. Isotherm 50, lowest liquid level
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
The embodiment provides a production process for reducing czochralski single crystal breaking, which is suitable for the equal-diameter initial drawing process after shoulder rotation, particularly suitable for the crystal with the equal-diameter of 210 plus 330mm, wherein the growth height of the crystal 10 in the drawing process is divided into four stages, namely an entry 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 the crystal rotating speed, the quartz crucible rotating speed and the thermal field temperature for controlling the growth of the crystal 10. In the equal-diameter initial stage after shoulder turning, from the entry stage of the first stage to the stabilization stage of the fourth stage, the crystal rotation speed is increased slowly after the crystal rotation speed is operated at the initial rotation speed, and then the crystal rotation speed 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 rotary shoulder to the equal-diameter initial stage; the stable thermal field temperature is firstly stably operated at the initial temperature of the constant-diameter initial stage after the shoulder turning is finished, then slowly reduced, and then continuously operated at the constant temperature.
In this example, the diameter of the crystal 10 is chosen to be 210 mm.
Specifically, the first stage height is 0 to 150mm, and the crystal 10 enters the entry stage of the initial process of constant diameter. After the shoulder of the crystal 10 has been turned, the crystal 10 proceeds to the constant diameter stage, in which not only the diameter of the crystal 10 is controlled, but it is more important to maintain dislocation-free growth of the crystal 10. The initial rotation speed of the crystal 10 is the same as its rotation speed at the end of the shoulder rotation, 10rpm, and the entire first phase is run steadily at this initial rotation speed of 10 rpm. At this time, accordingly, the initial rotation speed of the quartz crucible 20 was 10rpm, which was the same as the rotation speed thereof at the end of the shoulder rotation. At this time, 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 the crystal growth.
In the process of crystal isodiametric measurement, if the rotating speed of the quartz crucible 20 is too high, the movement of the melt 30 itself may be more violent, and further, the metal ions on the inner wall layer of the quartz crucible 20 react with the molten silicon liquid to generate impurities which are not beneficial to crystal growth, and the impurities move along with the melt 30 more violent, and once the impurities are too much, the crystal is easy to break. If the rotation speed of the quartz crucible 20 is too low, the temperature of the solid-liquid interface of the crystal becomes too low, and dislocation in the crystal becomes more serious, which seriously affects the crystal quality. Therefore, in the initial stage of the crystal constant diameter, the rotation speed of the quartz crucible 20 is kept constant, and the rotation speed at the end of the shoulder rotation is maintained until the fourth stage is finished.
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. On the premise that the thermal field environment is approximately unchanged, in addition to compensating the heat transfer loss caused by the reduction of the silicon material in the growth process, the crystal rotating speed is required to be higher so as to keep the diameter of the crystal unchanged. In this phase, the crystal 10 is slowly raised from an initial rotation speed of 10rpm to 12rpm in steps; as the rotating speed of the crystal 10 is increased, under the action of the rotation of the crystal 10, the melt 30 below the solid-liquid interface flows upwards along the Z-axis direction under the action of the rotation of the crystal 10, heat enters the vicinity of the growth interface in a convection mode through the melt 30, so that the heat dissipation on the interface close to the edge of the crystal 10 is faster than that of the center, the shape of the solid-liquid interface, namely the crystal growth interface, is concave towards the melt 30 and continuously moves towards one side of the crystal, as shown in FIG. 2, the temperature variable of the thermal field is still 0 at the moment, and the position of the lowest liquid level 50 is at the solid-liquid intersection position.
In the case of equal-diameter drawing, the distribution of the solid-liquid interface is preferably in a smooth shape, and in order to reduce the tendency of the solid-liquid interface to be concave toward the melt 30, the temperature of the thermal field is reduced while the rotation speed of the crystal is kept constant, so that the change of the solid-liquid interface to be convex toward the crystal is reduced, and the change of the distance from the lowest liquid level 50 to the convex direction is reduced. Therefore, the crystal 10 is stably operated at the rotation speed of 12rpm in the third stage and the fourth stage, and the thermal field temperature is lowered in the third stage, and the thermal field temperature after having been lowered in the fourth stage is stable and unchanged.
In the process of increasing the crystal rotation speed, the solid-liquid interface and the crystals in the melt 30 rotate together, which causes the melt 30 to have viscosity, and the melt 30 forms forced convection after being influenced by the centrifugal force. As shown in FIG. 2, which is a graph illustrating the distribution of isotherms 40 in a melt at different crystal rotation speeds, it can be seen that the convection data for the melt 30 is different for different crystal rotations and that the isotherms 40 in the crystal portion all intersect at the lowest liquid level 50. When the crystal rotation speed reaches about 10rpm, the solid-liquid interface convection value at this time 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 with the increase of crystal transition, and the isotherm of the solid-liquid interface had the same tendency as that of FIG. 1, i.e., a convex direction toward the crystal 10 side. The rise 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 reducing and then increasing. As can be seen in the figure, the temperature at the bottom of the crucible is lowest at the crystal rotation speed of l0 rpm; when the crystal rotation speed is increased to 12rpm, the temperature of the bottom of the quartz crucible begins to rise, and when the crystal rotation speed is gradually increased to 14rpm, the temperature of the bottom of the crucible is obviously increased. Therefore, when the crystal grows in the initial stage with the same diameter, the crystal rotation speed is slowly increased to 12rpm, the quartz crucible rotation speed is kept at 10rpm, the crystal pulling speed is optimized correspondingly, 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, the original pulling speed is kept for pulling, and the crystal 10 with the stable diameter and good consistency can be obtained.
The height of the third stage is 300-500mm, which is an increasing stage in the initial growth process of the crystal 10 with the same diameter, in this stage, in order to keep the crystal 10 stably growing and simultaneously reduce the influence of the hot gas flow of the melt 30 on the solid-liquid interface, the variable of the thermal field temperature is required to be 2-5Sp, that is, 2-5Sp is reduced on the basis of the initial temperature to obtain a new thermal field temperature, preferably, the thermal field temperature is reduced by 3Sp on the basis of the initial temperature in this stage and continuously and stably runs to the end of the fourth stage by using the thermal field temperature; at this time, the rotation speed of the quartz crucible 20 is always the same as that at the end of the shoulder rotation, and is 10 rpm; and the crystal 10 is rotated at the same speed as the second stage is ended, i.e. 12 rpm.
The height of the fourth stage is 500-800mm, and the fourth stage is a stable stage of the equal-diameter initial growth process of the crystal 10, and the crystal at the stage directly enters the long-time stable drawing process of the equal-diameter process. In the 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 and is 10 rpm; accordingly, the temperature of the thermal field is constant over the end of the third stage.
In the initial stage of drawing the crystal 10 with equal diameter, the rotating speed of the crystal 10 is increased, the silicon liquid funnel effect generated by the rotation of the quartz crucible can be counteracted, the impurity enrichment area is avoided, the solution near the outer edge of the crystal 10 is pressed downwards to form stable reverse convection, and therefore the situation of single crystal bract breaking is improved.
The same applies to pulling of crystal 10 with a diameter within 210-330mm, and also reduces the single crystal break.
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 impurities are prevented from being enriched in the head section of the crystal, and the probability of breaking the bracts of the single crystal is reduced; meanwhile, the influence of hot airflow of the silicon liquid in the thermal field on the quality of the crystal can be improved, so that the oxygen content at the head of the crystal is reduced, the quality of the product is improved, and the production cost is reduced.
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 equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (10)
1. A production process for reducing Czochralski single crystal bract breaking is characterized in that in the equal-diameter initial drawing process after shoulder rotation, the crystal growth height is divided into four stages, namely an entry stage of a first stage, a transition stage of a second stage, an increase stage of a third stage and a stabilization stage of a fourth stage;
the method comprises the steps of controlling the crystal rotating speed, the quartz crucible rotating speed and the thermal field temperature of crystal growth in each stage; in the first stage to the fourth stage, the crystal rotating speed is firstly operated at the initial rotating speed and then slowly increased, and then the crystal rotating speed is operated at the constant rotating speed; the rotating speed of the quartz crucible is stable and unchanged at the initial rotating speed from the rotating shoulder to the constant-diameter initial stage; the stable thermal field temperature is firstly stably operated at the initial temperature of the constant-diameter initial stage after the shoulder turning is finished, then slowly reduced, and then continuously operated at the constant temperature.
2. The production process for reducing bract breakage of a Czochralski single crystal according to claim 1, wherein in the first stage, the crystal is stably operated at an initial rotation speed; and the initial rotation speed of the crystal is the same as the rotation speed of the crystal at the end of shoulder rotation, and is 10 rpm.
3. The production process for reducing the bract breakage of the Czochralski single crystal according to claim 2, wherein the crystal is slowly raised from an initial rotation speed to 12rpm in the second stage; and stably operated at 12rpm in the third and fourth stages.
4. The production process for reducing the bract breakage of the Czochralski single crystal according to any one of claims 1 to 3, wherein the rotation speed of the quartz crucible is always the same as that at the end of the shoulder rotation and is 10 rpm.
5. The production process for reducing bract breakage of a Czochralski single crystal according to claim 4, wherein the temperature of the thermal field is constant in the first stage and the second stage and is the same as the initial temperature at which it shifts to the beginning of constant diameter at the end of shoulder-shifting.
6. The production process for reducing Czochralski single crystal bract breaking according to claim 5, wherein the thermal field temperature is reduced by 2-5Sp based on the initial temperature thereof in the third stage.
7. The production process for reducing Czochralski single crystal bract breaking according to claim 6, wherein the thermal field temperature is reduced by 3Sp based on the initial temperature in the third stage, and the process is stably operated at the reduced thermal field temperature until the fourth stage is finished.
8. The production process for reducing Czochralski single crystal bract breakage according to any one of claims 1-3 and 5-7, wherein the height of the first stage is 0-150 mm; the second stage height is 150-300 mm.
9. The production process for reducing Czochralski single crystal bract breakage according to claim 8, wherein the height of the third stage is 300-500 mm; the height of the fourth stage is 500-800 mm.
10. The process for reducing the bract breakage of the Czochralski single crystal according to any one of claims 1-3, 5-7 and 9, wherein the crystal has a constant diameter of 210-330 mm.
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| CN202011259858.1A CN114481301B (en) | 2020-11-12 | 2020-11-12 | Production process for reducing broken bracts of Czochralski single crystal |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115404541A (en) * | 2022-10-18 | 2022-11-29 | 四川晶科能源有限公司 | Crystal pulling method |
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| 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115404541A (en) * | 2022-10-18 | 2022-11-29 | 四川晶科能源有限公司 | Crystal pulling method |
| CN115404541B (en) * | 2022-10-18 | 2023-08-25 | 四川晶科能源有限公司 | Crystal pulling method |
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