CN113417003A - Large-diameter monocrystalline silicon production method and device capable of reducing oxygen content in head - Google Patents
Large-diameter monocrystalline silicon production method and device capable of reducing oxygen content in head Download PDFInfo
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- CN113417003A CN113417003A CN202110688408.2A CN202110688408A CN113417003A CN 113417003 A CN113417003 A CN 113417003A CN 202110688408 A CN202110688408 A CN 202110688408A CN 113417003 A CN113417003 A CN 113417003A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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Abstract
The invention provides a method and a device for producing large-diameter monocrystalline silicon capable of reducing oxygen content in a head, and belongs to the technical field of monocrystalline silicon production. During production, after a monocrystalline silicon raw material is melted, an oxygen reduction treatment process is added, the flow of argon is increased to 1.5-3 times of the flow of the argon after the melting is finished while the silicon melt is stirred, and/or the pressure in a crystal pulling furnace is increased to 1.5-3 times of the pressure in the furnace after the melting is finished.
Description
Technical Field
The invention belongs to the technical field of monocrystalline silicon production, and particularly relates to a method and a device for producing large-diameter monocrystalline silicon, which can reduce the oxygen content of a head.
Background
In the growth process of silicon single crystals by the Czochralski method, the oxygen content at the head of the crystal bar is often higher, the performances of the crystalline silicon and devices are influenced, and the photoelectric conversion efficiency of the silicon solar cell is reduced. In the prior art, the main ways of reducing the oxygen content at the head of the crystal bar comprise crystal rotation and/or crucible rotation adjustment, furnace pressure adjustment, argon flow adjustment, guide cylinder size change and the like.
However, when producing large-diameter silicon single crystal rods of more than 8 inches, once the size of the guide shell is designed and set, the guide shell cannot be easily adjusted. The oxygen content at the head of the crystal bar can be reduced only to a certain extent by adjusting crystal rotation and/or crucible rotation, furnace pressure, argon flow and the like (for example, when 8-inch single crystal silicon crystal bar is produced, the oxygen content can reach about 20ppma optimally), but after the bottle neck is reached, the oxygen content at the head of the crystal bar is difficult to further reduce by changing the above conditions.
In the prior art, the chinese patent No. 201610727739.1 discloses an oxygen reduction process and apparatus for pulling single crystal silicon by MCZ, which shows that when a small-diameter (4 inches) single crystal silicon ingot is produced, the oxygen content in the dissolved silicon can be effectively reduced and the oxygen content at the head of the single crystal silicon can be reduced by stirring after the material melting is completed. However, practice has shown that when producing large diameter single crystal silicon, stirring the silicon melt after melting is completed does not further reduce the oxygen content at the head of the ingot.
Disclosure of Invention
In view of the above, the present invention provides a method and an apparatus for producing large-diameter single crystal silicon, which can reduce the oxygen content at the head of the large-diameter single crystal silicon ingot, so as to solve the technical problem that the oxygen content at the head of the large-diameter single crystal silicon ingot cannot be further reduced during the pulling process.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for producing large-diameter monocrystalline silicon capable of reducing the oxygen content of a head part comprises the following steps:
material melting: melting the silicon material to obtain silicon melt; after the melting is finished, the flow of argon is a, the pressure in a crystal pulling furnace is b, and the rotating speed of a crucible is c;
and (3) oxygen reduction treatment: stirring the silicon melt while increasing the flow of argon gas to 1.5 a-3 a and/or increasing the pressure in the furnace to 1.5 b-3 b.
Preferably, in the step of "oxygen reduction treatment", the stirring direction is opposite to the crucible rotation direction, and the stirring rate is 1c to 3 c.
Preferably, in the step "oxygen reduction treatment", the silicon melt is stirred while increasing the flow of argon gas to 2a and/or increasing the pressure in the furnace to 2 b.
Preferably, in the step "oxygen reduction treatment", the silicon melt is stirred while increasing the flow of argon gas to 2a and increasing the pressure in the furnace to 2 b.
The utility model provides a can reduce major diameter monocrystalline silicon apparatus for producing of head oxygen content, includes the single crystal growing furnace body, sets up seed crystal lifting rotary mechanism and the setting on the single crystal growing furnace body are in the crucible in the single crystal growing furnace body, seed crystal lifting rotary mechanism includes weight and drive weight pivoted rotary drive subassembly, still includes the agitator, the agitator can with the weight can be dismantled and be connected, just the agitator tip can stretch into inside the crucible.
Preferably, the stirrer comprises a connecting shaft, and one end of the connecting shaft is provided with a connecting thread which can be screwed on the lower end of the heavy hammer.
Preferably, the stirrer further comprises at least two high-purity quartz paddles arranged at the lower end of the connecting shaft, and the high-purity quartz paddles are arranged to be arc-shaped surfaces.
Preferably, a clamping groove is formed in the connecting shaft.
Preferably, the height of the high-purity quartz paddle is 1/3-1/2 of the height of the crucible.
Preferably, the blade span of the high-purity quartz paddle is 1/3-1/2 of the radius of the crucible.
According to the technical scheme, the invention provides a method and a device for producing large-diameter monocrystalline silicon capable of reducing the oxygen content in the head, and the method and the device have the beneficial effects that: after melting, adding an oxygen reduction treatment process, stirring the silicon melt soup, and simultaneously increasing the argon flow to 1.5-3 times of the argon flow after melting, and/or increasing the pressure in the crystal pulling furnace to 1.5-3 times of the pressure in the furnace after melting, wherein practical results show that the oxygen content at the head of the monocrystalline silicon crystal rod can be effectively reduced by about 50% by adopting the above means, and the technical bottleneck that the oxygen content at the head of the large-diameter monocrystalline silicon crystal rod cannot be further reduced is effectively broken through.
Drawings
FIG. 1 is a schematic configuration diagram of a large-diameter single-crystal silicon production apparatus capable of reducing the head oxygen content.
FIG. 2 is a schematic view of the structure of the stirrer.
In the figure: the large-diameter monocrystalline silicon production device comprises a large-diameter monocrystalline silicon production device 10 capable of reducing the oxygen content of the head, a crucible 100, a heavy hammer 200, a stirrer 300, a connecting shaft 310, a connecting thread 311 and a high-purity quartz paddle 320.
Detailed Description
The technical solutions and effects of the embodiments of the present invention will be further described in detail below with reference to the accompanying drawings of the present invention.
Referring to fig. 1 and 2, in an embodiment, a large-diameter single crystal silicon production apparatus 10 capable of reducing the oxygen content at the head comprises a single crystal furnace body, a seed crystal lifting and rotating mechanism disposed on the single crystal furnace body, and a crucible 100 disposed in the single crystal furnace body, wherein the seed crystal lifting and rotating mechanism comprises a weight 200 and a rotating driving component for driving the weight 200 to rotate, and further comprises a stirrer 300, the stirrer 300 can be detachably connected with the weight 200, and the end of the stirrer 300 can extend into the crucible 100.
That is to say, the stirrer 300 is prefabricated, so that the stirrer 300 can be detachably connected to the weight 200 of the seed crystal lifting and rotating mechanism, when a large-diameter monocrystalline silicon crystal rod is produced, after melting, the stirrer 300 is connected to the weight 200 and extends into the furnace body of the monocrystalline furnace, the stirring part of the stirrer 300 is immersed below the silicon melt liquid level of the crucible 100, the rotary driving assembly is started to drive the weight 200 to rotate, so that the stirrer 300 completes stirring of the silicon melt, oxygen or oxygen-containing volatile gas phase in the silicon melt is fully separated out, and the oxygen content at the head of the monocrystalline silicon crystal rod is effectively reduced. Preferably, the stirrer 300 rotates the crucible 100 while stirring, and the rotation direction of the crucible 100 is opposite to the stirring direction of the stirrer 300, so as to enhance disturbance of the silicon melt and further reduce the head oxygen content of the single crystal silicon ingot.
Preferably, the oxygen content at the head of the single crystal silicon ingot can be further reduced by adjusting the flow rate of the argon gas and/or adjusting the pressure in the single crystal furnace body while stirring.
In an embodiment, the stirrer 300 includes a connecting shaft 310, and one end of the connecting shaft 310 is provided with a connecting screw 311, and the connecting screw 311 can be screwed to the lower end of the weight 200. For example, one end of the connection shaft 310 is provided with an internal thread to be screwed on the lower end of the weight 200 through the internal thread, so as to drive the stirrer 300 through the rotary driving assembly to stir the silicon melt.
Further, the stirrer 300 further comprises at least two high-purity quartz paddles 320 arranged at the lower end of the connecting shaft 310, wherein the high-purity quartz paddles 320 are arranged in an arc-shaped surface. The high-purity quartz paddle 320 is used for stirring the silicon melt in the crucible 100, so that the introduction of impurities is reduced. The arc-shaped high-purity quartz paddle 320 is beneficial to smooth stirring, so that the silicon melt soup forms convection in the crucible, oxygen in the silicon melt soup is fully volatilized, oxygen is further reduced to enter the crystal bar, and the oxygen content at the head of the monocrystalline silicon crystal bar is reduced.
In one embodiment, the connecting shaft 310 is provided with a slot for connecting the agitator 300 to the weight 200 by using a tool such as a wrench.
In another embodiment, the height of the high-purity quartz paddle 320 is 1/3-1/2 of the height of the crucible, so that on one hand, the high-purity quartz paddle 320 can be ensured to be completely immersed in the silicon melt in the crucible, and on the other hand, the high-purity quartz paddle 320 is prevented from contacting the crucible to cause accidents.
Further, the blade span of the high-purity quartz paddle 320 is 1/3-1/2 of the radius of the crucible. That is, the maximum width of the high purity quartz paddle 320 is 1/3 to 1/2 of the crucible radius, so that the stirring uniformity of the silicon melt is improved, and the contact between the high purity quartz paddle 320 and the crucible is prevented, which causes accidents.
In another embodiment of the present invention, a method for producing large-diameter single-crystal silicon capable of reducing head oxygen content includes the steps of:
s10, melting: melting the silicon material to obtain silicon melt; after the melting is finished, the flow of argon is a, the pressure in a crystal pulling furnace is b, and the rotating speed of a crucible is c;
s20, oxygen reduction treatment: stirring the silicon melt while increasing the flow of argon gas to 1.5 a-3 a and/or increasing the pressure in the furnace to 1.5 b-3 b.
In this embodiment, for example, when a large-diameter silicon single crystal ingot of 8 to 12 inches is pulled, the process steps of feeding, material melting, oxygen reduction, high-temperature treatment, stabilization, doping, seeding, shouldering, shoulder rotation, constant diameter, ending and cooling are performed in sequence, and in the case of the present invention, which is not particularly emphasized, the process steps include conventionally known parameters such as temperature, furnace pressure, crystal rotation, crucible rotation, argon flow and the like, and thus, the detailed description thereof is omitted. If the argon flow is a, the furnace pressure of the crystal pulling furnace is b and the crucible rotating speed is c after the material melting is finished, in the oxygen reduction treatment step, the argon flow is increased to 1.5 a-3 a and/or the furnace pressure is increased to 1.5 b-3 b while stirring. Preferably, the silicon melt is stirred while increasing the argon flow to 2a and/or increasing the pressure in the furnace to 2 b. Preferably, the silicon melt is stirred while increasing the argon flow to 2a and increasing the pressure in the furnace to 2 b.
Further, in the step of "oxygen reduction treatment", the stirring direction is opposite to the crucible rotation direction, and the stirring rate is 1c to 3 c.
The technical scheme and technical effects of the invention are further explained by the specific examples below.
Comparative example 1
A Hanhong FT-CZ2408S2 furnace was used to produce 200mm (8 inches) single crystal silicon ingots.
After the crucible 100 is charged, melting is performed to obtain the silicon melt. The stirrer 300 is installed on the weight 200, extends below the silicon melt level in the crucible 100, keeps the single crystal furnace body sealed, and is filled with argon gas, the argon gas flow is kept at 50 SLM, the pressure in the single crystal furnace body is kept at 8 Kpa, the crucible rotation speed is kept at 2 r/s, and the oxygen reduction treatment is carried out after 1 h. After the oxygen reduction treatment is finished, the conventional production mode, high-temperature treatment, stabilization, doping, seeding, shouldering, shoulder rotating, isometric diameter, ending and cooling process steps are sequentially installed to obtain the 8-inch large-diameter monocrystalline silicon crystal rod, the distribution condition of the oxygen content of the monocrystalline silicon crystal rod is detected by adopting an LECO method through a GFA method, and the detection result is shown in Table 1.
Comparative examples No. two to No. five
Referring to the first comparative example, the oxygen content distribution of the obtained single crystal silicon ingot was measured by gradually increasing the flow rate of argon while maintaining the other process conditions, and taking 75 SLM, 100 SLM, 125 SLM, and 150 SLM as argon flow rates, and the measurement results are shown in table 1.
TABLE 1 comparative examples one to five monocrystalline silicon rods oxygen content distribution test data
Comparative examples six to nine
Referring to the first comparative example, the internal pressure of the single crystal furnace was gradually increased while keeping the other process conditions constant, and the internal pressures were set to 12 Kpa, 16 Kpa, 20 Kpa, and 24 Kpa, respectively, and the oxygen content distribution of the obtained single crystal silicon ingot was measured, and the results of the measurements are shown in table 2.
Comparative example ten
Referring to the first comparative example, the distribution of oxygen content in the obtained single crystal silicon ingot was measured with the flow of argon gas being 100 SLM and the pressure in the furnace being 16 Kpa, and the results of the measurements are shown in table 2.
TABLE 2 comparative examples six to nine comparative examples oxygen content distribution test numbers of single crystal silicon rods
As can be seen from tables 1 and 2, after the production is stabilized, the influence on the oxygen content of the head of the monocrystalline silicon ingot is limited by increasing the flow of argon and/or by increasing the pressure in the monocrystalline furnace.
Experimental examples one to three
Referring to the first comparative example, other process conditions were kept unchanged, stirring was started during the oxygen reduction treatment, the stirring speed was adjusted to 2 r/s, 4 r/s, and 6r/s, respectively, and the oxygen content distribution of the obtained single crystal silicon ingot was examined, and the examination results are shown in table 3.
Table 3 experimental examples one to three-single crystal silicon ingot oxygen content distribution measurement data
As can be seen from table 3, only by stirring the silicon melt soup or changing the stirring rate, there is a limited effect on the head oxygen content of the single crystal silicon ingot.
Experimental examples four to seven
Referring to the second experimental example, other process conditions were kept unchanged, stirring was started during the oxygen reduction treatment, the stirring speed was adjusted to 4 r/s, the argon flow was 75 SLM, 100 SLM, 125 SLM, and 150 SLM, respectively, and the obtained distribution of the oxygen content of the single crystal silicon ingot was measured, and the measurement results are shown in table 4.
Table 4 experimental example four to experimental example seven single crystal silicon ingot oxygen content distribution measurement data
As can be seen from tables 1, 3, and 4, while stirring the silicon melt, the flow of argon gas is increased to 1.5 to 3 times of the flow of argon gas after the melting is completed, so that the head oxygen content of 8 inches of silicon single crystal ingot can be effectively reduced, and the head oxygen content of 8 inches of silicon single crystal ingot is reduced by about 35%. Meanwhile, as can be seen from table 4, the oxygen content at the head of the 8 inch single crystal silicon ingot tends to be further reduced with the increase of the argon gas flow, but when the argon gas flow reaches more than 2 times of the argon gas flow after the material melting is finished, the oxygen content at the head of the 8 inch single crystal silicon ingot tends to be stable, and a new bottleneck is reached.
Experimental examples eight to eleven
Referring to the second experimental example, while maintaining the other process conditions, stirring was started at the time of the oxygen reduction treatment, the stirring rotation speed was adjusted to 4 r/s, the furnace pressures were set to 12 Kpa, 16 Kpa, 20 Kpa, and 24 Kpa, respectively, and the oxygen content distribution of the obtained single crystal silicon ingot was measured, and the measurement results are shown in table 5.
Table 5 experimental examples eight to eleven experimental examples silicon single crystal ingot oxygen content distribution measurement data
As can be seen from tables 1, 3, and 4, while stirring the silicon melt, the pressure in the single crystal furnace is increased to 1.5 to 3 times of the pressure in the furnace after the melting is completed, so that the head oxygen content of the 8 inch single crystal silicon ingot can be effectively reduced, and the head oxygen content of the 8 inch single crystal silicon ingot is reduced by about 40%. Meanwhile, as can be seen from table 5, when the argon flow reaches 2 times or more of the argon flow after the melting is finished, the oxygen content of the head of the 8-inch single crystal silicon ingot approaches to be stable, and a new bottleneck is reached.
Experimental examples twelve to fourteen
Referring to the first comparative example, the other process conditions were kept unchanged, and during the oxygen reduction treatment, the flow rate of argon was taken as 100 SLM, the pressure in the furnace was taken as 16 Kpa, stirring was started, the stirring rotation speed was adjusted to 2 r/s, 4 r/s, and 6r/s, respectively, and the oxygen content distribution of the obtained single crystal silicon ingot was measured, and the measurement results are shown in Table 6.
Table 6 experimental examples twelve to fourteen single crystal silicon rods oxygen content distribution detection data
As can be seen from tables 4, 5, and 6, when the silicon melt is stirred, the argon flow is increased, the pressure in the single crystal furnace is increased, which is beneficial to further reducing the oxygen content at the head of the 8-inch single crystal silicon ingot, and compared with the method that when the silicon melt is stirred, the argon flow is increased or the pressure in the single crystal furnace is increased, which is reduced by about 10%. Meanwhile, as can be seen from table 6, further increase in stirring speed has limited effect on reducing the head oxygen content of 8 inch single crystal silicon rods.
It is worth noting that the method for reducing the head oxygen content of the monocrystalline silicon crystal rod provided by the embodiment of the invention is not only suitable for the production of 8 inches (200 mm) monocrystalline silicon crystal rods, but also can meet the drawing requirement of larger diameter (such as 12 inches, 300 mm) monocrystalline silicon crystal rods.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A method for producing large-diameter monocrystalline silicon capable of reducing the oxygen content of a head part is characterized by comprising the following steps:
material melting: melting the silicon material to obtain silicon melt; after the melting is finished, the flow of argon is a, the pressure in a crystal pulling furnace is b, and the rotating speed of a crucible is c;
and (3) oxygen reduction treatment: stirring the silicon melt while increasing the flow of argon gas to 1.5 a-3 a and/or increasing the pressure in the furnace to 1.5 b-3 b.
2. The method for producing large-diameter single-crystal silicon capable of reducing the head oxygen content as claimed in claim 1, wherein in the step "oxygen reduction treatment", the stirring direction is opposite to the crucible rotation direction, and the stirring rate is 1c to 3 c.
3. The method for producing large-diameter single-crystal silicon capable of reducing the head oxygen content as claimed in claim 1, wherein in the step "oxygen reduction treatment", the silicon melt is stirred while increasing the argon gas flow to 2a and/or increasing the pressure in the furnace to 2 b.
4. The method for producing large-diameter single-crystal silicon capable of reducing the head oxygen content as claimed in claim 3, wherein in the step "oxygen reduction treatment", the silicon melt is stirred while increasing the argon gas flow to 2a and increasing the pressure in the furnace to 2 b.
5. The utility model provides a can reduce major diameter monocrystalline silicon apparatus for producing of head oxygen content, includes the monocrystalline furnace body, sets up seed crystal lifting rotary mechanism on the monocrystalline furnace body and sets up the crucible in the monocrystalline furnace body, seed crystal lifting rotary mechanism includes the weight and drives weight pivoted rotary drive subassembly, its characterized in that still includes the agitator, the agitator can with the weight can be dismantled and be connected, just the agitator tip can stretch into inside the crucible.
6. The apparatus for producing a large-diameter single-crystal silicon capable of reducing the head oxygen content as claimed in claim 5, wherein said agitator includes a connecting shaft, one end of said connecting shaft is provided with a connecting screw thread capable of being screwed to the lower end of said weight.
7. The large-diameter single-crystal silicon production apparatus capable of reducing the head oxygen content as claimed in claim 6, wherein said agitator further comprises at least two high-purity quartz paddles disposed at a lower end of said connecting shaft, said high-purity quartz paddles being disposed in an arc-shaped plane.
8. The large-diameter single-crystal silicon production apparatus capable of reducing the head oxygen content as claimed in claim 6, wherein a notch is provided on said connection shaft.
9. The production apparatus for large-diameter single-crystal silicon capable of reducing the head oxygen content as claimed in claim 7, wherein the height of said high-purity quartz paddle is 1/3-1/2 of the crucible height.
10. The production apparatus for large-diameter single-crystal silicon capable of reducing the head oxygen content as claimed in claim 7, wherein the blade span of the high-purity quartz paddle is 1/3-1/2 of the crucible radius.
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| CN116084008A (en) * | 2023-04-10 | 2023-05-09 | 苏州晨晖智能设备有限公司 | Oxygen reduction protection device for pulling monocrystalline silicon |
| WO2023221576A1 (en) * | 2022-05-20 | 2023-11-23 | 隆基绿能科技股份有限公司 | Oxygen content control method and apparatus, and electronic device and storage medium |
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