CN117187938A - Preparation method of large-size high-quality n-type monocrystalline silicon wafer - Google Patents
Preparation method of large-size high-quality n-type monocrystalline silicon wafer Download PDFInfo
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- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 66
- 239000010703 silicon Substances 0.000 claims abstract description 66
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 238000004140 cleaning Methods 0.000 claims abstract description 21
- 238000010899 nucleation Methods 0.000 claims abstract description 18
- 238000005520 cutting process Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002844 melting Methods 0.000 claims abstract description 3
- 230000008018 melting Effects 0.000 claims abstract description 3
- 239000013078 crystal Substances 0.000 claims description 93
- 235000012431 wafers Nutrition 0.000 claims description 72
- 238000000034 method Methods 0.000 claims description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- 239000010453 quartz Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 5
- 230000007246 mechanism Effects 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 230000007547 defect Effects 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 2
- 230000008901 benefit Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 229910021419 crystalline silicon Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention provides a preparation method of a large-size high-quality n-type monocrystalline silicon wafer, and relates to the technical field of large-size silicon wafer processing. The preparation method mainly comprises the following steps: designing a heater and a water cooling screen in a furnace body, heating and melting, seeding, quickly pulling and reducing the diameter, slowly pulling and cooling to put the shoulder, growing with equal diameter, quickly pulling and heating to finish, cutting and cleaning, and the like. The invention overcomes the defects of the prior art, improves the uniformity of resistivity in the production of the silicon wafer, prolongs the minority carrier lifetime, and comprehensively improves the quality of the large-size n-type monocrystalline silicon wafer.
Description
Technical Field
The invention relates to the technical field of large-size silicon wafer processing, in particular to a preparation method of a large-size high-quality n-type monocrystalline silicon wafer.
Background
The photovoltaic power generation plays an increasingly important role in new energy resource transformation in China by virtue of the advantages of cleanness, safety, abundant resources and the like, and provides a powerful engine for realizing carbon peak and carbon neutralization in China. Crystalline silicon batteries are always dominant products in the photovoltaic market by virtue of mature preparation technology, higher photoelectric conversion efficiency and low cost. Compared with the boron-doped p-type crystalline silicon battery, the phosphorus-doped n-type battery has become a research hot spot in the photovoltaic industry due to the advantages of high battery efficiency, strong attenuation resistance and strong defect tolerance.
In the silicon wafer segment, in order to achieve high conversion efficiency, czochralski single crystal silicon is widely used because of its long minority carrier lifetime. The silicon wafer size has been rapidly developed in recent years, from early 100mm and 125mm, to the 210mm large silicon wafer which is mainstream nowadays. On one hand, the large-size silicon wafer can reduce the unit crystal growth cost at the silicon wafer end, and on the other hand, the Bao Shanwa non-silicon cost can be saved in the battery, the component and the system ring, so that the large-size silicon wafer has obvious economic benefit.
In conclusion, the n-type crystalline silicon battery and the large-size monocrystalline silicon wafer have remarkable advantages in terms of cost reduction and efficiency enhancement of the photovoltaic industry, research is conducted on the n-type large-size high-quality monocrystalline silicon growth technology and equipment thereof, autonomous innovation capability and core competitiveness of the photovoltaic industry in a silicon wafer manufacturing link are improved, technical progress of the industry is led, and driving force is provided for economic development.
The novel process and the matched equipment improvement technology of large charging, high pulling speed, repeated pulling and the like are benefited by a series of technical innovations of domestic photovoltaic silicon wafer manufacturing enterprises, and the pulling cost is greatly reduced due to the introduction of new materials and an automatic control system, so that the photovoltaic silicon wafer manufacturing in China is in a global leading position.
According to the yield caliber, the sum of the silicon wafer market share of the national long-base green energy and the TCL ring exceeds 50%, and the double-oligopolistic pattern is stable. The tap industry has increased in pace with increased production beyond 2020. It was expected that in 2022, the hump-base green could form a monocrystalline silicon wafer productivity 130GW, and the tcl ring formed a monocrystalline silicon wafer productivity 140GW. The wafer productivity of 50GW and 43GW are respectively formed by the energy source of the crystal division industry and the crystal Australian science and technology of the vertical integrated manufacturer in 2022. With the release of new productivity and the rapid iteration of large-size products, the industry trend of strong and constant intensity is more remarkable.
Along with the remarkable cost advantages of the large-size silicon wafer in each link, the silicon wafer manufacturers in China have successively improved the yield ratio of the large-size silicon wafer. Since the third quarter of 2021, most silicon manufacturers have begun to dominate large silicon wafer production. The silicon wafers of 210mm and 210mm have been expected to expand to 75% in recent years by the China photovoltaic society. But the production of large-size monocrystalline silicon wafers is difficult to ensure the consistency of the quality of monocrystalline silicon, and the minority carrier lifetime is lower, which brings a certain trouble to practical production and application.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the preparation method of the large-size high-quality n-type monocrystalline silicon wafer, which improves the uniformity of resistivity in the production of the silicon wafer, prolongs the minority carrier lifetime and comprehensively improves the quality of the large-size n-type monocrystalline silicon wafer.
In order to achieve the above object, the technical scheme of the present invention is realized by the following technical scheme:
the preparation method of the large-size high-quality n-type monocrystalline silicon wafer comprises the following steps:
(1) Designing a furnace body: the heating mechanism in the single crystal furnace is a cylindrical graphite heater with a hole at the lower end, the height of a quartz crucible is 700+/-50 mm, the diameter of the crucible is 1200+/-100 mm, the upper end of a water cooling screen is cylindrical, and the lower end of the water cooling screen is funnel-shaped;
(2) Heating and melting: putting the high-purity polycrystalline silicon raw material into a quartz crucible in a single crystal furnace, and heating until the high-purity polycrystalline silicon raw material is completely melted under the conditions of vacuumizing and gas protection to obtain a silicon melt;
(3) Seeding: slowly immersing seed crystal into the surface of the silicon melt after the temperature in the furnace is stable, and seeding;
(4) Reducing: after seeding is completed, the crystal is quickly pulled upwards, the diameter of the crystal is reduced, and the diameter is reduced;
(5) Shoulder placing: after the diameter reduction is completed, the pulling speed and the heating temperature are reduced, so that the diameter of the monocrystalline silicon is gradually increased to the target diameter, and shoulder placing is carried out;
(6) And (3) equal-diameter growth: after the diameter of the crystal reaches the target diameter, adjusting the power and the pulling speed of the heater to perform equal diameter growth;
(7) Ending: when the crystal growth is finished, the crystal pulling speed and the heating temperature are increased, so that the crystal diameter is continuously reduced, the crystal leaves the surface of the melt, ending is finished, the crystal is cooled to the room temperature, and the crystal is taken out after the furnace is opened;
(8) Cutting: and cutting the taken crystal into large-size silicon wafers by a wire cutting machine, removing saw marks and damages generated during cutting the silicon wafers, and cleaning to obtain large-size high-quality n-type monocrystalline silicon wafers.
Preferably, in the step (1), vacuum is drawn to 0.01Pa, and argon is used for protection.
Preferably, the crystal orientation of the seed crystal in the step (2) is <100>.
Preferably, the temperature in the furnace in the step (3) is stabilized at 1500 ℃.
Preferably, the speed of pulling up the crystals rapidly in the step (4) is 200-250mm/h.
Preferably, the pulling speed is reduced to 60-80mm/h in step (5), and the heating temperature is reduced to 1400-1450 ℃.
Preferably, the change of the diameter of the control crystal in the step (6) during the equal diameter growth is kept within a range of +/-2 mm.
Preferably, the pulling rate is increased to 200-250mm/h in step (7), and the heating temperature is increased to 1500-1550 ℃.
Preferably, the method for removing saw marks and damages generated during cutting the silicon wafer in the step (8) is to grind the silicon wafer on a grinder.
Preferably, the cleaning mode in the step (8) is cleaning by adopting a cleaning liquid, and the cleaning liquid is prepared from the following components in proportion: NH (NH) 4 OH∶H 2 O 2 ∶H 2 O＝1∶1∶5。
The invention provides a preparation method of a large-size high-quality n-type monocrystalline silicon piece, which has the advantages that compared with the prior art:
(1) The cylindrical graphite heater with the bottom open hole and the cooling screen with the funnel-shaped lower end of the upper end barrel are arranged, the radiation area of the cylindrical graphite heater is large, the heating effect is good, the temperature gradient between the cylindrical graphite heater and the crucible is small, the heat convection in the crucible can be effectively reduced, the heating uniformity is improved, the cooling uniformity and the cooling stability can be improved due to the arrangement of the cooling screen, a high-stability thermal field for preparing large-size monocrystalline silicon is comprehensively provided, the quality of the large-size monocrystalline silicon is improved, the instability of the quality of the monocrystalline silicon among the secondary is reduced, the yield of the monocrystalline silicon prepared in the whole life cycle of the monocrystalline furnace is improved, and meanwhile, the size of the quartz crucible is controlled to ensure that the large-size monocrystalline silicon can be produced.
(2) According to the invention, through optimizing the parameter process of Czochralski crystal growth, adopting multi-parameter target optimization, pulling and shrinking the diameter through the early stage of high Wen Kuaisu, then reducing the temperature and reducing the speed to carry out shouldering, then carrying out constant diameter growth, finally carrying out high-speed pulling and ending, and optimizing each parameter to improve the stability and uniformity of radial resistivity, ensure the service life of minority carriers, further reduce the oxygen content of the head of a monocrystal, and comprehensively improve the quality of a 210mm large-size monocrystalline silicon wafer.
Description of the drawings:
FIG. 1 is a schematic view of the structure of the single crystal furnace in example 1;
FIG. 2 is a flow chart of the design and research of the present invention.
In the figure: 1. a single crystal furnace; 2. a quartz crucible; 3. a graphite heater; 4. and (5) cooling the screen.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
1. design of single crystal furnace, refer to fig. 1: the heating mechanism in the single crystal furnace 1 is a cylindrical graphite heater 3 with a hole at the lower end, the height of the quartz crucible 2 is 700mm, the diameter of the quartz crucible 2 is 1200mm, the upper end of the water cooling screen 4 is cylindrical, the lower end of the water cooling screen is funnel-shaped, and the quartz crucible 2 is entirely arranged in the graphite heater 3;
2. preparing cleaning liquid: NH is added to 4 OH、H 2 O 2 、H 2 O is mixed according to the mass ratio of 1:1:5, and the cleaning liquid is obtained.
Example 2:
production of 210mm large-size monocrystalline silicon piece (monocrystalline furnace designed with the above example 1):
(1) 500kg of high-purity polycrystalline silicon raw material is placed in a crucible, vacuumized to 0.01Pa, and argon is introduced into the furnace for protection, and then a graphite heater is started to enable the raw material in the crucible to be completely melted, so that a silicon melt is obtained.
(2) Slowly immersing a seed crystal with the crystal orientation of <100> into the surface of a silicon melt by adopting a pulling device when the temperature in the furnace is stabilized at 1500 ℃, seeding, controlling the seeding speed to be 80mm/h, controlling the crystal diameter to be 8mm and controlling the crystal length to be 280mm;
(3) After seeding is completed, the crystal is quickly pulled up at the speed of 250mm/h, the diameter of the crystal is reduced to 6mm, and the diameter is reduced;
(4) After diameter reduction is completed, the pulling speed is reduced to 80mm/h, the heating temperature is reduced to 1450 ℃, the diameter of the monocrystalline silicon is gradually increased to 280mm of the target diameter, and shoulder placing is carried out;
(5) After shouldering, carrying out equal diameter growth, and controlling the temperature and the stretching speed to ensure that the diameter of the crystal is maintained within the range of 280mm plus or minus 2 mm;
(6) After the isodiametric growth is completed, a final stage is carried out, the crystal pulling speed is increased to 250mm/h, the heating temperature is increased to 1550 ℃, the crystal diameter is continuously reduced, the crystal leaves the surface of the melt, the final stage is completed, the crystal is cooled to room temperature, and the crystal is taken out after the furnace is opened;
(7) After the crystal was taken out, a wire-cut machine (a silicon wafer of 4mm thickness was cut longitudinally and transversely along a single crystal silicon rod, and cleaved into a square silicon wafer and a round silicon wafer, respectively; the silicon wafer was ground on a grinder to remove saw marks and damages generated during cutting, and the cleaning solution in example 1 was used for cleaning to remove organic matters, particles and metal ions on the surface of the silicon wafer.
Example 2:
production of 210mm large-size monocrystalline silicon piece (monocrystalline furnace designed with the above example 1):
(1) 500kg of high-purity polycrystalline silicon raw material is placed in a crucible, vacuumized to 0.01Pa, and argon is introduced into the furnace for protection, and then a graphite heater is started to enable the raw material in the crucible to be completely melted, so that a silicon melt is obtained.
(2) Slowly immersing a seed crystal with the crystal orientation of <100> into the surface of a silicon melt by adopting a pulling device when the temperature in the furnace is stabilized at 1500 ℃, seeding, controlling the seeding speed to be 80mm/h, controlling the crystal diameter to be 8mm and controlling the crystal length to be 280mm;
(3) After seeding is completed, the crystal is quickly pulled up at the speed of 200mm/h, the diameter of the crystal is reduced to 6mm, and the diameter is reduced;
(4) Reducing the pulling speed to 60mm/h after diameter reduction is completed, reducing the heating temperature to 1400 ℃, gradually increasing the diameter of monocrystalline silicon to 280mm of the target diameter, and shouldering;
(5) After shouldering, carrying out equal diameter growth, and controlling the temperature and the stretching speed to ensure that the diameter of the crystal is maintained within the range of 280mm plus or minus 2 mm;
(6) After the isodiametric growth is completed, the crystal enters a finishing stage, the crystal pulling speed is increased to 200mm/h, the heating temperature is increased to 1500 ℃, the crystal diameter is continuously reduced, the crystal leaves the surface of the melt, finishing the finishing is completed, the crystal is cooled to room temperature, and the crystal is taken out after opening the furnace;
(7) After the crystal was taken out, a wire-cut machine (a silicon wafer of 4mm thickness was cut longitudinally and transversely along a single crystal silicon rod, and cleaved into a square silicon wafer and a round silicon wafer, respectively; the silicon wafer was ground on a grinder to remove saw marks and damages generated during cutting, and the cleaning solution in example 1 was used for cleaning to remove organic matters, particles and metal ions on the surface of the silicon wafer.
Comparative example 1:
production of 210mm large-size monocrystalline silicon piece (monocrystalline furnace designed with the above example 1):
(1) 500kg of high-purity polycrystalline silicon raw material is placed in a crucible, vacuumized to 0.01Pa, and argon is introduced into the furnace for protection, and then a graphite heater is started to enable the raw material in the crucible to be completely melted, so that a silicon melt is obtained.
(2) Slowly immersing a seed crystal with the crystal orientation of <100> into the surface of a silicon melt by adopting a pulling device when the temperature in the furnace is stabilized at 1500 ℃, seeding, controlling the seeding speed to be 80mm/h, controlling the crystal diameter to be 8mm and controlling the crystal length to be 280mm;
(3) Reducing the pulling speed to 60mm/h, reducing the heating temperature to 1400 ℃, gradually increasing the diameter of monocrystalline silicon to 280mm of the target diameter, and shouldering;
(4) After shouldering, carrying out equal diameter growth, and controlling the temperature and the stretching speed to ensure that the diameter of the crystal is maintained within the range of 280mm plus or minus 2 mm;
(5) After the isodiametric growth is completed, the crystal enters a finishing stage, the crystal pulling speed is increased to 200mm/h, the heating temperature is increased to 1500 ℃, the crystal diameter is continuously reduced, the crystal leaves the surface of the melt, finishing the finishing is completed, the crystal is cooled to room temperature, and the crystal is taken out after opening the furnace;
(6) After the crystal was taken out, a wire-cut machine (a silicon wafer of 4mm thickness was cut longitudinally and transversely along a single crystal silicon rod, and cleaved into a square silicon wafer and a round silicon wafer, respectively; the silicon wafer was ground on a grinder to remove saw marks and damages generated during cutting, and the cleaning solution in example 1 was used for cleaning to remove organic matters, particles and metal ions on the surface of the silicon wafer.
Comparative example 2:
production of 210mm large-size monocrystalline silicon piece (monocrystalline furnace designed with the above example 1):
(1) 500kg of high-purity polycrystalline silicon raw material is placed in a crucible, vacuumized to 0.01Pa, and argon is introduced into the furnace for protection, and then a graphite heater is started to enable the raw material in the crucible to be completely melted, so that a silicon melt is obtained.
(3) Slowly immersing a seed crystal with the crystal orientation of <100> into the surface of the silicon melt by adopting a pulling device after the temperature of the silicon melt is stabilized at 1450 ℃, seeding, controlling the seeding speed to be 250mm/h, controlling the crystal diameter to be 8mm and controlling the crystal length to be 280mm;
(4) After seeding is finished, starting to put a shoulder, reducing the pulling speed to 80mm/h, keeping the temperature unchanged, and gradually increasing the diameter of the crystal to 280mm;
(5) After shouldering, carrying out equal diameter growth, and controlling the temperature and the stretching speed to ensure that the diameter of the crystal is maintained within the range of 280mm plus or minus 2 mm;
(6) After the isodiametric growth is completed, the crystal enters a finishing stage, the lifting speed of the crystal is controlled to be 80mm/h, the diameter of the crystal is continuously reduced, the crystal leaves the surface of the melt, finishing the finishing, cooling to room temperature, and opening a furnace to take out the crystal;
(7) After the crystal was taken out, a wire-cut machine (a silicon wafer of 4mm thickness was cut longitudinally and transversely along a single crystal silicon rod, and cleaved into a square silicon wafer and a round silicon wafer, respectively; the silicon wafer was ground on a grinder to remove saw marks and damages generated during cutting, and the cleaning solution in example 1 was used for cleaning to remove organic matters, particles and metal ions on the surface of the silicon wafer.
And (3) detection:
for the large-size silicon wafers of 210mm prepared in the above examples 1-2 and comparative examples 1-2, oxygen impurity distribution in the silicon wafer was measured by using a fourier transform infrared spectrometer, resistivity distribution of the silicon wafer was measured by using a four-probe resistivity meter, minority carrier lifetime of the silicon wafer was measured by using a minority carrier lifetime tester, and specific results are shown in the following table:
as can be seen from the above table, the large-size single crystal silicon prepared in examples 1-2 has higher stability and higher minority carrier lifetime, and comprehensively improves the quality of the large-size single crystal silicon.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the large-size high-quality n-type monocrystalline silicon wafer is characterized by comprising the following steps of:
(1) Designing a furnace body: the heating mechanism in the single crystal furnace is a cylindrical graphite heater with a hole at the lower end, the height of a quartz crucible is 700+/-50 mm, the diameter of the crucible is 1200+/-100 mm, the upper end of a water cooling screen is cylindrical, and the lower end of the water cooling screen is funnel-shaped;
(2) Heating and melting: putting the high-purity polycrystalline silicon raw material into a quartz crucible in a single crystal furnace, and heating until the high-purity polycrystalline silicon raw material is completely melted under the conditions of vacuumizing and gas protection to obtain a silicon melt;
(3) Seeding: slowly immersing seed crystal into the surface of the silicon melt after the temperature in the furnace is stable, and seeding;
(4) Reducing: after seeding is completed, the crystal is quickly pulled upwards, the diameter of the crystal is reduced, and the diameter is reduced;
(5) Shoulder placing: after the diameter reduction is completed, the pulling speed and the heating temperature are reduced, so that the diameter of the monocrystalline silicon is gradually increased to the target diameter, and shoulder placing is carried out;
(6) And (3) equal-diameter growth: after the diameter of the crystal reaches the target diameter, adjusting the power and the pulling speed of the heater to perform equal diameter growth;
(7) Ending: when the crystal growth is finished, the crystal pulling speed and the heating temperature are increased, so that the crystal diameter is continuously reduced, the crystal leaves the surface of the melt, ending is finished, the crystal is cooled to the room temperature, and the crystal is taken out after the furnace is opened;
(8) Cutting: and cutting the taken crystal into large-size silicon wafers by a wire cutting machine, removing saw marks and damages generated during cutting the silicon wafers, and cleaning to obtain large-size high-quality n-type monocrystalline silicon wafers.
2. The method for preparing the large-size high-quality n-type monocrystalline silicon wafer according to claim 1, wherein the method comprises the following steps: and (3) vacuumizing to 0.01Pa in the step (2), and protecting by adopting argon.
3. The method for preparing the large-size high-quality n-type monocrystalline silicon wafer according to claim 1, wherein the method comprises the following steps: the crystal orientation of the seed crystal in the step (3) is <100>.
4. The method for preparing the large-size high-quality n-type monocrystalline silicon wafer according to claim 1, wherein the method comprises the following steps: in the step (3), the temperature in the furnace is stabilized at 1500 ℃.
5. The method for preparing the large-size high-quality n-type monocrystalline silicon wafer according to claim 1, wherein the method comprises the following steps: the speed of pulling up the crystal rapidly in the step (4) is 200-250mm/h.
6. The method for preparing the large-size high-quality n-type monocrystalline silicon wafer according to claim 1, wherein the method comprises the following steps: and (3) reducing the lifting speed to 60-80mm/h in the step (5), and reducing the heating temperature to 1400-1450 ℃.
7. The method for preparing the large-size high-quality n-type monocrystalline silicon wafer according to claim 1, wherein the method comprises the following steps: and (3) controlling the change of the crystal diameter in the equal diameter growth process in the step (6) to be within +/-2 mm.
8. The method for preparing the large-size high-quality n-type monocrystalline silicon wafer according to claim 1, wherein the method comprises the following steps: in the step (7), the pulling speed is increased to 200-250mm/h, and the heating temperature is increased to 1500-1550 ℃.
9. The method for preparing the large-size high-quality n-type monocrystalline silicon wafer according to claim 1, wherein the method comprises the following steps: the method for removing saw marks and damages generated during the cutting of the silicon wafer in the step (8) is to grind the silicon wafer on a grinder.
10. Root of Chinese characterThe method for preparing a large-size high-quality n-type monocrystalline silicon wafer according to claim 1, characterized by: the cleaning mode in the step (8) is cleaning by adopting a cleaning liquid, and the cleaning liquid is prepared from the following components in proportion: NH (NH) 4 OH∶H 2 O 2 ∶H 2 O＝1∶1∶5。
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| CN116065229A (en) * | 2023-02-06 | 2023-05-05 | 四川晶科能源有限公司 | Drawing method of purification rod |
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| CN110983429A (en) * | 2019-12-23 | 2020-04-10 | 西安奕斯伟硅片技术有限公司 | Single crystal furnace and monocrystalline silicon preparation method |
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| CN115652426A (en) * | 2022-08-31 | 2023-01-31 | 包头美科硅能源有限公司 | Drawing method for reducing fragmentation rate of large-size N-type straight-pulled monocrystalline silicon wafer |
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