CN117305987B - Method for eliminating bubble wrapping in liquid phase method silicon carbide crystal growth process - Google Patents
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- 239000013078 crystal Substances 0.000 title claims abstract description 186
- 238000000034 method Methods 0.000 title claims abstract description 55
- 230000008569 process Effects 0.000 title claims abstract description 30
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 26
- 239000007791 liquid phase Substances 0.000 title claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 28
- 239000010439 graphite Substances 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 238000002844 melting Methods 0.000 claims abstract description 19
- 230000008018 melting Effects 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000000956 alloy Substances 0.000 claims description 33
- 229910045601 alloy Inorganic materials 0.000 claims description 33
- 239000007788 liquid Substances 0.000 claims description 7
- 230000001133 acceleration Effects 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims description 2
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 2
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- 239000004065 semiconductor Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 238000005275 alloying Methods 0.000 description 4
- 230000006698 induction Effects 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000006184 cosolvent Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
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- 238000005086 pumping Methods 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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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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Abstract
The invention relates to the technical field of semiconductor materials, in particular to a method for eliminating bubble wrapping in a liquid phase silicon carbide crystal growth process. The crystal growth device is used for supporting the crystal growth and comprises a furnace body, a graphite crucible for Cheng Fangchang crystal raw materials is arranged in the furnace body, a seed rod is arranged above the graphite crucible, a seed holder is arranged at one end of the seed rod, a silicon carbide seed crystal is arranged on the seed holder, a heating device is used for providing the temperature required by crystal growth, and a vacuumizing device is used for providing the vacuum environment required by crystal growth; the method for eliminating the bubble wrapping comprises the following steps: charging a, melting b, remelting c, lifting d, rotating e, remelting f, growing g crystals, and cooling after the growth of the crystals is completed, and taking down the crystals after cooling to complete the crystal growth. The method provided by the invention eliminates bubbles on the surface of the seed crystal in the crystal growth process, so that the surface of the seed crystal is smooth, and high-quality silicon carbide crystals can be grown.
Description
Technical Field
The invention relates to the technical field of semiconductor materials, in particular to a method for eliminating bubble wrapping in a liquid phase silicon carbide crystal growth process.
Background
Silicon carbide (SiC) is a representative third-generation wide-bandgap semiconductor material, and has wide application prospects in the fields of new energy automobiles, energy storage and the like. Physical Vapor Transport (PVT) is a common method for growing SiC crystals, and Top Seed Solution (TSSG) is receiving attention because of the advantages of easy expanding diameter, low defect density, and the like. The TSSG method is generally carried out by placing a Si raw material and a cosolvent into a graphite crucible, and melting the Si raw material and the cosolvent to form a solution by induction heating or resistance heating. The carbon element in the graphite crucible gradually dissolves in the solution and approaches a saturation concentration. The solution at the seed crystal has low temperature and is in a solute supersaturation state, so that SiC is gradually precipitated and grown on the seed crystal.
In the prior art, seed crystal remelting technology is required for liquid phase growth of silicon carbide. In the process of melting raw materials, a seed crystal is placed above the raw materials (in order to ensure the uniformity of a temperature field, the seed crystal rotates slowly), after the raw materials are completely melted, the seed crystal is lowered to be in contact with a solution, and is inserted into the solution to a certain depth for seed crystal remelting, so that volatile matters adhered to the surface of the seed crystal in the process of processing damage and temperature rising are eliminated. In the process, as the seed crystal is uneven, bubbles are easily wrapped in the process of contacting the seed crystal with the solution, small bubbles gather on the surface of the seed crystal, and large bubbles penetrate through the whole crystal, so that the quality of the crystal is seriously affected.
Disclosure of Invention
The invention aims to provide a method for eliminating bubble wrapping in the liquid phase silicon carbide crystal growth process so as to improve the growth quality of silicon carbide crystals.
To achieve the purpose, the invention adopts the following technical scheme:
the method for eliminating bubble wrapping in the liquid phase silicon carbide crystal growing process is characterized in that crystal growing is supported on a crystal growing device, and the crystal growing device comprises a furnace body;
a graphite crucible for Cheng Fangchang crystal raw materials is arranged in the furnace body;
a seed rod is arranged above the graphite crucible;
the seed crystal support is arranged at one end of the seed crystal rod, and a silicon carbide seed crystal is arranged on the seed crystal support;
heating means for providing a temperature required for crystal growth;
the vacuumizing device is used for providing a vacuum environment required by crystal growth;
the method for eliminating the bubble wrapping comprises the following steps:
a, charging: uniformly mixing the crystal growth raw materials, and then placing the mixture in a graphite crucible;
b, material melting: heating the crystal growth raw material to 1600-2100 ℃ to melt the raw material and form an alloy solution;
c, remelting: lowering the seed rod to make the seed crystal immersed in the alloy solution for back melting;
d, lifting: raising the seed rod to separate the seed crystal from the alloy solution;
and e, rotating: rotating the seed rod, and throwing out bubbles in the seed crystal to wrap the seed crystal;
and f, remelting: lowering the seed rod to make the seed crystal immersed in the alloy solution for re-melting;
and g, growing: lifting and rotating the seed rod, and rotating the graphite crucible to perform crystal pulling growth;
and h, after the crystal growth is completed, lifting the seed rod, enabling the lower surface of the crystal to leave the alloy solution, cooling, and taking down the crystal after cooling to complete crystal growth.
Further, in the material melting process in the step b, the distance between the seed crystal and the liquid level of the alloy solution is more than 50mm.
Further, the seed rod rotation is not carried out in the step c remelting process and the step f remelting process;
no graphite crucible rotation was performed.
Further, in the pulling process of the step d, the pulling speed is 5000-6000mm/h;
and lifting the seed crystal until the seed crystal is separated from the alloy liquid level.
Further, during the rotation of the step e, the rotation comprises clockwise rotation, anticlockwise rotation and clockwise and anticlockwise rotation alternately.
Further, the rotating speed of the rotation is 60-100rpm;
the rotation is variable speed rotation with acceleration of more than 120 rpm/min;
the rotation time is 2-10 minutes.
And c, after remelting in the step, carrying out d pulling-e rotating-f remelting steps for a plurality of times before growing the crystals in the step g.
Further, step d pulling-step e rotation is accompanied by a decrease in furnace pressure.
Further, in the first depressurization, the furnace pressure is reduced to 1/2-2/3 of that before depressurization;
when the pressure is reduced again, the furnace pressure is reduced to 1/5-1/15 of that before the pressure reduction.
Further, the first time of depressurization is 3-5min.
The invention has the beneficial effects that:
in the liquid phase method silicon carbide crystal growth process, the seed crystal is far away from the liquid level of the alloy solution during material melting, so that the vapor generated by volatilization of silicon during material melting is prevented from being contacted and solidified with the seed crystal at the cold end, and uneven attachment is generated. The seed rod and the graphite crucible are not rotated during the remelting, so that the convection of the solution is reduced, and the generation of bubble wrapping on the surface of the seed crystal is reduced. After the seed crystal is remelted, the seed crystal is pulled up rapidly at 5000-6000mm/h, and is rotated at variable speed, the alloy solution layer on the surface of the seed crystal is thinned, and bubbles wrapped on the surface of the seed crystal are thrown out. And the discharge of bubbles on the surface of the seed crystal is promoted along with the depressurization in the furnace. The steps of rotation and depressurization can be repeated for a plurality of times, so that bubbles on the surface of the seed crystal are eliminated, the surface of the seed crystal is smooth, and high-quality silicon carbide crystals are grown.
Drawings
FIG. 1 is a schematic diagram of a crystal growth apparatus according to the present invention;
FIG. 2 is a diagram showing a silicon carbide crystal obtained by the preparation of example 1 of the present invention;
FIG. 3 is a diagram showing a silicon carbide crystal obtained by the preparation of example 2 of the present invention;
FIG. 4 is a diagram showing a silicon carbide crystal obtained by preparing comparative example 1 according to the present invention;
FIG. 5 is a diagram showing a silicon carbide crystal obtained by preparing comparative example 2 according to the present invention;
FIG. 6 is a diagram showing a silicon carbide crystal obtained by preparing comparative example 3 according to the present invention;
in the figure: 1-seed crystal; 2-alloy solution; 3-a seed crystal holder; 4-seed crystal rods; 5-graphite crucible; 6-a crucible shaft; 7-heat preservation felt; 8-an induction coil; 9-furnace body.
Detailed Description
The invention is described in further detail below with reference to the drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting thereof.
The method for eliminating bubble wrapping in the liquid phase silicon carbide crystal growing process provided by the invention is carried out by a crystal growing device. The crystal growing device comprises a furnace body 9, and a graphite crucible 5 for Cheng Fangchang crystal raw materials is arranged in the furnace body 9. A seed rod 4 is arranged above the graphite crucible 5, a seed crystal support 3 is arranged at one end of the seed rod 4, and a silicon carbide seed crystal 1 is arranged on the seed crystal support 3. The graphite crucible 5 is provided with a thermal insulation felt 7, and the graphite crucible 5 is arranged on a crucible shaft 6. And a heating device for providing the temperature required by crystal growth, wherein in the embodiment provided by the invention, an induction coil 8 is adopted as the heating device, and the induction coil 8 heats and melts the crystal growth raw material into an alloy solution 2. And the vacuum pumping device is used for providing vacuum environment required by crystal growth.
Example 1
a, charging: and uniformly mixing the crystal growth raw materials, and then placing the mixture in a graphite crucible. The crystal growth raw material is configured as Si x Cr y Al z The raw materials comprise 49% of Si, 40% of Cr, 10% of Al and Sc, mn, mg, ge, as, sn, P, N, O, B, dy, Y, nb, nd, fe.
b, material melting: vacuumizing the furnace body to 5×10 -3 And (3) Pa, backfilling Ar gas to 90KPa in the furnace, heating the temperature in the furnace to 1800 ℃ at a heating rate of 800 ℃/h, and keeping the temperature for 1 hour to melt the crystal growth raw material in the graphite crucible to form an alloy solution. In the process of heating and melting, the distance between the seed crystal and the liquid level of the alloy solution is kept to be more than 50mm, so that the vapor generated by volatilization of silicon during melting is prevented from being contacted and solidified with the seed crystal at the cold end, and uneven attachment is generated.
c, remelting: lowering the seed rod to make the seed crystal immersed in the alloy solution for back melting; the seed rod is lowered at a speed of 500um/h to contact with the solution, the current seed crystal position is recorded, then lowered by 0.25mm, and remelted at a temperature of 1800 ℃ for 60min. The seed rod and the graphite crucible are not rotated during the remelting, so that the convection of the solution is reduced, and the generation of bubble wrapping on the surface of the seed crystal is reduced.
d, lifting: the seed rod was raised at a rise rate of 5000mm/h to disengage the seed from the alloying solution by 5mm.
And e, rotating: rotating the seed rod, and throwing out bubbles in the seed crystal to wrap the seed crystal; and (3) applying a rotating speed of 100rpm to the seed rod, performing clockwise and anticlockwise switching rotation at an acceleration of 200rpm/min, rotating for 2min, thinning the solution layer on the surface of the seed crystal, and throwing out surface bubbles.
The pulling and rotating process is accompanied by a reduction in pressure of 50KPa for 3 minutes to reduce the pressure in the furnace to 40KPa. As the pressure in the furnace drops, bubbles on the seed crystal are pushed out by the pressure.
And f, remelting: the seed rod is lowered at 300um/h, so that the seed crystal is immersed into the alloy solution for remelting for 10min.
And g, growing: the seed rod was rotated at a speed of 60rpm while being raised at 200mm/h, and the graphite crucible was rotated reversely at a speed of 10rpm, and crystal pulling growth was carried out for a period of 20 hours.
And h, after the crystal growth is completed, lifting the seed rod, enabling the lower surface of the crystal to leave the alloy solution, cooling, controlling the cooling rate at 200 ℃/h, rotating the seed rod at the speed of 1rpm in the cooling process, enabling the temperature of the crystal to be uniform, taking down the crystal after cooling, and completing crystal growth, wherein the method is shown in fig. 2. The surface is smooth, and only a small amount of bubbles (shown by circles) exist, so that the subsequent use is not affected.
Example 2
a, charging: and uniformly mixing the crystal growth raw materials, and then placing the mixture in a graphite crucible. The crystal growth raw material is configured as Si x Cr y Al z The raw materials comprise 49% of Si, 40% of Cr, 10% of Al and Sc, mn, mg, ge, as, sn, P, N, O, B, dy, Y, nb, nd, fe.
b, material melting: vacuumizing the furnace body to 5×10 -3 And (3) Pa, backfilling Ar gas to 90KPa in the furnace, heating the temperature in the furnace to 1800 ℃ at a heating rate of 800 ℃/h, and keeping the temperature for 1 hour to melt the crystal growth raw material in the graphite crucible to form an alloy solution. In the process of heating and melting, the distance between the seed crystal and the liquid level of the alloy solution is kept larger than50mm, avoiding the contact solidification of vapor generated by volatilization of silicon and cold end seed crystal during material melting, and generating uneven attachment.
c, remelting: lowering the seed rod to make the seed crystal immersed in the alloy solution for back melting; the seed rod is lowered at a speed of 500um/h to contact with the solution, the current seed crystal position is recorded, then lowered by 0.25mm, and remelted at a temperature of 1800 ℃ for 60min. The seed rod and the graphite crucible are not rotated during the remelting, so that the convection of the solution is reduced, and the generation of bubble wrapping on the surface of the seed crystal is reduced.
d, lifting: the seed rod was lifted at a lifting speed of 6000mm/h to disengage the seed from the alloying solution by 5mm.
And e, rotating: rotating the seed rod, and throwing out bubbles in the seed crystal to wrap the seed crystal; and (3) applying a rotating speed of 60rpm to the seed rod, performing clockwise and anticlockwise switching rotation at an acceleration of 120rpm/min, rotating for 3min, thinning the solution layer on the surface of the seed crystal, and throwing out surface bubbles.
The pulling and rotating process is accompanied by a pressure reduction speed of 45KPa for 3min to reduce the pressure in the furnace to 45KPa. As the pressure in the furnace drops, bubbles on the seed crystal are pushed out by the pressure.
And f, remelting: the seed rod is lowered at 300um/h, so that the seed crystal is immersed into the alloy solution for remelting for 10min.
And (3) secondary lifting: the seed rod was lifted at a lifting speed of 6000mm/h to disengage the seed from the alloying solution by 5mm.
And (3) secondary rotation: rotating the seed rod, and throwing out bubbles in the seed crystal to wrap the seed crystal; and (3) applying a rotating speed of 80rpm to the seed rod, performing clockwise and anticlockwise switching rotation at an acceleration of 150rpm/min, rotating for 2min, thinning the solution layer on the surface of the seed crystal, and throwing out surface bubbles.
The secondary pulling and rotating process is accompanied by reducing the pressure reducing speed of 5KPa to 40KPa in 2 min. As the pressure in the furnace drops, bubbles on the seed crystal are pushed out by the pressure.
And (5) secondary remelting: the seed rod is lowered at 300um/h, so that the seed crystal is immersed into the alloy solution for remelting for 10min.
Three times of lifting: the seed rod was lifted at a lifting speed of 6000mm/h to disengage the seed from the alloying solution by 5mm.
Three rotations: rotating the seed rod, and throwing out bubbles in the seed crystal to wrap the seed crystal; and (3) applying a rotating speed of 80rpm to the seed rod, performing clockwise and anticlockwise switching rotation at an acceleration of 150rpm/min, rotating for 2min, thinning the solution layer on the surface of the seed crystal, and throwing out surface bubbles.
The three pulling and rotating processes are accompanied by reducing the pressure reducing speed of 5KPa to 35KPa in 2 min. As the pressure in the furnace drops, bubbles on the seed crystal are pushed out by the pressure.
And (3) remelting for three times: the seed rod is lowered at 300um/h, so that the seed crystal is immersed into the alloy solution for remelting for 10min.
And g, growing: the seed rod was rotated at a speed of 60rpm while being raised at 200mm/h, and the graphite crucible was rotated reversely at a speed of 10rpm, and crystal pulling growth was carried out for a period of 20 hours.
And h, after the crystal growth is completed, lifting the seed rod, enabling the lower surface of the crystal to leave the alloy solution, cooling, controlling the cooling rate at 200 ℃/h, rotating the seed rod at the speed of 1rpm in the cooling process, enabling the temperature of the crystal to be uniform, taking down the crystal after cooling, and completing the crystal growth, wherein the figure 3 is shown. After multiple pulling-rotating accompanied depressurization treatments, almost no bubbles exist, and the crystal quality is high.
Comparative example 1
In comparison with example 1, the difference is that the d-pulling, e-spinning process is not accompanied by depressurization, and the resulting crystal is prepared as shown in FIG. 4. The rotation is not accompanied by depressurization, and part of bubbles are difficult to release, and part of bubbles still exist in the crystal.
Comparative example 2
The difference from example 1 is that the e-rotation treatment is not performed after the d-pulling.
d, pulling is carried out along with depressurization, the time for pulling out the alloy solution by the seed crystal is 2min, and after the pulling is finished, f is directly carried out, and g is grown. The crystals obtained are shown in FIG. 5. After pulling, only the pressure is reduced without rotation, so that bubbles are difficult to discharge, and a large number of bubbles remain in the crystal.
Comparative example 3
Compared with example 1, the difference is that the e-rotation and depressurization treatment is not performed after the d-pulling.
The time for pulling out the alloy solution by the seed crystal is 2min, and after the pulling is finished, f is directly carried out and then remelting and g crystal growth are carried out. The crystals obtained are shown in FIG. 6. The bubble wrapping is serious in the crystal growth process, and the quality of the grown crystal is poor and cannot be applied.
According to the embodiment and the comparative example, in the liquid phase method silicon carbide crystal growth process, the seed crystal is quickly pulled up after being remelted, and the speed change rotation is carried out, so that the alloy solution layer on the surface of the seed crystal is thinned, and bubbles wrapped on the surface of the seed crystal are thrown out. Pulling and rotating are accompanied with depressurization in the furnace, so that the discharge of bubbles on the surface of the seed crystal is promoted. Therefore, bubbles on the surface of the seed crystal are eliminated, the surface of the seed crystal is smooth, and high-quality silicon carbide crystals can be grown.
It is to be understood that the above examples of the present invention are provided for clarity of illustration only and are not limiting of the embodiments of the present invention. Various obvious changes, rearrangements and substitutions can be made by those skilled in the art without departing from the scope of the invention. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (7)
1. The method for eliminating bubble wrapping in the liquid phase silicon carbide crystal growth process is characterized by comprising the following steps of: the crystal growth is supported on a crystal growth device, and the crystal growth device comprises a furnace body;
a graphite crucible for Cheng Fangchang crystal raw materials is arranged in the furnace body;
a seed rod is arranged above the graphite crucible;
the seed crystal support is arranged at one end of the seed crystal rod, and a silicon carbide seed crystal is arranged on the seed crystal support;
heating means for providing a temperature required for crystal growth;
the vacuumizing device is used for providing a vacuum environment required by crystal growth;
the method for eliminating the bubble wrapping comprises the following steps:
a, charging: uniformly mixing the crystal growth raw materials, and then placing the mixture in a graphite crucible;
b, material melting: heating the crystal growth raw material to 1600-2100 ℃ to melt the raw material and form an alloy solution;
c, remelting: lowering the seed rod to make the seed crystal immersed in the alloy solution for back melting;
d, lifting: raising the seed rod to separate the seed crystal from the alloy solution;
and e, rotating: rotating the seed rod, and throwing out bubbles in the seed crystal to wrap the seed crystal;
and f, remelting: lowering the seed rod to make the seed crystal immersed in the alloy solution for re-melting;
and g, growing: lifting and rotating the seed rod, and rotating the graphite crucible to perform crystal pulling growth;
h, after the crystal growth is completed, lifting the seed rod to enable the lower surface of the crystal to leave the alloy solution, cooling, and taking down the crystal after cooling to complete crystal growth;
in the material melting process in the step b, the distance between the seed crystal and the liquid level of the alloy solution is more than 50mm;
step c, the remelting process and step f, the seed rod rotation and the graphite crucible rotation are not carried out;
step d pulling-step e rotation is accompanied by a decrease in furnace pressure.
2. The method according to claim 1, characterized in that: in the pulling process of the step d, the pulling speed is 5000-6000mm/h;
and lifting the seed crystal until the seed crystal is separated from the alloy liquid level.
3. The method according to claim 1, characterized in that: and e, in the rotating process of the step e, the rotation comprises clockwise rotation, anticlockwise rotation and clockwise and anticlockwise alternating rotation.
4. A method according to claim 3, characterized in that: the rotating speed of the rotation is 60-100rpm;
the rotation is variable speed rotation with acceleration of more than 120 rpm/min;
the rotation time is 2-10 minutes.
5. The method according to claim 1, characterized in that: and c, after the remelting in the step c, carrying out a plurality of d pulling-e rotating-f remelting steps before the crystal growth in the step g.
6. The method according to claim 5, wherein: when the pressure is reduced for the first time, the furnace pressure is reduced to 1/2-2/3 of that before the pressure reduction;
when the pressure is reduced again, the furnace pressure is reduced to 1/5-1/15 of that before the pressure reduction.
7. The method according to claim 6, wherein: the first time of depressurization is 3-5min.
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