CN117005031A - Method for inhibiting growth of nanowires on seed crystal in AlN single crystal growth process - Google Patents
Method for inhibiting growth of nanowires on seed crystal in AlN single crystal growth process Download PDFInfo
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- CN117005031A CN117005031A CN202310997952.4A CN202310997952A CN117005031A CN 117005031 A CN117005031 A CN 117005031A CN 202310997952 A CN202310997952 A CN 202310997952A CN 117005031 A CN117005031 A CN 117005031A
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- 239000013078 crystal Substances 0.000 title claims abstract description 100
- 238000000034 method Methods 0.000 title claims abstract description 48
- 239000002070 nanowire Substances 0.000 title claims abstract description 36
- 230000002401 inhibitory effect Effects 0.000 title claims abstract description 11
- 239000002994 raw material Substances 0.000 claims description 36
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 34
- 238000010438 heat treatment Methods 0.000 claims description 25
- 238000005086 pumping Methods 0.000 claims description 24
- 230000006698 induction Effects 0.000 claims description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- 238000007789 sealing Methods 0.000 claims description 9
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 9
- 229910052721 tungsten Inorganic materials 0.000 claims description 9
- 239000010937 tungsten Substances 0.000 claims description 9
- 230000000630 rising effect Effects 0.000 abstract description 9
- 238000000859 sublimation Methods 0.000 abstract description 8
- 230000008022 sublimation Effects 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 abstract description 3
- 230000005764 inhibitory process Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 16
- 238000001816 cooling Methods 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 238000003825 pressing Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008646 thermal stress Effects 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
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
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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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
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- Crystallography & Structural Chemistry (AREA)
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- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to the technical field of aluminum nitride growth, in particular to a method for inhibiting growth of nanowires on seed crystals in an AlN single crystal growth process. In order to solve the problem that nanowires are easy to generate in the growth process, the invention provides the optimal condition for inhibiting the nanowires, firstly, the height of the materials needs to be sufficiently supplemented, and the height of the materials needs to be maintained at 5/12-7/12 of the height of the crucible; in addition, the temperature rising rate of the middle temperature rising section in the crucible is accelerated, namely the sublimation rate of AlN vapor in the early growth stage is accelerated, so that the partial pressure of the Al vapor at the seed crystal surface above the top of the crucible rapidly reaches a supersaturation state, and the generation of AlN nanowires is inhibited. The method has extremely obvious inhibition effect on the nanowire, and the AlN crystal ingot obtained by growth mainly grows along the seed crystal surface, so that the generation of AlN polycrystal can be reduced, and the problem that the AlN crystal cannot grow along the seed crystal is solved to a certain extent.
Description
Technical Field
The invention relates to the technical field of aluminum nitride growth, in particular to a method for inhibiting growth of nanowires on seed crystals in an AlN single crystal growth process.
Background
The AlN crystal has an ultra-wide forbidden bandwidth (6.2 eV) and high thermal conductivity (3.2W cm -1 K -1 ) Excellent physical properties such as high resistivity and high surface acoustic velocity (5600-6000 m/s) have been receiving attention from scientists. Devices made using AlN crystals have extremely excellent optoelectronic properties, but are very expensive, mainly due to the difficulty in growing AlN crystals. Currently known growth methods include an aluminum metal direct nitriding method, a solution method, a hydride vapor phase epitaxy method, a physical vapor transport method (PVT) and the like, and through decades of research, the physical vapor transport method is considered to be the most effective method capable of preparing high-quality large-size AlN crystals, but the method still has the disadvantage that the problem of having the greatest influence on the crystal quality is growing polycrystal, and the polycrystal greatly influences the quality of the whole crystal. It is found that the reason for the generation of polycrystal is mainly that a large number of nanowires are generated on the surface of the seed crystal in the nucleation stage of the initial growth stage of the AlN crystal, so that the seed crystal loses the inducibility, and polycrystal is bred. Therefore, how to prevent the generation of AlN nanowires at the early stage of crystal growth becomes the most important problem to be solved in the AlN single crystal growth process.
A large number of experimental researches show that the growth temperature of the AlN nanowire is 1700-2050 ℃, when the temperature is just in the stage in the growth temperature rising process of AlN, the AlN raw material area below can not sublimate in a large amount to provide sufficient aluminum vapor because the temperature just reaches the sublimation point of AlN, only a small part of the Al vapor is transmitted to a seed crystal interface, and the growth of AlN at the seed crystal is linear due to insufficient raw materials.
Therefore, how to maintain the aluminum vapor in a supersaturated state in a short time and to suppress the growth of nanowires has become a challenge to be solved in the current growth of AlN bulk crystals.
Disclosure of Invention
In order to achieve the above object, the present invention provides the following technical solutions:
a method for inhibiting growth of nanowires on a seed crystal during growth of an AlN single crystal, comprising the steps of:
s1, filling a raw material for AlN growth in a crucible, and controlling the height of the raw material to be 5/12-7/12 of the height of the crucible;
s2, sealing the crucible and placing the crucible into an AlN growth furnace chamber, adjusting the position of the crucible so that the highest temperature point of the crucible is at the center position of the raw material, vacuumizing and filling nitrogen to more than 1atm;
s3, maintaining the pressure constant, and raising the temperature in the AlN growing furnace from room temperature to 1700 ℃ at a speed of 5-6 ℃/min, and keeping the temperature constant; then rapidly heating to 2200 ℃ at the speed of 9-12 ℃/min, and keeping the temperature constant again; after the temperature is stable, pumping pressure is carried out to 0.3-0.4atm; heating to the growth temperature after the pumping is completed; continuing to perform crystal growth at constant temperature;
s4, after the constant-temperature growth is completed, nitrogen is filled to increase the pressure to more than 1atm, then the temperature is reduced to room temperature at a temperature reduction rate of 5-6 ℃/min, and the crucible is taken out.
According to a preferred embodiment of the present invention, in step S1, the crucible is a tungsten crucible.
According to a preferred embodiment of the present invention, in step S2, the AlN growth furnace is an induction furnace or a resistance furnace.
According to the invention, in the step S3, the temperature in the AlN growing furnace is raised to 1700 ℃ from room temperature at a speed of 5-6 ℃/min, the temperature is kept constant for 1-1.5h, and the temperature is accelerated to rise after the temperature is stabilized at 1700 ℃.
According to the invention, in the step S3, the pumping time is 3-4h.
According to the invention, in step S3, the temperature is rapidly increased to 2200 ℃ at a speed of 9-12 ℃/min, the temperature is kept constant again for 1-1.5h, and then the subsequent pumping operation is carried out.
Compared with the prior art, the invention has the following beneficial technical effects:
in order to solve the problem that nanowires are easy to generate in the growth process, the invention provides the optimal condition for inhibiting the nanowires, firstly, the height of the materials needs to be sufficiently supplemented, and the height of the materials needs to be maintained at 5/12-7/12 of the height of the crucible; in addition, the temperature rising rate of the middle temperature rising section in the crucible is accelerated, namely the sublimation rate of AlN vapor in the early growth stage is accelerated, so that the partial pressure of the Al vapor at the seed crystal surface above the top of the crucible rapidly reaches a supersaturation state, and the generation of AlN nanowires is inhibited. The method has extremely obvious inhibition effect on the nanowire, and the AlN crystal ingot obtained by growth mainly grows along the seed crystal surface, so that the generation of AlN polycrystal can be reduced, and the problem that the AlN crystal cannot grow along the seed crystal is solved to a certain extent.
Drawings
FIG. 1 shows an AlN seed crystal used in example 1.
Fig. 2 is a photograph of AlN ingot obtained in example 1.
Fig. 3 is a picture of AlN nanowires obtained by short-time growth in comparative example 1.
Fig. 4 is a photograph of AlN ingot obtained in comparative example 2.
Fig. 5 is a photograph of AlN ingot obtained in comparative example 3.
Fig. 6 is a photograph of AlN ingot obtained in comparative example 4.
Fig. 7 is a photograph of AlN ingot obtained in comparative example 5.
Fig. 8 is a photograph of AlN ingot obtained in comparative example 6.
Detailed Description
The present invention now will be described more fully hereinafter with reference to the accompanying drawings, in which exemplary embodiments of the invention are shown. This invention may, however, be embodied in many different forms and should not be construed as limited to the exemplary embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The growth temperature was the same in the examples of the present invention and comparative examples.
Example 1
A method for inhibiting growth of nanowires on a seed crystal in an AlN single crystal growth process, comprising the steps of:
s1, filling AlN growth raw materials into a common tungsten crucible by using an induction method, and controlling the height of the raw materials to be 1/2 of the height of the crucible;
s2, sealing the crucible and placing the crucible into an AlN induction growth furnace chamber, adjusting the position of the crucible to a high crucible position, enabling the highest temperature point of the crucible to be at the center position of the raw material, vacuumizing and filling nitrogen to 1.1atm;
s3, starting to heat, heating the temperature from room temperature to 1700 ℃ at a speed of 5 ℃/min, and keeping the temperature for 1 hour after the temperature reaches 1700 ℃; then rapidly heating to 2200 ℃ at the speed of 10 ℃/min, and keeping the temperature for 1 hour after reaching 2200 ℃; pumping the pressure to 0.3atm after constant temperature; heating to the growth temperature after the pumping is completed; and continuing to keep the temperature for 30 hours for crystal growth.
And S4, after the crystal growth is completed, charging nitrogen to increase the pressure to 1.1atm, cooling to room temperature at a cooling rate of 5-6 ℃/min, and taking out the crucible and the crystal.
In the embodiment, the height of the raw materials accounts for 1/2 of the height of the crucible, the heating rate of the middle heating section is 10 ℃/min, the AlN vapor sublimation rate in the early growth stage is accelerated, the partial pressure of the Al vapor of the upper seed crystal face rapidly reaches a supersaturated state, and the AlN nanowire is restrained from being generated. FIG. 1 shows a seed crystal used in example 1. After 30h of growth, the AlN ingot with the thickness of 8mm is finally obtained, as shown in fig. 2, the surface shape of the ingot is basically consistent with that of the seed crystal, the seed crystal in the early growth stage is not interfered by the nanowire to generate a polycrystalline region, and by adopting the method of the embodiment, the growth of the nanowire in the early growth stage is obviously reduced, so that the AlN ingot can smoothly grow along the trace of the seed crystal, the generation of AlN polycrystal is reduced, and the defect that an AlN crystal cannot grow along the seed crystal in the prior art can be overcome to a certain extent.
Comparative example 1
In order to trace the reason of growing polycrystal, we can cool down to stop the crystal growth at the initial stage of growth, and observe the reason, the specific steps are as follows:
s1, filling AlN growth raw materials into a common tungsten crucible by using an induction method, and controlling the height of the raw materials to be 1/2 of the height of the crucible;
s2, sealing the crucible and placing the crucible into an AlN induction growth furnace chamber, adjusting the position of the crucible to a high crucible position, enabling the highest temperature point of the crucible to be at the center position of the raw material, vacuumizing and filling nitrogen to 1.1atm;
s3, starting to heat, heating the temperature from room temperature to 2200 ℃ at a speed of 5 ℃/min, and keeping the temperature at the constant temperature for 1 hour after the temperature reaches 2200 ℃; pumping pressure to 0.3atm after constant temperature; heating to the growth temperature after the pumping is completed; and continuing to perform crystal growth at constant temperature for only 1 hour.
And S4, cooling after the crystal growth is completed, and taking out the crucible.
As a result, the ingot is shown in FIG. 3, and a large number of nanowires are grown on the early-stage seed crystal, and the traces of the seed crystal are basically completely covered by the nanowires, so that the seed crystal is invalid, the crystal can not grow along the seed crystal, and a large number of polycrystal growth occurs.
Comparative example 2
The AlN single crystal is grown by adopting the method in the prior art, and the method comprises the following steps:
s1, filling AlN growth raw materials into a common tungsten crucible by using an induction method, and controlling the height of the raw materials to be 1/4 of the height of the crucible;
s2, sealing the crucible and placing the crucible into an AlN induction growth furnace chamber, adjusting the position of the crucible to a high crucible position, enabling the highest temperature point of the crucible to be at the center position of the raw material, vacuumizing and filling nitrogen to 1.1atm;
s3, starting to heat, heating the temperature from room temperature to 1700 ℃ at a speed of 5 ℃/min, and keeping the temperature for 1 hour after the temperature reaches 1700 ℃; then rapidly heating to 2200 ℃ at the speed of 10 ℃/min, and keeping the temperature for 1 hour after reaching 2200 ℃; pumping pressure to 0.3atm after constant temperature; heating to the growth temperature after the pumping is completed; and continuing to keep the temperature for 30 hours for crystal growth.
And S4, after the crystal growth is completed, charging nitrogen to increase the pressure to 1.1atm, cooling to room temperature at a cooling rate of 5-6 ℃/min, and taking out the crucible and the crystal.
Because the height of the raw material is too low, the consumption of the raw material is too small (the weight is only 150 g), and when the temperature reaches the sublimation point of aluminum nitride, sufficient aluminum vapor cannot be provided for a seed crystal face, as shown in fig. 4, so that the growth mode of AlN crystals is changed from columnar growth to needle growth, a punctiform AlN polycrystalline layer is macroscopically formed, and even if the temperature rising rate of an intermediate temperature rising section is accelerated, the generation of AlN nanowires cannot be avoided.
Comparative example 3
The AlN single crystal is grown by adopting the method in the prior art, and the method comprises the following steps:
s1, filling AlN growth raw materials into a common tungsten crucible by using an induction method, and controlling the height of the raw materials to be 3/4 of the height of the crucible;
s2, sealing the crucible and placing the crucible into an AlN induction growth furnace chamber, adjusting the position of the crucible to a high crucible position, enabling the highest temperature point of the crucible to be at the center position of the raw material, vacuumizing and filling nitrogen to 1.1atm;
s3, starting to heat, heating the temperature from room temperature to 1700 ℃ at a speed of 5 ℃/min, and keeping the temperature for 1 hour after the temperature reaches 1700 ℃; then rapidly heating to 2200 ℃ at the speed of 10 ℃/min, and keeping the temperature for 1 hour after reaching 2200 ℃; pumping the pressure to 0.3atm after constant temperature; heating to the growth temperature after the pumping is completed; and continuing to keep the temperature for 30 hours for crystal growth.
And S4, after the crystal growth is completed, charging nitrogen to increase the pressure to 1.1atm, cooling to room temperature at a cooling rate of 5-6 ℃/min, and taking out the crucible and the crystal.
When the height of the internal raw material is 3/4, the weight of the raw material exceeds 350g, the excessive raw material causes an excessively high growth rate, which is unfavorable for controlling the AlN growth rate, the excessively high growth rate easily causes the deterioration of the crystallization quality of the crystal, as shown in FIG. 5, more vacancy defects and dislocation appear in the interior, and a plurality of holes and cracks appear on the macro scale, which are extremely unfavorable for growth and are difficult to eliminate in the later stage.
Comparative example 4
The AlN single crystal is grown by adopting a common temperature rising process, which comprises the following steps:
s1, filling AlN growth raw materials into a common tungsten crucible by using an induction method, and controlling the height of the raw materials to be 1/2 of the height of the crucible;
s2, sealing the crucible and placing the crucible into an AlN induction growth furnace chamber, adjusting the position of the crucible to a high crucible position, enabling the highest temperature point of the crucible to be at the center position of the raw material, vacuumizing and filling nitrogen to 1atm;
s3, starting to heat, heating the temperature from room temperature to 2200 ℃ at a speed of 5 ℃/min, keeping the temperature constant, pumping and pressing for 3 hours, and pumping the pressure to 0.3atm; heating to the growth temperature after the pumping is completed; and continuing to keep the temperature for 30 hours for crystal growth.
And S4, after the crystal growth is completed, nitrogen is filled to raise the pressure to 1.1atm, the temperature is reduced to room temperature, and the crucible and the crystal are taken out.
According to a large number of experimental researches, 1700-2100 ℃ is the temperature stage at which the nanowires are most easily generated, in the comparative example, the temperature is increased from room temperature to 2200 ℃ at a speed of 5 ℃/min, and the temperature is in a temperature stage at which the AlN nanowires are easily generated for a long time in the heating process. In the early stage of temperature rising, only part of raw materials reach the gaseous sublimation point of AlN and form Al vapor, and only a small part of the Al vapor reaches a deposition interface, so that columnar crystals cannot be formed at the deposition interface due to the fact that the aluminum vapor content is too low, the columnar crystals grow in a needle shape, finally the nanowire is formed, and as shown in fig. 6, traces of existence of seed crystals are basically not seen.
Comparative example 5
The AlN single crystal is grown by adopting the method in the prior art, and the method comprises the following steps:
s1, filling AlN growth raw materials into a common tungsten crucible by using an induction method, and controlling the height of the raw materials to be 1/2 of the height of the crucible;
s2, sealing the crucible and placing the crucible into an AlN induction growth furnace chamber, adjusting the position of the crucible to a high crucible position, enabling the highest temperature point of the crucible to be at the center position of the raw material, vacuumizing and filling nitrogen to 1.1atm;
s3, starting to heat, heating the temperature from room temperature to 1800 ℃ at a speed of 5 ℃/min, and keeping the temperature for 1 hour after reaching 1800 ℃; then rapidly heating to 2200 ℃ at the speed of 10 ℃/min, and keeping the temperature for 1 hour after reaching 2200 ℃; after constant temperature, pumping and pressing for 3 hours, and pumping the pressure to 0.3atm; heating to the growth temperature after the pumping is completed; and continuing to keep the temperature for 30 hours for crystal growth.
And S4, after the crystal growth is completed, nitrogen is filled to raise the pressure to 1.1atm, the temperature is reduced to room temperature, and the crucible and the crystal are taken out.
In this comparative example, when the temperature is raised from room temperature to 1800 ℃, and at this time, the temperature reaches the theoretical sublimation point of AlN powder, and the nanowire is formed at the seed crystal surface after the temperature is maintained for 1 hour at 1800 ℃, as shown in fig. 8, the subsequent nanowire substantially shields the seed crystal, so that the seed crystal loses the induction effect, and the subsequent continued growth of the crystal is affected.
Comparative example 6
The AlN single crystal is grown by adopting the method in the prior art, and the method comprises the following steps:
s1, filling AlN growth raw materials into a common tungsten crucible by using an induction method, and controlling the height of the raw materials to be 1/2 of the height of the crucible;
s2, sealing the crucible and placing the crucible into an AlN induction growth furnace chamber, adjusting the position of the crucible to a high crucible position, enabling the highest temperature point of the crucible to be at the center position of the raw material, vacuumizing and filling nitrogen to 1.1atm;
s3, starting to heat, and heating the temperature from room temperature to 1600 ℃ at a speed of 5 ℃/min until the temperature reaches 1600 ℃; after constant temperature, pumping and pressing for 3 hours, and pumping the pressure to 0.3atm; heating to the growth temperature after the pumping is completed; and continuing to keep the temperature for 30 hours for crystal growth.
And S4, after the crystal growth is completed, nitrogen is filled to raise the pressure to 1.1atm, the temperature is reduced to room temperature, and the crucible and the crystal are taken out.
In this comparative example, the temperature rise to 1600 ℃ did not reach the theoretical sublimation point of AlN, as shown in fig. 8, but the phenomenon of seed crystal cracking occurred, possibly related to excessive thermal stress during the rapid temperature rise, and the rapid temperature rise at 1700 ℃ did not occur instead.
The above description is only for the purpose of illustrating the invention, and it should be understood that the invention is not limited to the above embodiments, but various modifications consistent with the idea of the invention are within the scope of the invention.
Claims (6)
1. A method for inhibiting growth of nanowires on a seed crystal during growth of an AlN single crystal, comprising the steps of:
s1, filling a raw material for AlN growth in a crucible, and controlling the height of the raw material to be 5/12-7/12 of the height of the crucible;
s2, sealing the crucible and placing the crucible into an AlN growth furnace chamber, adjusting the position of the crucible so that the highest temperature point of the crucible is at the center position of the raw material, vacuumizing and filling nitrogen to more than 1atm;
s3, maintaining the pressure constant, and raising the temperature in the AlN growing furnace from room temperature to 1700 ℃ at a speed of 5-6 ℃/min, and keeping the temperature constant; then rapidly heating to 2200 ℃ at the speed of 9-12 ℃/min, and keeping the temperature constant again; after the temperature is stable, pumping pressure is carried out to 0.3-0.4atm; heating to the growth temperature after the pumping is completed; performing crystal growth at the growth temperature;
s4, after the constant-temperature growth is completed, nitrogen is filled to increase the pressure to more than 1atm, then the temperature is reduced to room temperature at a temperature reduction rate of 5-6 ℃/min, and the crucible is taken out.
2. A method of suppressing growth of nanowires on a seed crystal during growth of an AlN single crystal according to claim 1, wherein in step S1, the crucible is a tungsten crucible.
3. A method of suppressing growth of nanowires on a seed crystal during growth of an AlN single crystal according to claim 1, wherein in step S2, the AlN growth furnace is an induction furnace or a resistance furnace.
4. A method for suppressing growth of nanowires on seed crystal during growth of AlN single crystal according to claim 1, wherein in step S3, the temperature in the AlN growth furnace is raised from room temperature to 1700 ℃ at a rate of 5-6 ℃/min, and the temperature is maintained for 1-1.5 hours.
5. A method for inhibiting growth of nanowires on a seed crystal during growth of an AlN single crystal according to claim 1, wherein the time for the pumping is 3-4 hours in step S3.
6. A method for inhibiting growth of nanowires on seed crystal during growth of AlN single crystal according to claim 1, characterized in that in step S3, the temperature is raised rapidly to 2200 ℃ at a rate of 9-12 ℃/min, and the temperature is maintained again for 1-1.5h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310642515 | 2023-06-01 |
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