CN109440189B - Crystal growth device with locally reinforced light modulation - Google Patents
Crystal growth device with locally reinforced light modulation Download PDFInfo
- Publication number
- CN109440189B CN109440189B CN201811615323.6A CN201811615323A CN109440189B CN 109440189 B CN109440189 B CN 109440189B CN 201811615323 A CN201811615323 A CN 201811615323A CN 109440189 B CN109440189 B CN 109440189B
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- light source
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- beam shaping
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- crystal growth
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- 239000013078 crystal Substances 0.000 title claims abstract description 85
- 238000007493 shaping process Methods 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims description 21
- 230000003287 optical effect Effects 0.000 claims description 20
- 230000033001 locomotion Effects 0.000 claims description 12
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 6
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 230000005674 electromagnetic induction Effects 0.000 claims description 3
- 239000003562 lightweight material Substances 0.000 claims description 3
- 230000000737 periodic effect Effects 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 229910052594 sapphire Inorganic materials 0.000 claims description 3
- 239000010980 sapphire Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 230000005469 synchrotron radiation Effects 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 229910002601 GaN Inorganic materials 0.000 description 5
- 230000001965 increasing effect Effects 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 229910052733 gallium Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 238000007716 flux method Methods 0.000 description 2
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- C30B29/406—Gallium nitride
-
- 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
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
- C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
- C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
- C30B9/10—Metal solvents
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a crystal growth device with locally enhanced light modulation, which comprises a reaction kettle, a laser light source, a crucible arranged in the reaction kettle, a reaction solution loaded in the crucible, seed crystals immersed in the reaction solution and a beam shaping component, wherein the reaction kettle is provided with an incident window, a light beam emitted by the laser light source is injected into the crucible through the incident window, the beam shaping component is arranged between the incident window and the seed crystals, the light beam can be converged at the local position of the seed crystals through the beam shaping component or can be weakened through the beam shaping component.
Description
Technical Field
The invention relates to the technical field of crystal growth, in particular to a crystal growth device with locally reinforced optical modulation.
Background
Gallium nitride (GaN) has been widely used in photoelectric and power microwave devices because of its advantages of large forbidden bandwidth, stable chemical properties, high temperature resistance, high mobility, etc. Currently, the growth methods of GaN crystals include Metal Organic Chemical Vapor Deposition (MOCVD), hydride Vapor Phase Epitaxy (HVPE), ammonothermal method (Ammothermal Growth) and sodium Flux method (Na Flux), wherein the sodium Flux method for growing GaN crystals has better crystal quality and faster growth rate, which is one of the preferred growth methods. At present, nitrogen is required to be introduced into an autoclave adopting a sodium flow method, the nitrogen in the autoclave is dissolved into Ga-Na solution in a crucible under the conditions of high temperature and high pressure, so that a seed crystal can be subjected to reaction to grow into GaN crystals, meanwhile, the electrolysis of the nitrogen can be promoted by introducing light into the autoclave, the dissolution of the nitrogen into the reaction solution is accelerated, and the growth rate of the GaN crystals is improved, but in the growth process of the GaN crystals, the whole seed crystal is in a constant state, and the local temperature adjustment cannot be performed according to the growth state of crystal materials, so that the local growth rate of the seed crystal cannot be adjusted.
Disclosure of Invention
In order to solve the above problems, the present invention provides a locally enhanced optical modulation crystal growth apparatus which locally adjusts the optical intensity and temperature to effectively locally enhance or reduce the crystal growth rate.
In order to solve the above-mentioned purpose, the following technical scheme is adopted in the invention.
The utility model provides a crystal growth device that light modulation part was strengthened, includes reation kettle, laser source, the crucible of setting in reation kettle, load in the crucible reaction solution and soak the seed crystal in reaction solution, reation kettle is equipped with incident window, and the light beam that laser source sent is penetrated into in the crucible through incident window, still includes beam shaping components and parts, and beam shaping components and parts locate between incident window and the seed crystal, can assemble the light beam in the local position of seed crystal or can weaken the light beam in the local position of seed crystal through beam shaping components and parts.
Preferably, the reactor further comprises an open cavity seed crystal clamp, wherein the seed crystal is arranged on the open cavity seed crystal clamp, and the open cavity seed crystal clamp can be suspended in the reaction solution.
Preferably, the beam shaping element is mounted in the open cavity seed crystal holder with the beam shaping element located above the seed crystal.
Preferably, the open-cavity seed holder is made primarily of a lightweight material, which may be SiC or thin-walled quartz.
Preferably, the beam shaping device is provided with at least one optical lens arranged with a number of microstructures which may be arranged as optical lenses or filters to enhance or attenuate the beam at the local position of the seed crystal.
Preferably, the light beam emitted by the laser light source can be kept stationary or can perform scanning movement in the reaction kettle cavity, and the scanning movement can be periodic movement scanning or irregular movement scanning.
Preferably, the laser light source may be one or more of a synchrotron radiation light source, an LD light source, an LED light source or a frequency multiplication light source, and the light intensity of the light beam emitted from the laser light source may be constant or adjustable.
Preferably, the laser light source emits ultraviolet light or infrared light, and the light beam emitted by the laser light source may be continuous light or pulsed light.
Preferably, the reactor further comprises a heating device, wherein the heating device can heat the reaction solution in the crucible to reach the required crystal growth temperature, the heating device is one or more of an electromagnetic induction heating device, a heat conduction heating device or a radio frequency heating device, and the reactor is provided with an air inlet and an air outlet for introducing air and adjusting pressure.
Preferably, the seed crystal may be one or more of a sapphire substrate or a silicon carbide substrate and the beam shaping device may be one or more of a convex lens or a prism.
The beneficial effects of the invention are as follows:
compared with the prior art, the invention is additionally provided with the beam shaping component, the light beam emitted by the laser light source is injected into the crucible through the incident window, the beam shaping component can converge or weaken the light beam, and a bright and dark area is formed on the back surface of the seed crystal after the light beam passes through the beam shaping component, so that the light intensity and the temperature of the local position of the seed crystal are adjusted, the crystal growth rate is effectively and locally enhanced or weakened, in the practical application process, when the beam shaping component converges the light beam at the local point on the back surface of the seed crystal, the temperature of the local area with high light intensity is gradually increased under the action of high illumination, the crystal growth rate is effectively and when the beam shaping component weakens the light beam, the temperature of the local area with low light intensity is lower than the temperature of the local area with high light intensity, and the crystal growth rate is relatively and locally weakened.
Drawings
FIG. 1 is a schematic cross-sectional view of one embodiment of the present invention;
fig. 2 is a schematic structural diagram of a beam shaping element according to an embodiment of the present invention.
Reference numerals illustrate: 1. the reaction kettle, 2, an air inlet, 3, an air outlet, 4, a heating device, 5, a crucible, 6, a reaction solution, 7, a seed crystal and 8, a seed crystal fixture with an open cavity, 9, a laser light source, 10, an incident window, 11, a light beam shaping component and 110, and a microstructure.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
Referring to fig. 1 to 2, a crystal growth apparatus with locally enhanced light modulation includes a reaction kettle 1, a laser light source 9, a crucible 5 disposed in the reaction kettle 1, a reaction solution 6 loaded in the crucible 5, a seed crystal 7 immersed in the reaction solution 6, and a beam shaping device 11, wherein the reaction kettle 1 is provided with an incident window 10, the beam emitted from the laser light source 9 is injected into the crucible 5 through the incident window 10, the beam shaping device 11 is disposed between the incident window 10 and the seed crystal 7, the beam can be converged at a local position of the seed crystal 7 by the beam shaping device 11 or can be weakened by the beam shaping device 11, compared with the prior art, the embodiment is additionally provided with the beam shaping device 11, the beam emitted from the laser light source 9 is injected into the crucible 5 through the incident window 10, the beam shaping device 11 can be converged or weakened, and forms a bright and dark area on the back surface of the seed crystal 7 after the beam shaping device 11, thereby realizing light intensity and temperature adjustment of the local position of the seed crystal 7, effectively enhancing or crystal growth rate locally, in the practical application, when the beam shaping device 11 is a local light intensity is converged at a local position of the seed crystal 7 or a local light intensity point, the local light intensity is reduced at a local temperature increasing area, and the local light intensity is gradually reduced at a local temperature increasing area when the local light intensity is locally increasing and locally increasing the crystal growth rate is relatively high.
In this embodiment, the beam shaping device converges the light beam at a local point on the back of the seed crystal 7, referring to fig. 2, the beam shaping device employs a complete optical lens, where a plurality of microstructures 110 are arranged, the microstructures 110 may be configured as optical lenses, and the local point after the light beam passes through the optical lenses converges on the back of the seed crystal 7, so as to locally change the growth rate of the crystal material, in other preferred embodiments, the microstructures 110 may be configured as optical filters, and weaken the light beam at the local position of the seed crystal 7, so as to locally change the growth rate of the sample material, and in other preferred embodiments, the beam shaping device may be one or more of a convex lens or a prism, so as to locally change the growth rate of the sample material, which is not described herein.
As shown in fig. 1, the embodiment further includes an open cavity seed crystal holder 8, the seed crystal 7 is mounted in the open cavity seed crystal holder 8, the open cavity seed crystal holder 8 can be suspended in the reaction solution 6, the beam shaping component 11 is mounted in the open cavity seed crystal holder 8, and the beam shaping component 11 is located above the seed crystal 7, the open cavity seed crystal holder 8 is mainly made of a light material, the light material can be SiC or thin-walled quartz, the seed crystal 7 of the embodiment can be one or more of a sapphire substrate or a silicon carbide substrate, the reaction solution 6 of the embodiment is a liquid gallium source, the open cavity seed crystal holder 8 is suspended at a certain depth inside the liquid gallium source under the buoyancy effect, the seed crystal 7 is also suspended in the liquid gallium source, the crystal material starts to grow, the laser light source 9 is injected into the crucible 5 from the incident window 10, and the beam passing through the beam shaping component is converged at a local point on the back of the seed crystal 7, so that the material growth rate of the sample can be changed locally.
In the present embodiment, the laser light source 9 emits ultraviolet light, and the light beam emitted by the laser light source 9 is continuous light, but in other preferred embodiments, the laser light source 9 emits infrared light, and the light beam emitted by the laser light source 9 is pulsed light, so as to accelerate the crystal growth efficiency, the light beam emitted by the laser light source 9 in the present embodiment may be kept stationary or perform a scanning motion in the cavity of the reaction kettle 1, the scanning motion may be a periodic motion scanning or a random motion scanning, the laser light source 9 may be one or more of a synchrotron radiation light source, an LD light source, an LED light source or a frequency multiplication light source, and the light intensity of the light beam emitted by the laser light source 9 may be constant or adjustable, and may be selected according to the requirement, so as to irradiate the back surface of the seed crystal 7 according to the specified requirement.
Fig. 1 shows that this embodiment further includes three sets of heating devices 4, where the three sets of heating devices are located at two sides of the crucible and the bottom of the crucible, respectively, the heating devices 4 can heat the reaction solution 6 in the crucible 5 to reach the required crystal growth temperature, the heating devices 4 are set as electromagnetic induction heating devices 4, heat conduction heating devices 4 or radio frequency heating devices 4, and the reaction kettle 1 is provided with an air inlet 2 and an air outlet 3 for introducing air and adjusting pressure, so that the pressure and the temperature in the cavity of the reaction kettle 1 reach the conditions required for growth through the heating devices 4, the air inlet 2 and the air outlet 3.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (9)
1. The utility model provides a crystal growth device that light modulation part was strengthened, includes reation kettle, laser source, the crucible of setting in reation kettle, load in crucible reaction solution and soak the seed crystal in reaction solution, reation kettle is equipped with incident window, and the light beam that laser source sent is penetrated into in the crucible through incident window, its characterized in that still includes beam shaping components and parts, beam shaping components and parts are equipped with at least one optical lens, the optical lens is arranged and is had a plurality of microstructure, the microstructure sets up to optical lens or light filter, beam shaping components and parts locate between incident window and the seed crystal, assemble the light beam in the local position of seed crystal or weaken the light beam of seed crystal local position through beam shaping components and parts.
2. The locally enhanced optical modulation crystal growth apparatus of claim 1, further comprising an open cavity seed holder, wherein the seed is mounted to the open cavity seed holder and the open cavity seed holder is suspended within the reaction solution.
3. A locally enhanced optical modulation crystal growth apparatus according to claim 2 wherein the beam shaping element is mounted in the open cavity seed holder and the beam shaping element is located above the seed.
4. A locally enhanced optical modulation crystal growth apparatus according to claim 2 wherein the open-cavity seed holder is made of a lightweight material, the lightweight material being SiC or thin-walled quartz.
5. The locally enhanced optical modulation crystal growing apparatus according to claim 1, wherein the light beam emitted by the laser light source is kept stationary or performs a scanning motion in the reaction kettle cavity, and the scanning motion is a periodic motion scanning or a random motion scanning.
6. The locally enhanced optical modulation crystal growing apparatus according to claim 5, wherein the laser light source is one or more of a synchrotron radiation light source, an LD light source, an LED light source or a frequency multiplication light source, and the light intensity of the light beam emitted from the laser light source is constant or adjustable.
7. The locally enhanced optical modulation crystal growing apparatus according to claim 5, wherein the laser light source emits ultraviolet light or infrared light, and the beam emitted from the laser light source is continuous light or pulsed light.
8. The locally enhanced optical modulation crystal growth apparatus of claim 1, further comprising a heating device for heating the reaction solution in the crucible to a desired crystal growth temperature, wherein the heating device is configured as one or more of an electromagnetic induction heating device, a heat conduction heating device, or a radio frequency heating device, and the reaction vessel is provided with an air inlet and an air outlet for introducing air and adjusting pressure.
9. The locally enhanced optical modulation crystal growth apparatus of claim 1, wherein the seed crystal is one or more of a sapphire substrate or a silicon carbide substrate, and the beam shaping element is one or more of a convex lens or a prism.
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CN109440189B true CN109440189B (en) | 2024-01-30 |
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