AU2021103774A4 - Method for Preparing GaN Crystal by Composite Flux-Temperature Gradient Technology - Google Patents
Method for Preparing GaN Crystal by Composite Flux-Temperature Gradient Technology Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 83
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 238000005516 engineering process Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 12
- 230000004907 flux Effects 0.000 claims abstract description 7
- 230000001681 protective effect Effects 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 239000011575 calcium Substances 0.000 claims description 5
- 229910052744 lithium Inorganic materials 0.000 claims description 5
- 238000005192 partition Methods 0.000 claims description 5
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 4
- 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 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- 229910052783 alkali metal Inorganic materials 0.000 claims description 4
- 150000001340 alkali metals Chemical class 0.000 claims description 4
- 229910052733 gallium Inorganic materials 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 3
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052788 barium Inorganic materials 0.000 claims description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 6
- 229910052757 nitrogen Inorganic materials 0.000 claims 3
- 238000002791 soaking Methods 0.000 claims 1
- 229910002601 GaN Inorganic materials 0.000 description 51
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 5
- 150000004767 nitrides Chemical class 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000007716 flux method Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000004377 microelectronic Methods 0.000 description 3
- 230000005693 optoelectronics Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004943 liquid phase epitaxy Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000012546 transfer Methods 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
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0632—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with gallium, indium or thallium
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for preparing GaN crystal by a composite flux-temperature
gradient technology. The method comprises the following steps. 1) In a glove box filled with
protective gas, put composite flux and metal Ga in a molar ratio of 1: 9-10: 0 into a crucible.
Put GaN crystal powder at the bottom of the crucible, and place GaN seed crystal at the upper
part of the crucible. 2) Put the crucible into a high-temperature reaction kettle and seal the
reaction kettle. Then the reaction kettle is put into a high-temperature crystal growth furnace
with negative temperature gradient. Raise the temperature to around 600-900°C, and keep the
pressure at 0.5-10.0MPa. The temperature gradient range is 0-70°C/cm, and the rotation speed
of the reaction kettle is 0-85rpm. The growth temperature was maintained for some time. After
the growth is finished, cool the reaction kettle to room temperature naturally, and then open it
and take out the crucible. Treat the product in the crucible to finally obtain GaN crystal.
Description
Method for Preparing GaN Crystal by Composite Flux-Temperature Gradient
Technology
The invention belongs to the technical field of crystal growth, and relates to a composite
flux-temperature gradient technology for growing GaN crystal, particularly to GaN
crystal grown by composite flux-temperature gradient technology.
With the continuous development of modern science and technology, the requirements of
various working systems for the performance of microelectronic devices and
optoelectronic devices are constantly improving. However, due to the limitation of
intrinsic physical properties of materials, the performance improvement of traditional Si
based devices and GaAs-based devices through structural optimizationwas very difficult.
Therefore, it is very urgent to find new semiconductor materials to make devices. GaN is
the representative of a new wide band gap nitride semiconductor material. It has excellent
properties such as high breakdown voltage, wide band gap, high thermal conductivity,
high electron saturation drift speed, strong radiation resistance and good chemical
stability. Therefore it has become an excellent material for making new generation
microelectronic devices and optoelectronic devices. GaN also has a very broad
application prospect in weapons and equipment, aerospace, 5G network communication,
lighting, new energy vehicles and automatic driving. In addition, nitride-based
microelectronic devices and optoelectronic devices have very high energy conversion
efficiency. The use of such devices can improve the use efficiency of electric energy, reduce the burning of fossil fuels and the emission of related pollutants, help alleviate and solve the energy problems facing the current society. They can also improve the living environment on which we live, which is of great significance for building an environment-friendly society. Therefore, GaN materials and related devices have been extensively and deeply studied. Among them, Shuji Nakamura, Hiroshi Amano and
Isamu Akasaki won the Nobel Prize in Physics in 2014 for successfully fabricating blue
light emitting diode devices on GaN thin films.
At present, nitride-based semiconductor devices are still in the initial stage of research.
Except for GaN-based light-emitting diode devices, the commercial performance of other
devices is far below the laboratory level in the same period. There are still many
scientific and technical problems to be solved in such fields as reliability, fabrication
technology and device performance. Among them, the lack of high crystal quality GaN
substrate is one of the most important technical bottlenecks hindering the development of
devices. At present, GaN devices mainly use sapphire single crystal and silicon single
crystal as substrates. However, their lattice constants and thermal expansion coefficients
are quite different. This will lead to a large number of dislocation defects in the device,
which will seriously affect the performance and life of the device. In addition, some high
performance GaN devices use SiC as the substrate. This can improve the performance of
the devices relatively, but the SiC substrate has the defect of high price. The most ideal
substrate for manufacturing nitride-based semiconductor devices is the corresponding
nitride single crystal. It can solve the crystal defect problem caused by lattice mismatch
and thermal conductivity mismatch. Meanwhile, it can reduce the tedious process in the
manufacturing process of devices and improve the yield of devices. In order to grow GaN crystal, several methods were investigated. Among them, Na flux method has the advantages of mild growth conditions, low cost, high crystal quality and fast growth rate.
In addition, experiments show that dislocation density in GaN crystal will decrease with
the increase of growth thickness. Therefore, it has the potential to realize large-size and
high-quality GaN crystal growth in industry. At present, the flux method mainly uses
liquid phase epitaxy technology to grow gallium nitride crystals. However, this
technology has the defects of poor stability and limited growth time, so it is difficult to
obtain large size gallium nitride crystals with high quality. According to the invention, a
technology for growing GaN crystal by composite flux-temperature gradient method is
designed. N sources and Ga sources are provided for crystal growth through GaN
powder, so that difficulties encountered in GaN crystal growth can be overcome.
The purpose of the present invention is to overcome the above technical problems and
provide a method for preparing GaN crystal by composite flux-temperature gradient
technology, so as to provide a stable growth environment for crystal growth.
The invention is realized by the following technical scheme.
The method for preparing GaN crystal by composite flux-temperature gradient
technology comprises the following steps.
1) In a glove box filled with protective gas, the composite flux and metal gallium are put
into a crucible according to the molar ratio of (1:9)(10:0) and mixed uniformly. GaN
crystal powder is placed at the bottom of the crucible, a partition plate with holes is
placed, and a seed crystal is placed at the upper part of the crucible.
2) The crucible filled with flux, metal gallium, GaN powder, partition plate and GaN
seed crystal is put into a high-temperature reaction kettle. Seal the reaction kettle, put
it into a crystal growth equipment, raise the temperature to 600-900°C.Keep the
pressure at 0.5-10.OMpa, and control the temperature gradient at 0-70°C/cm.
3) Start a rotating device in crystal growth equipment. Rotate the crucible at a speed of 0
-85 rpm, naturally cool to room temperature after the growth is finished. Take out the
crucible, and treat the GaN crystal in the crucible. Finally obtain pure GaN crystal.
The treatment of the grown product is as follows. The growth product in the crucible was
soaked in the alcohol, cold water and hydrochloric acid in turn. After the growth residues
was removed in the crucible. Taking out the top GaN crystal, and then cleaning and
drying the GaN crystal.
The crystal growth equipment comprises a high-temperature reaction kettle, a heating
device and a rotating device.
The method for preparing GaN crystal by composite flux-temperature gradient
technology according to Claim 1 is characterized in that the crucible adopts molybdenum
crucible, alumina crucible and boron nitride crucible. The shape of the crucible is
cylindrical.
The composite fluxing agent comprises one or more of alkali metal and alkaline earth
metal. The alkali metal is one or two of sodium and lithium. The alkaline earth metal is
one or more of barium, strontium, calcium and magnesium.
The protective gas is inert gas.
The method for preparing GaN crystal by composite flux-temperature gradient
technology according to Claim 1 is characterized in that the high-temperature crystal
growth equipment comprises a high-temperature furnace, a rotating device and a lifting
device. The set of devices can provide a temperature range of 600-900°C, a temperature
gradient range of 0-70°C/cm and a rotation speed range of 0-85rpm.
Compared with the prior art, the invention has the following beneficial technical effects.
Technical effects brought by the invention include the following aspects.
1. Temperature gradient technology was introduced into the composite flux method to
form a closed GaN crystal growth system. This improves the stability of GaN crystal
growth.
2. In the composite flux method, GaN powder is used as the raw material for crystal
growth. This enhances the continuity of crystal growth and increases the time for
crystal growth.
3. It is convenient to adjust the supersaturation of solution and inhibit the growth of
GaN polycrystal through temperature gradient. Therefore high-quality crystal with
smooth and flat crystal surface can be obtained.
Figure 1 A main process flowchart of GaN crystal grown by the composite flux
temperature gradient technology provided by the present invention
Figure 2 A structural diagram of crystal growth equipment, wherein, 1-high temperature
furnace, 2-upper heater, 3-lower heater, 4-rotary lifting controller, 5-rotary lifting shaft,
6-rotary platform and 7-reaction kettle
Figure 3 A schematic diagram of the growth process of GaN crystal grown by the
composite flux-temperature gradient technology provided by the present invention
Figure 4 An optical photograph of the Embodiment 1 of GaN crystal grown by the
composite flux-temperature gradient technology provided by the present invention
Figure 5 An optical photograph of the Embodiment 3 of GaN crystal grown by the
composite flux-temperature gradient technology provided by the present invention
The invention will be further described in detail with reference to the attached
embodiments.
Embodiment 1:
Referring to the process in Figure 1 and the schematic diagram of crystal growth
equipment in Figure 2.
The method for preparing GaN crystal by composite flux-temperature gradient
technology comprises the following steps.
1) In a glove box filled with inert gas, 8.006g of metal Ga, 13.055g of metal Na, 0.924g
of metal calcium, 0.12g of graphite powder and 0.245g of metal lithium are put into a
crucible and mixed uniformly. GaN crystal powder is placed at the bottom of the crucible, a partition plate with holes is placed, and a seed crystal is placed at the upper part of the crucible.
2) Put the crucible into a high-temperature reaction kettle and seal the reaction kettle.
Transfer the high-temperature reaction kettle to the rotating platform in the high
temperature furnace, and adjust the rotation speed of the rotating platform to 5
revolutions per minute. Control the furnace temperature to make the temperature near
the polycrystal at the bottom of the solution around 850°C. Control the N2 pressure at
3.2MPa. The temperature near the top seed crystal is around 810°C, and the
temperature is kept for 200h.
3) After growth, naturally cool to room temperature, open the reaction kettle and take
out the crucible. Soak the grown product in the crucible in alcohol, cold water and
hydrochloric acid in turn. Remove the growth residues in the crucible. Take out the
top GaN crystal, and then clean and dry the GaN crystal. The gallium nitride crystal
with the size of 3Omm*8mm*1mm is grown.
Embodiment 2:
With reference to Embodiment 1, 6.035g of metal sodium, 4.034g of metal Ga, 0.222g of
metal calcium and 0.061g of metal lithium are put into a metal molybdenum crucible in
an argon glove box. Then the gallium nitride powder is put into the bottom of the
solution, and the single crystal gallium nitride seed crystal is placed on the top of the
solution. The crucible is transferred into a high-temperature corrosion-resistant reaction
kettle and is fixed. The furnace temperature is controlled to make the temperature near
the GaN powder at the bottom of the solution around 850°C. The N2 pressure is controlled at 2.5MPa. The temperature near the top seed crystal is around 790°C. The running time of growth is 100h. The impeller rotation speed is 0 revolutions per minute.
The gallium nitride crystal with the size of 5mm*15mm*40[m is grown.
Embodiment 3:
With reference to Example 1, 13.03g of metal sodium, 8.03g of metal Ga, 0.463g of
metal calcium, 0.122g of graphite powder and 0.123g of metal lithium are put into a
metal molybdenum crucible in an argon glove box. Then the gallium nitride powder is
put into the bottom of the solution, and the single crystal gallium nitride seed crystal is
placed on the top of the solution. The crucible is transferred into a high-temperature
corrosion-resistant reaction kettle and is fixed. The furnace temperature is controlled to
make the temperature near the GaN powder at the bottom of the solution around 850°C
. The N2 pressure is controlled at 3.OMPa. The temperature near the top seed crystal is
around 790°C. The running time of growth is 150h. The impeller rotates at a speed of 5
revolutions per minute. The gallium nitride crystal with the size of 30mm*Omm*2.5mm
is grown.
Claims (7)
1. The method for preparing GaN crystal by composite flux-temperature gradient
technology is characterized by comprising the following steps:
1) in a glove box filled with inert protective gas, the composite flux and metal gallium
are put into a crucible in a molar ratio of 1: 9-10: 0 for uniform mixing;_GaN crystal
powder is placed at the bottom of the crucible, a partition plate with holes is placed,
and a seed crystal is placed in the solution area at the upper part of the crucible;
2) put the crucible filled with flux, metal gallium, GaN powder, partition plate and GaN
seed crystal into a high-temperature reaction kettle and seal the reaction kettle; and
then put the reaction kettle into high temperature crystal growth equipment with
negative temperature gradient; raise the temperature to around 600-900°C, and keep
the growth gas pressure at 0.5-10.MPa; temperature gradient range is 0-70°C/cm;
rotation speed of the reaction kettle is between 0 and 0-85rpm; the growth
temperature was maintained for some time;
3) After the growth is finished, cool the reaction kettle to room temperature, and then
open it and take out the crucible; treat the product in the crucible to finally obtain
GaN crystal.
2. The method for preparing GaN crystal by composite flux-temperature gradient
technology according to Claim 1 is characterized in that the product treatment
comprises soaking the growth product in the crucible in alcohol, cold water and
hydrochloric acid in turn, removing the growth residue in the crucible, taking out the top GaN crystal, and then cleaning and drying the GaN crystal.
3. The method for preparing GaN crystal by composite flux-temperature gradient
technology according to Claim 1 is characterized in that the crucible adopts
molybdenum crucible, alumina crucible and boron nitride crucible, and the shape of
the crucible is cylindrical.
4. The method for preparing GaN crystal by composite flux-temperature gradient
technology according to Claim 1 is characterized in that the composite flux comprises
one or more of alkali metal and alkaline earth metal, wherein the alkali metal is one or
two of sodium and lithium, and the alkaline earth metal is one or more of barium,
strontium, calcium and magnesium.
5. The method for preparing GaN crystal by composite flux-temperature gradient
technology according to Claim 1 is characterized in that the protective gas is inert gas
and nitrogen.
6. The method for preparing GaN crystal by composite flux-temperature gradient
technology according to Claim 1 is characterized in that the high-temperature crystal
growth equipment comprises a high-temperature furnace, a rotating device and a
lifting device; the equipment can provide a temperature range of 600-900'C, a
pressure range of 0.5-10.0MPa, a temperature gradient range of 0-70'C/cm and a
rotation speed range of 0-85rpm.
7. The method for preparing GaN crystal by composite flux-temperature gradient
technology according to Claim 1 is characterized in that the growth gas is nitrogen or a mixed gas of nitrogen and inert gas.
FIGURES 1/5
Figure 1
3
5 6 7
4 2/5
Figure 2
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| Application Number | Priority Date | Filing Date | Title |
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| AU2021103774A AU2021103774A4 (en) | 2021-07-01 | 2021-07-01 | Method for Preparing GaN Crystal by Composite Flux-Temperature Gradient Technology |
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ID=77369630
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2021
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