CN106757359B - Adjusting reaction kettle for crystal growth and control method thereof - Google Patents
Adjusting reaction kettle for crystal growth and control method thereof Download PDFInfo
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- CN106757359B CN106757359B CN201611110488.9A CN201611110488A CN106757359B CN 106757359 B CN106757359 B CN 106757359B CN 201611110488 A CN201611110488 A CN 201611110488A CN 106757359 B CN106757359 B CN 106757359B
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- crucible
- crystal growth
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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
- C30B29/406—Gallium nitride
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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
- 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
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- Crystallography & Structural Chemistry (AREA)
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a regulating reaction kettle for crystal growth and a control method thereof, and the regulating reaction kettle comprises a kettle body and a heater arranged in the kettle body, wherein at least one crucible for crystal growth and one reactant solution regulating crucible are arranged in the kettle body, the crucible for crystal growth and the reactant solution regulating crucible are connected through a communication pipeline filled with reactant solution, a lifting movement control mechanism is arranged on the kettle body, and the lifting movement control mechanism is respectively connected with the crucible for crystal growth and the reactant solution regulating crucible to drive the crucible for crystal growth and the reactant solution regulating crucible to ascend or descend. The invention realizes the circulating flow of the reactant liquid between the two crucibles, and the flow can further promote the fluctuation of the liquid level of the reactant, enhance the further mixing of the reactant liquid and the nitrogen and improve the growth rate and the quality of the material.
Description
Technical Field
The invention belongs to the technical field of semiconductor, in particular to a preparation technology of third generation III group nitride semiconductor, and specifically relates to a regulating reaction kettle for crystal growth and a control method thereof.
Background
Gallium nitride (GaN) as a third generation group III nitride semiconductor belongs to wide band gap semiconductor materials (3.4 eV), and thick film GaN as a homoepitaxial substrate plays a great promoting role in improving the performance of devices in various application fields such as photoelectronic devices. The current development methods of GaN crystal thick films mainly include Metal Organic Chemical Vapor Deposition (MOCVD), Hydride Vapor Phase Epitaxy (HVPE), Molecular Beam Epitaxy (MBE), and the like. The dislocation density of the gallium nitride crystal obtained by the vapor phase growth method is high, and the traditional liquid phase pulling method for preparing the silicon (Si) and gallium arsenide (GaAs) single crystal substrate is difficult to be used for growing the GaN substrate material. Therefore, it has been proposed that a nitride crystal such as GaN can be grown in a liquid phase under relatively mild conditions using an alkali metal such as sodium (Na) as a solvent. In the GaN crystal growing by the liquid phase method, the crystal growth quality and speed are greatly influenced by the nitrogen concentration in the Ga-Na solution on the surface of the seed crystal template, at present, methods such as rotation, swing, stirring and the like are adopted to promote the mixing of nitrogen and a Ga source, but the methods can not make the whole reaction solution move uniformly, and are not beneficial to obtaining the GaN crystal material with uniform quality.
Disclosure of Invention
The invention aims to provide a regulating reaction kettle for crystal growth and a control method thereof, which are convenient to control and operate.
In order to solve the technical problems, the invention adopts the following technical scheme:
the utility model provides an adjust reation kettle for crystal growth, includes the cauldron body and establishes the internal heater at the cauldron, the internal at least of cauldron sets up a crucible for crystal growth and a reactant solution adjustment crucible, and this crucible for crystal growth and reactant solution adjustment crucible are connected through the intercommunication pipeline that is full of reactant solution, is equipped with lift movement control mechanism on the cauldron body, and this lift movement control mechanism is connected with crucible for crystal growth and reactant solution adjustment crucible respectively, drives this crucible for crystal growth and reactant solution adjustment crucible and rises or descend.
At least one communication pipeline is arranged.
The communicating pipe is made of quartz, ceramics, high-purity copper pipes or stainless steel pipe materials.
Heaters are arranged on the side surface and the bottom surface of the crucible for crystal growth and the reactant solution adjusting crucible.
The number of the crucibles for crystal growth and the number of the reactant solution adjusting crucibles may be the same or different.
The heater is an infrared heater, a resistance heater or a radio frequency heater.
A method of controlling a conditioning reactor for crystal growth, comprising the steps of:
in an initial state, placing a seed crystal template and filling a reactant solution in a crucible for crystal growth, filling the reactant solution in a reactant solution adjusting crucible, and enabling the liquid level of the crucible for crystal growth and the liquid level of the reactant solution adjusting crucible to be located at the same height;
starting a heater to heat and raise the temperature, and introducing nitrogen into the kettle body;
in the heating and temperature rising process, adjusting the relative height of the crucible for crystal growth and the reactant solution adjusting crucible, so that the reactant solutions in the crucible for crystal growth and the reactant solution adjusting crucible flow mutually through a communicating pipeline until the crystal growth is finished;
after the crystal growth is finished, the crucible for crystal growth and the reactant solution adjusting crucible are reset, and the same height of the liquid level is maintained again.
When the relative height of the crucible for crystal growth and the crucible for reactant solution adjustment is controlled, the crucible for crystal growth is kept still, and the crucible for reactant solution adjustment is made to ascend and descend; or keeping the reactant solution to adjust the crucible to be still, so that the crucible for crystal growth is lifted and lowered; or the crucible for crystal growth and the crucible for reactant solution adjustment are raised and lowered, respectively.
The crucible for crystal growth and/or the reactant solution adjusting crucible move in a continuous motion, a periodic motion or an intermittent motion when ascending and descending.
In the heating and temperature rising process, the temperature of the crucible for crystal growth and the temperature of the crucible for reactant solution adjustment are the same or different.
The invention adjusts the rising and falling of the crucible by controlling the crucible for crystal growth and/or reactant solution, so that the reactant solution between the crucible and the crucible flows mutually, the fluctuation of the liquid level of the reactant can be further promoted, the further mixing of the reactant liquid and nitrogen is enhanced, and the growth rate and the quality of the material are improved.
Drawings
FIG. 1 is a schematic view showing a state in which a crucible for crystal growth and a reactant solution adjusting crucible of the present invention are on the same horizontal plane;
FIG. 2 is a schematic view showing a state in which a crucible for crystal growth and a reactant solution adjusting crucible of the present invention are located on different horizontal planes;
FIG. 3 is a schematic top view of a plurality of crystal growth crucibles and a reactant solution adjusting crucible according to the present invention.
Reference numerals:
1-crucible for crystal growth; 2-adjusting the crucible with reactant solution; 30 a reactant solution in a crucible for crystal growth; 31-adjusting the reactant solution in the crucible by the reactant solution; 10-kettle body; 20-a heater; 40-communication pipeline.
Detailed Description
In order to facilitate understanding of the present invention, a description of the present invention is provided below with reference to the accompanying drawings.
As shown in attached figures 1 and 2, the invention discloses a regulating reaction kettle for crystal growth, which comprises a kettle body 10 and a heater 20 arranged in the kettle body 10, wherein at least one crucible 1 for crystal growth and one reactant solution regulating crucible 2 are arranged in the kettle body 10, the crucible 1 for crystal growth and the reactant solution regulating crucible 2 are connected through a communication pipeline 40 filled with reactant solution, and the kettle body 10 is provided with a lifting movement control mechanism which is respectively connected with the crucible 1 for crystal growth and the reactant solution regulating crucible 2 to drive the crucible for crystal growth and the reactant solution regulating crucible to ascend or descend. The lifting movement control mechanism can be provided with a cylinder or a motor, and is connected with the cylinder or the motor through a connecting rod, and the connecting rod is connected with a crucible for crystal growth and a reactant solution adjusting crucible, so that the lifting movement is driven. Or other forms of lifting movement control mechanisms, as long as the lifting movement can be realized, which are not listed here.
The number of the communicating pipes 40 is at least one, and a plurality of communicating pipes may be provided, and the crucible for crystal growth and the crucible for reactant solution adjustment are connected by the plurality of communicating pipes, thereby realizing faster flow of the reactant solution. The communicating pipe is made of quartz, ceramics, high-purity copper pipes or stainless steel pipe materials.
In the whole growth process, the crucible 1 for crystal growth and the crucible 2 for reactant solution adjustment are in alternate ascending and descending circular motion to realize circulation of reactant solutions among each other, each circulation can promote the flow of the reactant solutions, fresh nitrogen continuously enters liquid gallium through the change of the liquid level in the flow, the nitrogen is supplemented into unsaturated liquid which consumes the nitrogen, and the reaction is smoothly carried out. When the crucible 1 for crystal growth is higher than the reactant solution adjusting crucible 2, the reactant solution 30 in the crucible 1 for crystal growth flows to the reactant solution adjusting crucible 2; when the reactant solution adjusting crucible 2 is higher than the crystal growth crucible 1, the reactant solution 31 of the reactant solution adjusting crucible 2 flows toward the crystal growth crucible 1, and the reactant solutions flow each other, thereby facilitating the promotion of the high-speed growth of the gallium nitride crystal.
Further, the number of the crucible for crystal growth and the number of the reactant solution adjusting crucibles may be the same or different. Further, as shown in FIG. 3, two crystal growth crucibles 1 and two reactant solution adjustment crucibles 2 are provided, and the two crystal growth crucibles 1 and the two reactant solution adjustment crucibles 2 are connected two by two via a communication pipe 40.
In addition, the invention also discloses a control method of the regulating reaction kettle for crystal growth, which comprises the following steps:
s1, placing a seed crystal template and a reactant solution in the crystal growth crucible in an initial state, and filling the reactant solution in the reactant solution adjustment crucible, wherein the liquid level of the crystal growth crucible and the liquid level of the reactant solution adjustment crucible are at the same height. The reactant solutions of the two crucibles do not flow into each other at this time.
And S2, starting the heater to heat and raise the temperature, and introducing nitrogen into the kettle body. The temperature of the crucible for crystal growth and the temperature of the crucible for adjusting the reactant solution are the same or different.
S3, in the heating and temperature rising process, adjusting the relative height of the crucible for crystal growth and the reactant solution adjusting crucible, so that the reactant solutions in the crucible for crystal growth and the reactant solution adjusting crucible flow through the communicating pipeline until the crystal growth is finished;
and S4, after the crystal growth is finished, resetting the crucible for crystal growth and the reactant solution adjusting crucible, and keeping the liquid level at the same height again.
When the relative height of the crucible for crystal growth and the crucible for reactant solution adjustment is controlled, the crucible for crystal growth is kept still, and the crucible for reactant solution adjustment is made to ascend and descend; or keeping the reactant solution to adjust the crucible to be still, so that the crucible for crystal growth is lifted and lowered; or the crucible for crystal growth and the crucible for reactant solution adjustment are raised and lowered, respectively.
The present invention is described in detail and completely by the technical solutions in the above embodiments, and it is obvious that the described embodiments are a part of embodiments of the present invention, but not all of them. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. The utility model provides an adjust reation kettle for crystal growth, includes the cauldron body and establishes the internal heater in cauldron, its characterized in that, the internal crucible and the reactant solution adjustment crucible of using of setting up a crystal at least of cauldron, this crucible and reactant solution adjustment crucible for crystal growth are connected through the intercommunication pipeline that is full of reactant solution, are equipped with lift movement control mechanism on the cauldron body, and this lift movement control mechanism is connected with crucible and reactant solution adjustment crucible for crystal growth respectively, drives this crucible and reactant solution adjustment crucible for crystal growth and rises or descend.
2. The conditioning reactor for crystal growth as defined in claim 1, wherein at least one of said communication pipes is provided.
3. The conditioning reactor for crystal growth of claim 2, wherein the communicating tube is made of quartz, ceramic, high purity copper tube or stainless steel tube material.
4. A conditioning reactor for crystal growth as defined in claim 3 wherein the crucible for crystal growth and the reactant solution conditioning crucible are provided with heaters on both side surfaces and bottom surface thereof.
5. The conditioning reactor for crystal growth as set forth in claim 4, wherein the number of the crucibles for crystal growth and the number of the reactant solution adjusting crucibles are the same or different.
6. A conditioning reactor for crystal growth as defined in claim 5, wherein the heater is an infrared heater, a resistance heater, or a radio frequency heater.
7. A method of controlling a conditioning reactor for crystal growth according to any one of claims 1 to 6, comprising the steps of:
in an initial state, placing a seed crystal template and filling a reactant solution in a crucible for crystal growth, filling the reactant solution in a reactant solution adjusting crucible, and enabling the liquid level of the crucible for crystal growth and the liquid level of the reactant solution adjusting crucible to be located at the same height;
starting a heater to heat and raise the temperature, and introducing nitrogen into the kettle body;
in the heating and temperature rising process, adjusting the relative height of the crucible for crystal growth and the reactant solution adjusting crucible, so that the reactant solutions in the crucible for crystal growth and the reactant solution adjusting crucible flow mutually through a communicating pipeline until the crystal growth is finished;
after the crystal growth is finished, the crucible for crystal growth and the reactant solution adjusting crucible are reset, and the same height of the liquid level is maintained again.
8. The control method for a conditioning reactor for crystal growth as set forth in claim 7, characterized in that, while controlling the relative heights of the crystal growth crucible and the reactant solution conditioning crucible, the reactant solution conditioning crucible is raised and lowered while keeping the crystal growth crucible stationary; or keeping the reactant solution to adjust the crucible to be still, so that the crucible for crystal growth is lifted and lowered; or the crucible for crystal growth and the crucible for reactant solution adjustment are raised and lowered, respectively.
9. The control method of a conditioning reactor for crystal growth as set forth in claim 7, wherein the crucible for crystal growth and/or the reactant solution conditioning crucible is moved in a continuous motion, a periodic motion or an intermittent motion while being raised and lowered.
10. The control method of a conditioning reactor for crystal growth as set forth in claim 7, wherein the temperature of the crucible for crystal growth and the temperature of the reactant solution conditioning crucible are the same or different during the heating and raising process.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611110488.9A CN106757359B (en) | 2016-12-06 | 2016-12-06 | Adjusting reaction kettle for crystal growth and control method thereof |
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| CN201611110488.9A CN106757359B (en) | 2016-12-06 | 2016-12-06 | Adjusting reaction kettle for crystal growth and control method thereof |
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| CN106757359B true CN106757359B (en) | 2020-10-27 |
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| CN109440189B (en) * | 2018-12-27 | 2024-01-30 | 北京大学东莞光电研究院 | Crystal growth device with locally reinforced light modulation |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007122949A1 (en) * | 2006-03-23 | 2007-11-01 | Ngk Insulators, Ltd. | Apparatus for producing nitride single crystal |
| CN103526282A (en) * | 2013-10-22 | 2014-01-22 | 北京大学东莞光电研究院 | Device and method for growing nitride single-crystal material |
| CN105986313A (en) * | 2015-01-31 | 2016-10-05 | 东莞市中镓半导体科技有限公司 | Gallium source automatic supply and recovery device |
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- 2016-12-06 CN CN201611110488.9A patent/CN106757359B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007122949A1 (en) * | 2006-03-23 | 2007-11-01 | Ngk Insulators, Ltd. | Apparatus for producing nitride single crystal |
| CN103526282A (en) * | 2013-10-22 | 2014-01-22 | 北京大学东莞光电研究院 | Device and method for growing nitride single-crystal material |
| CN105986313A (en) * | 2015-01-31 | 2016-10-05 | 东莞市中镓半导体科技有限公司 | Gallium source automatic supply and recovery device |
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