CN106757359A - A kind of regulation reactor and its control method for crystal growth - Google Patents
A kind of regulation reactor and its control method for crystal growth Download PDFInfo
- Publication number
- CN106757359A CN106757359A CN201611110488.9A CN201611110488A CN106757359A CN 106757359 A CN106757359 A CN 106757359A CN 201611110488 A CN201611110488 A CN 201611110488A CN 106757359 A CN106757359 A CN 106757359A
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- China
- Prior art keywords
- crucible
- crystal growth
- reactant solution
- adjustment
- reactant
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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
-
- 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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- 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 discloses a kind of regulation reactor and its control method for crystal growth, including kettle and the heater being located in kettle, at least provided with a crucible for crystal growth and a reactant solution adjustment crucible in the kettle, the crucible for crystal growth and reactant solution adjustment crucible are connected by the connecting pipeline full of reactant solution, kettle is provided with lifting moving controlling organization, the lifting moving controlling organization is connected with crucible for crystal growth and reactant solution adjustment crucible respectively, the crucible for crystal growth and reactant solution adjustment crucible is driven to rise or fall.The present invention realizes that reactant liquid is circulated between two crucibles, and the flowing can further promote the fluctuation of reactant liquid level, and intensified response thing liquid body mixes with the further of nitrogen, improves Material growth speed and quality.
Description
Technical field
The invention belongs to semiconductor, the especially preparing technical field of the group-III nitride semiconductor of the third generation III, specifically
It is a kind of regulation reactor and its control method for crystal growth.
Background technology
Gallium nitride (GaN) belongs to wide bandgap semiconductor materials (~3.4eV) as the group-III nitride semiconductor of the third generation III,
In many application fields such as opto-electronic device, thick film GaN will be improved to device performance as homoepitaxy substrate and play huge
Impetus.The method of production of current GaN crystal thick film, mainly Metalorganic Chemical Vapor Deposition (MOCVD), hydrogenation
Thing vapour phase epitaxy method (HVPE), molecular beam epitaxy (MBE) etc..The gallium nitride dislocation density that vapor growth method is obtained compared with
Greatly, traditional prepare silicon (Si), the liquid phase czochralski method of GaAs (GaAs) single crystalline substrate are difficult to grow GaN substrate material
Material.Therefore, it has been proposed that using alkali metal such as sodium (Na) as solvent, can under the conditions of comparatively gentle the nitrogen such as liquid growth GaN
Compound crystal.In liquid phase method growing gan crystal, crystal growth quality and speed will be by crystal seed reticle surface Ga-Na solution
Middle nitrogen concentration material impact, has using rotation, waves and stir etc. the mixing in method promotion nitrogen and Ga sources at present, but these
Method cannot all make reaction solution integrally do homogeneous motion, be unfavorable for obtaining the homogeneous GaN crystal material of quality.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of is easy to the regulation for crystal growth for controlling and operating anti-
Answer kettle and its control method.
In order to solve the above-mentioned technical problem, the present invention takes following technical scheme：
A kind of regulation reactor for crystal growth, including kettle and the heater being located in kettle, in the kettle
At least provided with a crucible for crystal growth and a reactant solution adjustment crucible, the crucible for crystal growth and reactant are molten
Liquid is adjusted crucible and is connected by the connecting pipeline full of reactant solution, and kettle is provided with lifting moving controlling organization, the lifting
Moving control mechanism is connected with crucible for crystal growth and reactant solution adjustment crucible respectively, drives the crucible for crystal growth
Risen or fallen with reactant solution adjustment crucible.
The connecting pipeline is at least provided with one.
The connecting pipeline is made up of quartzy, ceramic, high-purity copper pipe or stainless steel tube material.
The side and bottom surface of the crucible for crystal growth and reactant solution adjustment crucible are all provided with having heaters.
The quantity of the crucible for crystal growth and reactant solution adjustment crucible is identical or difference.
The heater is infrared heater, resistance heater or radio heater.
A kind of control method of regulation reactor for crystal growth, comprises the following steps：
Under original state, crystal seed template and filling reactant solution are placed in crucible for crystal growth, in reactant solution
Filling reactant solution in adjustment crucible, the liquid level of liquid level and reactant solution the adjustment crucible of crucible for crystal growth is positioned at same
One height；
Starting heater carries out heat temperature raising, while introducing nitrogen toward kettle is interior；
In heating up process, the relative altitude of adjustment crucible for crystal growth and reactant solution adjustment crucible makes
Reactant solution in crucible for crystal growth and reactant solution adjustment crucible mutually flows through connecting pipeline, until crystal life
It is long to complete；
After the completion of crystal growth, crucible for crystal growth and reactant solution adjustment crucible is resetted, liquid level is kept again
Identical is highly.
When crucible for crystal growth is controlled and reactant solution adjusts the relative altitude of crucible, crystal growth earthenware is kept
Crucible transfixion, makes reactant solution adjust crucible raising and lowering；Or keep reactant solution to adjust crucible transfixion,
Make crucible for crystal growth raising and lowering；Or crucible for crystal growth and reactant solution adjustment crucible rise respectively and under
Drop.
The crucible for crystal growth and/or reactant solution adjust crucible in raising and lowering, continuously to move, week
Phase is moved or the mode of intermittent movement is moved.
In heating up process, the temperature of crucible for crystal growth and reactant solution adjustment crucible is identical or not phase
Together.
The present invention adjusts the raising and lowering of crucible by controlling crucible for crystal growth and/or reactant solution so that
Reactant solution between the two mutually flows, and can further promote the fluctuation of reactant liquid level, intensified response thing liquid body and nitrogen
The further mixing of gas, improves Material growth speed and quality.
Brief description of the drawings
Accompanying drawing 1 is that crucible for crystal growth of the present invention and reactant solution state of the adjustment crucible in same level are shown
It is intended to；
Accompanying drawing 2 is that crucible for crystal growth of the present invention and reactant solution state of the adjustment crucible in different level are shown
It is intended to；
The schematic top plan view of accompanying drawing 3 multiple crucible for crystal growth and reactant solution adjustment crucible for the present invention is set.
Reference：
1- crucible for crystal growth；2- reactant solutions adjust crucible；Reactant solution in 30 crucible for crystal growth；
Reactant solution in 31- reactant solutions adjustment crucible；10- kettlies；20- heaters；40- connecting pipelines.
Specific embodiment
For the ease of the understanding of those skilled in the art, make the description of a step to the present invention below in conjunction with the accompanying drawings.
As shown in figure 1 and 2, present invention is disclosed a kind of regulation reactor for crystal growth, including the He of kettle 10
It is located at molten at least provided with a crucible for crystal growth 1 and a reactant in the heater 20 in kettle 10, the kettle 10
Liquid adjusts crucible 2, and the crucible for crystal growth 1 and reactant solution adjust crucible 2 by the communicating pipe full of reactant solution
Road 40 connects, and kettle 10 is provided with lifting moving controlling organization, the lifting moving controlling organization respectively with crucible for crystal growth 1
Connected with reactant solution adjustment crucible 2, drive the crucible for crystal growth and reactant solution adjustment crucible to rise or fall.
The lifting moving controlling organization can set a cylinder or motor, by connecting rod and cylinder or motor connection, and even
Bar is connected with crucible for crystal growth and reactant solution adjustment crucible, so as to drive elevating movement.Or the liter of other forms
Drop moving control mechanism, as long as lifting moving can be realized, will not enumerate herein.
Connecting pipeline 40 is settable a plurality of at least provided with one, and crucible for crystal growth and reactant solution adjust crucible
Between connected by a plurality of connecting pipeline, realize faster reactant solution flowing.Connecting pipeline is by quartzy, ceramic, high-purity
Copper pipe or stainless steel tube material are made.
The side and bottom surface of crucible for crystal growth 1 and reactant solution adjustment crucible 2 are all provided with having heaters 20.The heating
Device be infrared heater, resistance heater or radio heater, or other modes heater.
In whole growth course, crucible for crystal growth 1 and reactant solution adjustment crucible 2 are by alternately rise and fall
Shuttling movement, realize reactant solution in circulation to each other, circulating can all promote the flowing of reactant solution each time, and
By the change of liquid level in flowing, realize that fresh nitrogen constantly enters liquid-gallium, to the unsaturation liquid for having consumed nitrogen
Nitrogen is supplemented in body, is reacted smooth.When crucible for crystal growth 1 adjusts crucible 2 higher than reactant solution, crystal
Reactant solution 30 in growth crucible 1 flows to reactant solution adjustment crucible 2；When reactant solution adjustment crucible 2 is higher than
During crucible for crystal growth 1, the reactant solution 31 of reactant solution adjustment crucible 2 flows to crucible for crystal growth 1, realizes anti-
The flowing each other of thing solution is answered, so as to may advantageously facilitate gallium nitride high-speed rapid growth.
Additionally, the quantity of crucible for crystal growth and reactant solution adjustment crucible is identical or difference.And, such as accompanying drawing
Shown in 3, two crucible for crystal growth 1 and two reactant solution adjustment crucibles 2, two crucible for crystal growth 1 are set
It is connected two-by-two by connecting pipeline 40 with two reactant solution adjustment crucibles 2.
In addition, present invention further teaches a kind of control method of the regulation reactor for crystal growth, including following step
Suddenly：
S1, under original state, crystal seed template and filling reactant solution is placed in crucible for crystal growth, molten in reactant
Filling reactant solution in liquid adjustment crucible, the liquid level of liquid level and reactant solution the adjustment crucible of crucible for crystal growth is located at
Sustained height.Now two reactant solutions of crucible will not mutually flow.
S2, starting heater carries out heat temperature raising, while introducing nitrogen toward kettle is interior.Crucible for crystal growth and reactant
The temperature of solution adjustment crucible is identical or differs.
S3, in heating up process, the relative altitude of adjustment crucible for crystal growth and reactant solution adjustment crucible,
The reactant solution in crucible for crystal growth and reactant solution adjustment crucible is set mutually to be flowed through connecting pipeline, until crystal
Growth is completed；
S4, after the completion of crystal growth, makes crucible for crystal growth and reactant solution adjustment crucible reset, and liquid is kept again
Face identical is highly.
When crucible for crystal growth is controlled and reactant solution adjusts the relative altitude of crucible, crystal growth earthenware is kept
Crucible transfixion, makes reactant solution adjust crucible raising and lowering；Or keep reactant solution to adjust crucible transfixion,
Make crucible for crystal growth raising and lowering；Or crucible for crystal growth and reactant solution adjustment crucible rise respectively and under
Drop.
Clear, complete description is carried out to the present invention by the technical scheme in above example, it is clear that described reality
Example is applied for a part of embodiment of the invention, rather than whole.Based on the embodiment in the present invention, those of ordinary skill in the art exist
The every other embodiment obtained under the premise of creative work is not made, the scope of protection of the invention is belonged to.
Claims (10)
1. a kind of regulation reactor for crystal growth, including kettle and the heater being located in kettle, it is characterised in that institute
State in kettle at least provided with a crucible for crystal growth and a reactant solution adjustment crucible, the crucible for crystal growth and
Reactant solution is adjusted crucible and is connected by the connecting pipeline full of reactant solution, and kettle is provided with lifting moving control machine
Structure, the lifting moving controlling organization is connected with crucible for crystal growth and reactant solution adjustment crucible respectively, drives the crystal
Growth crucible and reactant solution adjustment crucible rise or fall.
2. the regulation reactor for crystal growth according to claim 1, it is characterised in that the connecting pipeline is at least
Set one.
3. the regulation reactor for crystal growth according to claim 2, it is characterised in that the connecting pipeline is by stone
English, ceramics, high-purity copper pipe or stainless steel tube material are made.
4. the regulation reactor for crystal growth according to claim 3, it is characterised in that the crystal growth earthenware
The side and bottom surface of crucible and reactant solution adjustment crucible are all provided with having heaters.
5. the regulation reactor for crystal growth according to claim 4, it is characterised in that the crystal growth earthenware
The quantity of crucible and reactant solution adjustment crucible is identical or difference.
6. the regulation reactor for crystal growth according to claim 5, it is characterised in that the heater is infrared
Heater, resistance heater or radio heater.
7. a kind of control method of regulation reactor for crystal growth according to any one of claim 1-6, wraps
Include following steps：
Under original state, crystal seed template and filling reactant solution are placed in crucible for crystal growth, in reactant solution adjustment
Filling reactant solution in crucible, the liquid level of liquid level and reactant solution the adjustment crucible of crucible for crystal growth is located at same height
Degree；
Starting heater carries out heat temperature raising, while introducing nitrogen toward kettle is interior；
In heating up process, the relative altitude of adjustment crucible for crystal growth and reactant solution adjustment crucible makes crystal
Reactant solution in growth crucible and reactant solution adjustment crucible mutually flows through connecting pipeline, until crystal growth is complete
Into；
After the completion of crystal growth, crucible for crystal growth and reactant solution adjustment crucible is resetted, keep liquid level identical again
Height.
8. it is according to claim 7 for crystal growth regulation reactor control method, it is characterised in that control
When crucible for crystal growth and reactant solution adjust the relative altitude of crucible, crucible for crystal growth transfixion is kept, made
Reactant solution adjusts crucible raising and lowering；Or reactant solution adjustment crucible transfixion is kept, use crystal growth
Crucible raising and lowering；Or crucible for crystal growth and reactant solution adjustment crucible difference raising and lowering.
9. it is according to claim 7 for crystal growth regulation reactor control method, it is characterised in that the crystalline substance
Body growth crucible and/or reactant solution adjust crucible in raising and lowering, and continuously to move, periodic motion or interval transport
Dynamic mode is moved.
10. it is according to claim 7 for crystal growth regulation reactor control method, it is characterised in that plus
In hot temperature-rise period, crucible for crystal growth is identical with the temperature of reactant solution adjustment crucible or differs.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611110488.9A CN106757359B (en) | 2016-12-06 | 2016-12-06 | Adjusting reaction kettle for crystal growth and control method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611110488.9A CN106757359B (en) | 2016-12-06 | 2016-12-06 | Adjusting reaction kettle for crystal growth and control method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106757359A true CN106757359A (en) | 2017-05-31 |
| CN106757359B CN106757359B (en) | 2020-10-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201611110488.9A Active CN106757359B (en) | 2016-12-06 | 2016-12-06 | Adjusting reaction kettle for crystal growth and control method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109440189A (en) * | 2018-12-27 | 2019-03-08 | 北京大学东莞光电研究院 | A kind of crystal growing apparatus of light modulation local strengthening |
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 |
-
2016
- 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109440189A (en) * | 2018-12-27 | 2019-03-08 | 北京大学东莞光电研究院 | A kind of crystal growing apparatus of light modulation local strengthening |
| 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 |
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| Publication number | Publication date |
|---|---|
| CN106757359B (en) | 2020-10-27 |
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