CN106367804A - Pressure-intensity-control crystal growth reaction kettle - Google Patents
Pressure-intensity-control crystal growth reaction kettle Download PDFInfo
- Publication number
- CN106367804A CN106367804A CN201610963655.8A CN201610963655A CN106367804A CN 106367804 A CN106367804 A CN 106367804A CN 201610963655 A CN201610963655 A CN 201610963655A CN 106367804 A CN106367804 A CN 106367804A
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- CN
- China
- Prior art keywords
- pressure
- crystal growth
- kettle
- connecting hole
- growth reactor
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Classifications
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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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/08—Reaction chambers; Selection of materials therefor
-
- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/16—Controlling or regulating
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a pressure-intensity-control crystal growth reaction kettle. The pressure-intensity-control crystal growth reaction kettle comprises a kettle body. Crystal growth chambers are formed in the kettle body, a heating device is arranged outside the kettle body, the kettle body is filled with liquid gallium sources, a pressure-intensity adjusting chamber is also formed in the kettle body, partition plates are arranged on the bottom faces of the crystal growth chambers, connecting holes are formed in the partition plates, the crystal growth chambers are communicated with the pressure-intensity adjusting chamber through the connecting holes, a pressure increasing valve and a pressure reducing valve are arranged on the pressure-intensity adjusting chamber, joining pipe openings extruding towards the crystal growth chambers are formed in the partition plates, and the connecting holes are formed in the side walls of the joining pipe openings. According to the pressure-intensity-control crystal growth reaction kettle, as the difference between the pressure intensity of the two crystal growth chambers and the pressure intensity of the pressure-intensity adjusting chamber is finely adjusted, controllable flowing of the liquid gallium sources in the reaction kettle can be effectively achieved.
Description
Technical field
The present invention relates to a kind of pressure regulation and control crystal growth reactor for hydride gas-phase epitaxy.
Background technology
Gallium nitride (gan) as most important group-III nitride semiconductor, belong to wide bandgap semiconductor materials (～
3.4ev), in many applications such as opto-electronic device, thick film gan will improve to device performance as homoepitaxy substrate
To huge impetus.The method of production of gan crystal thick film at present, mainly Metalorganic Chemical Vapor Deposition
(mocvd), hydride vapour phase epitaxy method (hvpe) etc., the gallium nitride dislocation density that vapor growth method obtains is larger, and passes
System prepare silicon (si), the liquid phase czochralski method of GaAs (gaas) single crystalline substrate be difficult to grow gan backing material.For this reason,
It has been proposed that using alkali metal such as sodium (na) as solvent, can under the conditions of comparatively gentle the element nitride crystal such as liquid growth gan.
In liquid phase method growth gan crystal, crystal growth quality and speed will be by nitrogen concentration weights in crystal seed reticle surface ga-na solution
Affect, have at present using the mixing method promotion nitrogen and ga source such as rotating, waving and stir, but these methods all cannot
Make reaction solution integrally do homogeneous motion, be unfavorable for obtaining the homogeneous gan crystalline material of quality.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of pressure to regulate and control crystal growth reactor, by adjust pressure
Realize the controllable flow in liquid-gallium source in reactor.
In order to solve above-mentioned technical problem, the present invention takes below scheme:
A kind of pressure regulates and controls crystal growth reactor, including kettle, is provided with crystal growing chamber in kettle, and kettle is externally provided with and adds
Thermal, is filled with liquid-gallium source in kettle, be additionally provided with pressure regulation room in described kettle, crystal growing chamber bottom surface be provided with every
Plate, this dividing plate is provided with connecting hole, and this crystal growing chamber is connected with pressure regulation room by connecting hole, and pressure regulation room is provided with
Pressure charging valve and air relief valve.
The linking mouth of pipe of crystal growing chamber protrusion is provided with described dividing plate, connecting hole is arranged on this linking mouth of pipe side
Wall.
The mouth of pipe is rectangular or arc or semicircle or polygon for described linking.
Described linking mouth of pipe side wall is provided with least one connecting hole, and this connecting hole is circular, square, oval or many
Side shape.
Described connecting hole is provided with least two, and two neighboring connecting hole towards identical or different.
Crystal growing chamber in described kettle and pressure regulation room each setting one or more than one quantity, this crystal
Growth room is identical with the quantity of pressure regulation room or different.
Described kettle is cylindrical, prismatic or rectangle.
The side of described kettle and bottom surface are equipped with heater.
Described heater is resistive heating device, induction heating apparatus or radio frequency heating apparatus.
The present invention passes through the pressure regulation room that setting is connected with crystal growing chamber, and the pressure by adjustment pressure regulation room is big
Little come to realize the liquid-gallium source flow in kettle ground purpose it is ensured that in reactor liquid-gallium source can be sufficiently mixed with nitrogen, and
Avoid liquid surface to form thin film, stop reaction from continuing to occur.By the difference of pressure between trickle adjustment two chambers, permissible
It is effectively realized the controllable flow in liquid-gallium source in reactor, is conducive to accelerating response speed, thus promoting and improving crystal
Growth quality.
Brief description
Accompanying drawing 1 is the cross-sectional view of the embodiment of the present invention one；
Accompanying drawing 2 is that the liquid of the embodiment of the present invention one flows to structural representation；
Accompanying drawing 3 is the cross-sectional view of the embodiment of the present invention two.
Specific embodiment
For the ease of the understanding of those skilled in the art, the invention will be further described below in conjunction with the accompanying drawings.
Embodiment one
As shown in Figure 1, a kind of pressure regulates and controls crystal growth reactor, including kettle, is provided with crystal growing chamber in kettle
30, kettle is externally provided with heater 20, is filled with liquid-gallium source 50, is additionally provided with pressure regulation room 31 in described kettle in kettle,
Crystal growing chamber 30 bottom surface is provided with dividing plate, and this dividing plate is provided with connecting hole 40, and this crystal growing chamber 30 passes through connecting hole 40 and pressure
Strong regulation room 31 connects, and pressure regulation room 31 is provided with pressure charging valve 10 and air relief valve 11.Liquid-gallium source is filled in crystal growing chamber
In pressure regulation room, in the case of the pressure identical of crystal growing chamber and pressure regulation room two chambers, crystal growing chamber
The liquid level adjusting indoor liquid-gallium source with pressure is located in same level.Kettle is cylindrical, prismatic or rectangle.Kettle
Side and bottom surface be equipped with heater, and this heater be resistive heating device, induction heating apparatus or radio frequency add
Thermal, or the heater of other modes.
The linking mouth of pipe of crystal growing chamber protrusion is provided with described dividing plate, connecting hole 40 is arranged on this linking mouth of pipe side
Wall.The mouth of pipe is rectangular or arc or semicircle or polygon for linking, or can also be other shapes, as irregular
Curve form.
Linking mouth of pipe side wall is provided with least one connecting hole, and this connecting hole is circular, square, oval or polygon
Shape, or triangle, or other shapes.The size of connecting hole is flexibly arranged according to practical situation.
Described connecting hole is provided with least two, and two neighboring connecting hole towards identical or different.Preferable case
Under, including at least two towards different connecting holes in setting multiple connecting holes, and the plurality of connecting hole.Each connecting hole is permissible
Regularly arrangement is it is also possible to irregular arrangement.
One pressure regulation room and a crystal growing chamber are set in the present embodiment.
In the present embodiment, as shown in figure 1 and 2, when initial, pressure regulation room is identical with the pressure of crystal growing chamber,
The liquid level in the liquid-gallium source of two chambers is located in same level.Heated up by heating devices heat, and logical toward in kettle
Gas nitrogen pressurizes, and makes to reach growth conditionss in kettle.After reaching crystal growth temperature and other growth conditions, adjust to pressure
Section interior is passed through nitrogen, noble gases or mixed gas, increases pressure, then in pressure regulation room 31, pressure increases, and will result in this
Pressure adjusts indoor liquid-gallium source 50 liquid level and declines, due to the connectedness of liquid, the liquid-gallium source in crystal growth reative cell 30
Liquid level rises, and meanwhile, at connecting hole 40, liquid-gallium source will spray (liquid from connection towards crystal growing chamber with same speed
Gallium source injection direction is as shown in accompanying drawing 3 arrow), this flowing will result in the flowing of whole liquid, also results in the fluctuation of liquid level, from
And accelerate liquid-gallium source and nitrogen mutually to mix diffusion.After some time, the pressure in pressure regulation room 31 is reduced by air relief valve
By force, then in pressure regulation indoor 31, liquid-gallium source 50 surface will rise, and liquid-gallium source upper surface in crystal growth reative cell 30
To decline, so move in circles, the flowing that goes round and begins again in liquid-gallium source will be formed, so that nitrogen adds to gallium source in time
In solution, beneficial to accelerating response speed, improve crystal mass.
Embodiment two
Agent structure in the present embodiment is identical with embodiment one, differs only in: as shown in Figure 3, is provided with one
Pressure regulation room 31 and two crystal growing chambers 30, the structure of this two crystal growing chambers is identical, all by the dividing plate of bottom surface even
Connect hole to connect with pressure regulation room.Liquid-gallium source is consistent with embodiment one with regulative mode, and it is no longer repeated for here.
Certainly, the present invention can also arrange two pressure regulation rooms and a crystal growing chamber, or the pressure of other quantity
Strong regulation room and crystal growing chamber, here will not enumerate.
It should be noted that the above is not limited to the present invention, in the creation design without departing from the present invention
Under the premise of, any obvious replacement is all within protection scope of the present invention.
Claims (9)
1. a kind of pressure regulates and controls crystal growth reactor, including kettle, is provided with crystal growing chamber in kettle, kettle is externally provided with heating
Device, is filled with liquid-gallium source it is characterised in that being additionally provided with pressure regulation room, crystal growing chamber bottom in described kettle in kettle
Face is provided with dividing plate, and this dividing plate is provided with connecting hole, and this crystal growing chamber is connected with pressure regulation room by connecting hole, and pressure is adjusted
Room is provided with pressure charging valve and air relief valve.
2. pressure regulation and control crystal growth reactor according to claim 1 is it is characterised in that be provided with described dividing plate
The linking mouth of pipe that crystal growing chamber protrudes, connecting hole is arranged on this linking mouth of pipe side wall.
3. pressure regulation and control crystal growth reactor according to claim 2 is it is characterised in that the described linking mouth of pipe is rectangular
Or arc or semicircle or polygon.
4. pressure according to claim 3 regulation and control crystal growth reactor is it is characterised in that on the wall of described linking mouth of pipe side
It is provided with least one connecting hole, this connecting hole is circular, square, oval or polygon.
5. pressure regulation and control crystal growth reactor according to claim 4 is it is characterised in that described connecting hole is provided with least
Two, and two neighboring connecting hole towards identical or different.
6. pressure according to claim 5 regulates and controls crystal growth reactor it is characterised in that the crystal in described kettle is given birth to
Long room and pressure regulation room each setting one or more than one quantity, the quantity phase of this crystal growing chamber and pressure regulation room
Same or different.
7. pressure according to claim 6 regulation and control crystal growth reactor it is characterised in that described kettle be cylindrical,
Prismatic or rectangle.
8. pressure according to claim 7 regulation and control crystal growth reactor is it is characterised in that the side of described kettle and bottom
Face is equipped with heater.
9. pressure regulation and control crystal growth reactor according to claim 8 is it is characterised in that described heater is resistance
Heater, induction heating apparatus or radio frequency heating apparatus.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610963655.8A CN106367804B (en) | 2016-10-28 | 2016-10-28 | A kind of pressure regulation crystal growth reaction kettle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610963655.8A CN106367804B (en) | 2016-10-28 | 2016-10-28 | A kind of pressure regulation crystal growth reaction kettle |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106367804A true CN106367804A (en) | 2017-02-01 |
| CN106367804B CN106367804B (en) | 2019-01-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610963655.8A Active CN106367804B (en) | 2016-10-28 | 2016-10-28 | A kind of pressure regulation crystal growth reaction kettle |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3486937A (en) * | 1967-03-24 | 1969-12-30 | Perkin Elmer Corp | Method of growing a single crystal film of a ferrimagnetic material |
| WO2010084675A1 (en) * | 2009-01-21 | 2010-07-29 | 日本碍子株式会社 | Group 3b nitride crystal plate |
| 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 |
| CN103603049A (en) * | 2013-12-06 | 2014-02-26 | 北京大学东莞光电研究院 | Multi-piece nitride monocrystal material growing device and method |
| CN104894644A (en) * | 2015-06-29 | 2015-09-09 | 北京大学东莞光电研究院 | Nitride crystal growing device and method |
| CN105442046A (en) * | 2016-01-11 | 2016-03-30 | 东莞市中镓半导体科技有限公司 | Nitride mono-crystal growth device and method |
| 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
- 2016-10-28 CN CN201610963655.8A patent/CN106367804B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3486937A (en) * | 1967-03-24 | 1969-12-30 | Perkin Elmer Corp | Method of growing a single crystal film of a ferrimagnetic material |
| WO2010084675A1 (en) * | 2009-01-21 | 2010-07-29 | 日本碍子株式会社 | Group 3b nitride crystal plate |
| 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 |
| CN103603049A (en) * | 2013-12-06 | 2014-02-26 | 北京大学东莞光电研究院 | Multi-piece nitride monocrystal material growing device and method |
| 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 |
| CN104894644A (en) * | 2015-06-29 | 2015-09-09 | 北京大学东莞光电研究院 | Nitride crystal growing device and method |
| CN105442046A (en) * | 2016-01-11 | 2016-03-30 | 东莞市中镓半导体科技有限公司 | Nitride mono-crystal growth device and method |
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|---|---|
| CN106367804B (en) | 2019-01-15 |
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