CN105442046A - Nitride mono-crystal growth device and method - Google Patents
Nitride mono-crystal growth device and method Download PDFInfo
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- CN105442046A CN105442046A CN201610017711.9A CN201610017711A CN105442046A CN 105442046 A CN105442046 A CN 105442046A CN 201610017711 A CN201610017711 A CN 201610017711A CN 105442046 A CN105442046 A CN 105442046A
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- crystal seed
- bracing
- strutting arrangement
- reactor
- crystal
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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
- C30B9/12—Salt solvents, e.g. flux growth
Abstract
The invention discloses a nitride mono-crystal growth device and method. The nitride mono-crystal growth device comprises a reaction kettle, wherein the reaction kettle is internally filled with a reactant solution; a crystal seed supporting device is arranged in the reaction kettle; the supporting device is completely soaked into the reactant solution. The nitride mono-crystal growth device is characterized in that the reaction kettle is internally provided with the crystal seed supporting device with a special structure body; a crystal seed template is arranged in the supporting device; the reactant solution flows in from a plurality of holes in side faces of the crystal seed supporting device and flows out from a plurality of holes in the upper and lower bottom faces through a drainage device. With the adoption of the nitride mono-crystal growth device and method, the problem that the reactant solution in a traditional reaction kettle flows without sequence is effectively solved and the quality of crystals is effectively improved.
Description
Technical field
The present invention relates to a kind of growing nitride single crystal device and method.
Background technology
Gan, owing to having the premium properties such as broad-band gap, high withstand voltage, high thermal conductance, has broad application prospects in fields such as laser apparatus (LD), photodiode (LED), High Electron Mobility Transistor (HEMT).
At present, the growth substrates of most of gallium nitride device is the foreign substrate such as sapphire, SiC, because foreign substrate exists the mismatch problem of thermal conductivity and lattice, makes gan there is larger dislocation desity, affects the performance of gallium nitride device.Homo-substrate is used to be the ideal scheme addressed this problem.
At present, the Commercial processes of gallium nitride substrate is hydride gas-phase epitaxy (HVPE), although have larger growth velocity, crystal mass needs to improve further.In order to improve crystal mass, propose other gallium nitride single crystal growth methods in recent years.Compare additive method, the growth conditions of sodium flux method (NaFlux) is relatively gentle and crystal mass is higher, has larger application prospect.How improving crystal mass and the growth velocity of sodium flux method gallium nitride single crystal further, is the major issue being badly in need of at present solving.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of device that can improve gallium nitride single crystal crystal mass and growth velocity.
The present invention takes following technical scheme:
A kind of growing nitride single crystal device, comprises reactor, and fill reactant solution in reactor, be provided with crystal seed bracing or strutting arrangement in reactor, crystal seed bracing or strutting arrangement is immersed in reactant solution completely.It is characterized in that, in described reactor, be provided with the crystal seed bracing or strutting arrangement of special construction body.
Described crystal seed bracing or strutting arrangement is the hollow shell structure of porous, and surperficial through hole is communicated with hollow shell inside.
Described crystal seed bracing or strutting arrangement side is provided with catch, and catch has uniform shapes, size, and catch is connected with side through hole, and the angle of inclination between catch and side is 10 ~ 80 degree, and catch tilts to through hole direction.
Described crystal seed bracing or strutting arrangement is connected with interlinkage, and interlinkage rotates and drives crystal seed bracing or strutting arrangement to rotate, and turning direction is identical with catch vergence direction.
Described interlinkage is scalable at vertical direction, moves under driving crystal seed bracing or strutting arrangement in the vertical direction.
It is inner that crystal seed template is positioned over described crystal seed bracing or strutting arrangement, with through hole at a distance of 1 ~ 10mm.
Described crystal seed template, fixed placement is inner in described crystal seed bracing or strutting arrangement, and crystal seed template and through hole are at a distance of 1 ~ 10mm, and crystal seed masterplate follows crystal seed bracing or strutting arrangement synchronous axial system; Described crystal seed template, or be fixed on reactor inwall, crystal seed template and through hole are at a distance of 1 ~ 10mm, and crystal seed template is not followed crystal seed bracing or strutting arrangement and rotated.
Described crystal seed template is vertically placed, horizontal positioned or place with any oblique angle.
Described crystal seed bracing or strutting arrangement, its shape is cylindrical, square column type, elliptical cylinder-shape and other any geometrical bodies with hollow shell structure.
A growth method for nitride single-crystal, comprises the following steps:
S1, crystal seed template fixed placement is inner at crystal seed bracing or strutting arrangement, or be fixed on reactor inwall, crystal seed template is with horizontal positioned or vertically place or place with certain angle of inclination (0 ~ 90 degree), distance lead to the hole site 1 ~ 10mm;
S2, rises crystal seed bracing or strutting arrangement, placing response thing solution in reactor, ensures that crystal seed bracing or strutting arrangement is positioned at above reactant solution, not contact reacts thing solution;
S3, sealed reactor, passes into nitrogen, and heats reactor in reactor, and make the pressure of reactor reach 1 ~ 50MPa, temperature reaches 700 ~ 1000 DEG C;
S4, when temperature, pressure reaches growth conditions, controlling interlinkage makes crystal seed bracing or strutting arrangement drop to below liquid-gas interface, be immersed in completely in reactant solution, and start interlinkage rotation, drive crystal seed bracing or strutting arrangement to rotate, the growth solution in reactor is flowed, and flowpaths is through crystal seed template surface;
After S5, crystal growth reach target thickness, draw high crystal seed bracing or strutting arrangement above liquid-gas interface, carry out step-down cooling to reactor, then take out crystal, growth response terminates.
The present invention has following beneficial effect:
1. solution flows into bracing or strutting arrangement from side door through hole, flows through crystal seed template, flows out from upper bottom surface through hole, has the effect of solution circulated flowing, effectively promotes that the circulation of reactants dissolved and liquid-gas interface high density N participates in reaction, reduces liquid-gas interface polycrystal layer.
2. circulating of solution is flowed into by through hole, and crystal seed template is positioned over through hole annex, and reaction starting material directly reach crystal seed template surface, and reaction is more abundant, effectively improves crystal mass and the speed of growth.
3. crystal seed bracing or strutting arrangement can carry multi-disc crystal seed template, and multiple-piece crystal growth effectively can reduce growth cost, and crystal seed bracing or strutting arrangement is convenient to take off gallium nitride single crystal.
4., before reaching reaction conditions, keep crystal seed bracing or strutting arrangement to be on liquid level; After crystal growth reaches desired thickness requirement, above move crystal seed bracing or strutting arrangement, effectively avoid the by product reacted to produce, improve crystal mass further.
Accompanying drawing explanation
Accompanying drawing 1 is the embodiment of the present invention one structural representation (crystal seed bracing or strutting arrangement is sketch, sees Fig. 2);
Accompanying drawing 2 is the crystal seed support device structure schematic diagram of the embodiment of the present invention one;
Accompanying drawing 3 is the position view of the crystal seed template of the embodiment of the present invention one;
Accompanying drawing 4 is the view of the solution flowing of the embodiment of the present invention one;
Accompanying drawing 5 is the crystal seed support device structure schematic diagram of the embodiment of the present invention two;
Accompanying drawing 6 is the position view of the crystal seed template of the embodiment of the present invention two;
Accompanying drawing 7 is the view of the solution flowing of the embodiment of the present invention two.
Accompanying drawing mark illustrates:
In embodiment one: 10: reactor; 11: reactant solution; 12: the crystal seed bracing or strutting arrangement of embodiment one; 13: upper bottom surface through hole; 14: side through hole; 15: side flaps; 16: turning direction; 17: interlinkage; 18: crystal seed template; 19: solution flow direction
In embodiment two: 20: reactor; 21: reactant solution; 22: the crystal seed bracing or strutting arrangement of embodiment two; 23: upper bottom surface through hole; 24: side through hole; 25: side flaps; 26: turning direction; 27: interlinkage; 28: crystal seed template; 29: solution flow direction
Embodiment
For the ease of the understanding of those skilled in the art, below in conjunction with accompanying drawing, the invention will be further described.
Embodiment one, as shown in Figure 1, gallium nitride single crystal growing apparatus, comprises reactor 10, and fill reactant solution 11 in reactor, be provided with crystal seed bracing or strutting arrangement 12 in reactor, crystal seed bracing or strutting arrangement is immersed in reactant solution 11 completely.Crystal seed bracing or strutting arrangement 12 is the hollow cylinder shell structure of porous, and as shown in Figure 2, surperficial through hole 13,14 is communicated with hollow shell inside, and upper and lower bottom surface through hole 13 is manhole, diameter 5mm, and side through hole 14 is manhole, diameter 10mm.Crystal seed bracing or strutting arrangement side is provided with catch 15, and catch 15 is connected with side through hole 14, and catch 15 is semicolumn hull shape, length 10mm, diameter 10mm, and deflection side through hole 14 tilts 60 degree.Crystal seed bracing or strutting arrangement 12 is connected with interlinkage 17, and interlinkage 17 rotates and drives crystal seed bracing or strutting arrangement 12 to rotate, and turning direction 16 is identical with catch 15 vergence direction, looks down, even clockwise direction from reactor 10 top.Crystal seed template 18 totally 6, is all fixed on crystal seed bracing or strutting arrangement 12 inner, as shown in Figure 3.Wherein 2 fixed placement are in the upper and lower bottom surface parallel position of crystal seed bracing or strutting arrangement 12, respectively with upper and lower bottom surface through hole 13 10mm apart; Other 4 are securely installed in crystal seed bracing or strutting arrangement 12 medial surface, with side through hole 14 at a distance of 10mm.Rise crystal seed bracing or strutting arrangement 12, placing response thing starting material in reactor, ensure that crystal seed bracing or strutting arrangement is positioned at above reactant, not contact reacts thing; Sealed reactor 10, passes into nitrogen, and heats reactor in reactor, and make the pressure of reactor reach 5MPa, temperature reaches 900 DEG C; When temperature, pressure reaches growth conditions, controlling interlinkage 17 makes crystal seed bracing or strutting arrangement 12 drop to below liquid-gas interface, be immersed in reactant solution 11 completely, and start interlinkage 17 and rotate, crystal seed bracing or strutting arrangement 12 is driven to rotate, growth solution 11 in reactor is flowed, and flowpaths is surperficial through crystal seed template 18, as shown in Figure 4; Crystal growth draws high crystal seed bracing or strutting arrangement above liquid-gas interface after reaching target thickness (700 μm), and carry out step-down cooling to reactor 10, then take out crystal, growth response terminates.
Embodiment two, gallium nitride single crystal growing apparatus similar embodiment one, difference is that crystal seed bracing or strutting arrangement 22 is the hollow square body shell structure of porous, as shown in Figure 5, surface through hole 23,24 is communicated with hollow shell inside, and upper and lower bottom surface through hole 23 is manhole, diameter 5mm, side through hole 24 is manhole, diameter 5mm.Crystal seed bracing or strutting arrangement side is provided with catch 25, and catch 25 is connected with side through hole 24, and catch 25 is semicolumn hull shape, length 5mm, diameter 5mm, and deflection side through hole 24 tilts 70 degree.Crystal seed bracing or strutting arrangement 22 is connected with interlinkage 27, and interlinkage 27 rotates and drives crystal seed bracing or strutting arrangement 22 to rotate, and turning direction 26 is identical with catch 25 vergence direction, looks down, even clockwise direction from reactor 20 top.Crystal seed template 28 totally 6, is all fixed on crystal seed bracing or strutting arrangement 22 inner, as accompanying drawing
6shown in.Wherein 2 fixed placement are in the upper and lower bottom surface parallel position of crystal seed bracing or strutting arrangement 22, respectively with upper and lower bottom surface through hole 23 10mm apart; Other 4 are securely installed in crystal seed bracing or strutting arrangement 22 medial surface, with side through hole 24 at a distance of 10mm.Rise crystal seed bracing or strutting arrangement 22, placing response thing starting material in reactor, ensure that crystal seed bracing or strutting arrangement is positioned at above reactant, not contact reacts thing; Sealed reactor 20, passes into nitrogen, and heats reactor in reactor, and make the pressure of reactor reach 4.5MPa, temperature reaches 850 DEG C; When temperature, pressure reaches growth conditions, controlling interlinkage 27 makes crystal seed bracing or strutting arrangement 22 drop to below liquid-gas interface, be immersed in reactant solution 21 completely, and start interlinkage 27 and rotate, crystal seed bracing or strutting arrangement 22 is driven to rotate, growth solution 21 in reactor is flowed, and flowpaths is surperficial through crystal seed template 28, as shown in Figure 7; Crystal growth draws high crystal seed bracing or strutting arrangement above liquid-gas interface after reaching target thickness (800 μm), and carry out step-down cooling to reactor 20, then take out crystal, growth response terminates.
It should be noted that, the above is not the restriction to technical solution of the present invention, and under the prerequisite not departing from creation design of the present invention, any apparent replacement is all within protection scope of the present invention.
Claims (9)
1. a growing nitride single crystal device, comprises reactor, the crystal seed bracing or strutting arrangement arranged in reactor, and interlinkage, it is characterized in that, described crystal seed bracing or strutting arrangement is the hollow shell structure of porous, surface through hole is communicated with hollow shell inside, and side through hole has catch.
2. a kind of growing nitride single crystal device according to claim 1, is characterized in that, fill reactant solution in described reactor, described crystal seed bracing or strutting arrangement, in single crystal growth process, is immersed in reactant solution completely.
3. a kind of growing nitride single crystal device according to claim 1, is characterized in that, described crystal seed bracing or strutting arrangement side is provided with catch, and catch has uniform shapes, size, and catch is connected with side through hole; Angle of inclination between catch and side is 10 ~ 80 degree, and catch is to through hole lopsidedness.
4. a kind of growing nitride single crystal device according to claim 1, is characterized in that, described crystal seed bracing or strutting arrangement is connected with interlinkage, and described interlinkage rotates and drives crystal seed bracing or strutting arrangement to rotate, and turning direction is identical with catch vergence direction.
5. a kind of growing nitride single crystal device according to claim 1,4, it is characterized in that, described interlinkage is scalable at vertical direction, moves under driving crystal seed bracing or strutting arrangement in the vertical direction.
6. a kind of growing nitride single crystal device according to claim 1, is characterized in that, by crystal seed template, fixed placement is inner in described crystal seed bracing or strutting arrangement, and crystal seed template and through hole are at a distance of 1 ~ 10mm; Crystal seed template follows crystal seed bracing or strutting arrangement synchronous axial system; Described crystal seed template, or be fixed on reactor inwall, crystal seed template and through hole are at a distance of 1 ~ 10mm; Crystal seed template is not followed crystal seed bracing or strutting arrangement and is rotated.
7. a kind of growing nitride single crystal device according to claim 6, is characterized in that, described crystal seed template is vertically placed, horizontal positioned or place with any oblique angle.
8. a kind of growing nitride single crystal device according to claim 1, is characterized in that, described crystal seed bracing or strutting arrangement, and its shape is cylindrical, square column type, elliptical cylinder-shape and other any geometrical bodies with hollow shell structure.
9. a growth method for nitride single-crystal, comprises the following steps:
S1, crystal seed template fixed placement is inner in crystal seed bracing or strutting arrangement, or be fixed on reactor inwall, crystal seed template is with horizontal positioned or vertically place or place with certain angle of inclination (0 ~ 90 degree), distance lead to the hole site 1 ~ 10mm;
S2, rises crystal seed bracing or strutting arrangement, placing response thing solution in reactor, ensures that crystal seed bracing or strutting arrangement is positioned at above reactant solution, not contact reacts thing solution;
S3, sealed reactor, passes into nitrogen, and heats reactor in reactor, and make the pressure of reactor reach 1 ~ 50MPa, temperature reaches 700 ~ 1000 DEG C;
S4, when temperature, pressure reaches growth conditions, controlling interlinkage makes crystal seed bracing or strutting arrangement drop to below liquid-gas interface, be immersed in completely in reactant solution, and start interlinkage rotation, drive crystal seed bracing or strutting arrangement to rotate, the growth solution in reactor is flowed, and flowpaths is through crystal seed template surface;
After S5, crystal growth reach target thickness, draw high crystal seed bracing or strutting arrangement above liquid-gas interface, carry out step-down cooling to reactor, then take out crystal, growth response terminates.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106367804A (en) * | 2016-10-28 | 2017-02-01 | 北京大学东莞光电研究院 | Pressure-intensity-control crystal growth reaction kettle |
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| CN1938457A (en) * | 2004-03-31 | 2007-03-28 | 日本碍子株式会社 | Growing method of gallium nitride single crystal and gallium nitride single crystal |
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| CN106367804A (en) * | 2016-10-28 | 2017-02-01 | 北京大学东莞光电研究院 | Pressure-intensity-control crystal growth reaction kettle |
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