CN107687022A - Promote the method for seed crystal liquid phase epitaxy in flux growth metrhod growth GaN single crystal system - Google Patents
Promote the method for seed crystal liquid phase epitaxy in flux growth metrhod growth GaN single crystal system Download PDFInfo
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- CN107687022A CN107687022A CN201610633144.XA CN201610633144A CN107687022A CN 107687022 A CN107687022 A CN 107687022A CN 201610633144 A CN201610633144 A CN 201610633144A CN 107687022 A CN107687022 A CN 107687022A
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- growth
- single crystal
- gallium nitride
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- seed 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
- C30B19/00—Liquid-phase epitaxial-layer growth
- C30B19/02—Liquid-phase epitaxial-layer growth using molten solvents, e.g. flux
-
- 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
Abstract
The method for promoting seed crystal liquid phase epitaxy in GaN single crystal system is grown the invention discloses a kind of flux growth metrhod, it includes：During with flux growth metrhod growing gallium nitride single crystal, in adding carbonaceous additive in the growth system of gallium nitride single crystal, the carbonaceous additive includes the carbon material after nitridation.Than prior art, the inventive method is used as additive by the carbon material after nitridation is added in the system of flux growth metrhod growing gallium nitride single crystal, gallium nitride polycrystalline can effectively be suppressed to be formed, promote gallium nitride seed crystal rheotaxial growth, and effectively reduce the seed crystal back dissolving of gallium nitride seeded growth early stage.
Description
Technical field
The present invention relates to a kind of method of flux growth metrhod growing gallium nitride single crystal, more particularly to a kind of flux growth metrhod growth
Promote the method for seed crystal liquid phase epitaxy in GaN single crystal system, belong to materials science field.
Background technology
Flux growth metrhod (Na Flux method) growing gallium nitride (GaN) monocrystalline has many advantages, be at present in the world
One of generally acknowledged achievable high quality, growing technology of large scale gallium nitride body monocrystalline industrialization production.Due to gallium nitride single crystal
Growth system (referred to as following " growth system ") general use stickiness liquid metal and nitrogen containing metallic sodium and gallium
As growth source, in growth course, nitrogen source reaches supersaturation first at gas-liquid interface, forms gallium nitride polycrystalline shell, leads
Cause outside nitrogen to be blocked at gas-liquid interface, so as to cause the supply of growth system nitrogen source to be interrupted, and then make in growth system
Gallium nitride seed crystal stops rheotaxial growth；On the one hand the gallium nitride polycrystalline shell of formation blocks the supply of system nitrogen source, the opposing party
Gallium source in face consumption system.Therefore, effectively suppress this polycrystalline formation in growth system and have become the growing technology
In one of key difficulties.
The content of the invention
It is a primary object of the present invention to provide in a kind of flux growth metrhod growth GaN single crystal system to promote seed crystal liquid phase epitaxy
Method, to overcome deficiency of the prior art.
To realize aforementioned invention purpose, the technical solution adopted by the present invention includes：
Promote the method for seed crystal liquid phase epitaxy in a kind of flux growth metrhod growth GaN single crystal system provided in an embodiment of the present invention
Including：During with flux growth metrhod growing gallium nitride single crystal, in adding carbonaceous additive in the growth system of gallium nitride single crystal,
The carbonaceous additive includes the carbon material after nitridation.
More preferable, the carbonaceous additive is made up of the carbon material after nitrogenizing.
Promote the method for seed crystal liquid phase epitaxy in a kind of flux growth metrhod growth GaN single crystal system provided in an embodiment of the present invention
Specifically include：In anhydrous and oxygen-free environment, metallic sodium is mixed with gallium, sequentially adds carbon material and nitrogen after nitridation afterwards
Change gallium seed crystal, form the growth system of gallium nitride single crystal；
The growth system of the gallium nitride single crystal is transferred in epitaxial growth equipment, is 3~10MPa, temperature in pressure
Under the conditions of 700~1000 DEG C, the rheotaxial growth of gallium nitride single crystal is carried out.
Compared with prior art, in the inventive method, by being added in the system of flux growth metrhod growing gallium nitride single crystal
Carbon material after middle nitridation can effectively suppress gallium nitride polycrystalline and be formed, be promoted outside gallium nitride seed crystal liquid phase as additive
Epitaxial growth, and effectively reduce the seed crystal back dissolving of gallium nitride seeded growth early stage.
Brief description of the drawings
Fig. 1 is using different carbonaceous additives and gallium nitride seed crystal liquid phase epitaxy in 1-2 of the embodiment of the present invention and reference examples 1-2
The graph of a relation advanced the speed.
Fig. 2 a- Fig. 2 b are that seed crystal back dissolving SEM figures and full light CL after the mesoporous carbon not nitrogenized are added in comparative example 1 of the present invention
Figure.
Fig. 2 c- Fig. 2 d are seed crystal back dissolving SEM figures and full light CL figures after the mesoporous carbon that nitridation is added in the embodiment of the present invention 1.
Embodiment
In view of deficiency of the prior art, inventor is able to propose the present invention's through studying for a long period of time and largely putting into practice
Technical scheme.The technical scheme, its implementation process and principle etc. will be further explained as follows.
The side for promoting seed crystal liquid phase epitaxy in GaN single crystal system is grown the embodiments of the invention provide a kind of flux growth metrhod
Method, it includes：During with flux growth metrhod growing gallium nitride single crystal, add in adding carbon in the growth system of gallium nitride single crystal
Add agent, the carbonaceous additive includes the carbon material after nitridation.
In some more specific embodiment, promote seed crystal liquid in described flux growth metrhod growth GaN single crystal system
The method of phase epitaxy includes：In anhydrous and oxygen-free environment, metallic sodium, gallium, carbonaceous additive and gallium nitride seed crystal are uniformly mixed
Close, carry out the rheotaxial growth of gallium nitride single crystal with flux growth metrhod afterwards.
More preferable, the dosage of the carbonaceous additive is metallic sodium and gallium total amount in gallium nitride single crystal growth system
0.005mol%~1.0mol%.
It is more preferable, the reaction temperature used in the flux growth metrhod for 700~1000 DEG C, reaction pressure for 3~
10MPa。
More preferable, the carbonaceous additive is using the carbon material after nitridation.
Carbon material after foregoing nitridation, it is the nitrogenous carbon material that the carbon material of various structures is nitrogenized and formed.
Carbon material after foregoing nitridation can be obtained by commercially available approach, also can produce (example using mode known to industry
Such as it see：Appl.Phys.Lett., 2000,77,2530；Appl.Phys.Lett.2001,78,978 etc.).
Carbon material after typical nitridation can be selected from graphite, graphene, activated carbon, CNT and the mesoporous carbon of nitridation
In any one or two or more combinations, but not limited to this.
In some embodiments, carbon source can be subjected to high-temperature ammonolysis processing in nitrogen containing atmosphere, forms the nitridation
Carbon material afterwards.
In some embodiments, high-temperature ammonolysis processing is carried out after carbon source can be mixed with nitrogen source, obtains the nitridation
Carbon material afterwards.
Further, the carbon source includes any one in graphite, graphene, activated carbon, CNT and mesoporous carbon
Or two or more combinations, but not limited to this.
Further, the nitrogen source includes but is not limited to melamine.
Further, the nitrogen containing atmosphere includes nitrogen or ammonia atmosphere, but not limited to this.
In some more specific embodiment, promote seed crystal liquid phase in a kind of flux growth metrhod growth GaN single crystal system
The method of extension includes：
In anhydrous and oxygen-free environment (such as in glove box of exhausted water anoxybiotic), metallic sodium is mixed with gallium, Zhi Houyi
The secondary carbon material and gallium nitride seed crystal added after nitridation, form the growth system of gallium nitride single crystal；
The growth system of the gallium nitride single crystal is transferred in epitaxial growth equipment, is 3~10MPa, temperature in pressure
Under the conditions of 700~1000 DEG C, the rheotaxial growth of gallium nitride single crystal is carried out.
Further, the dosage of the carbon material after the nitridation is metallic sodium and gallium in gallium nitride single crystal growth system
0.005mol%~1.0mol% of total amount.
In some embodiments, gallium can be with metallic sodium mass ratio in the gallium nitride single crystal growth system
10：(2.0~15.0).
The selection range of carbon material after the nitridation is as it was noted above, but not limited to this.
Foregoing epitaxial growth equipment can use suitable epitaxial device known to industry.
Below in conjunction with accompanying drawing and some embodiments the technical solution of the present invention is further explained explanation.It is implemented as follows
The carbon material after nitridation in example can use Nano Lett., 2009,9 (5), and 1752-1758)；ACS Catalysis,2012,
2,781-794)；CN 102120572A；CN 104310322A；It is prepared by the documents such as CN 103145122A.Such as can be by stone
The direct high-temperature ammonolysis processing under nitrogen or ammonia atmosphere of the carbon materials such as ink, graphene, activated carbon, CNT, mesoporous carbon, or
High-temperature ammonolysis is handled after such carbon material is mixed with melamine, the carbon material after being nitrogenized.
Postscript, as follows in each embodiment, in gallium nitride crystal growth system, in addition to the carbon material after nitridation, each original
The consumption proportion of material may be referred to existing literature, such as：
(1)Jpn.J.Appl.Phys.2003,42:L879。
(2)Jpn.J.Appl.Phys.2004,43:L486。
Embodiment 1：In the glove box of exhausted water anoxybiotic by mass ratio be 10：The gallium of (2.0~5.0) exists with metallic sodium
Mix in crucible, the mesoporous carbon that adds after nitridation (addition be metallic sodium, gallium total amount 0.005mol%~
0.01mol%), gallium nitride seed crystal is added afterwards, is then transferred in epitaxial growth equipment, is 3~5MPa in pressure, temperature is
Under conditions of 700~800 DEG C, the rheotaxial growth of flux growth metrhod gallium nitride single crystal is carried out.
Comparative example 1：This reference examples is substantially the same manner as Example 1, but it is mesoporous after nitrogenizing to use commercially available mesoporous carbon instead of
Carbon.
Referring to Fig. 1, using the carbonaceous additive after nitridation, the increase of gallium nitride seed crystal liquid phase epitaxy speed.
Embodiment 2：In the glove box of exhausted water anoxybiotic by mass ratio be 10：The gallium and metallic sodium of (6.0~10.0)
Mixed in crucible, the activated carbon (addition is metallic sodium, 0.015~0.1mol% of gallium total amount) added after nitridation, it
Gallium nitride seed crystal is added afterwards, is then transferred in epitaxial growth equipment, is 6~8MPa in pressure, temperature is 800~900 DEG C
Under the conditions of, carry out the rheotaxial growth of flux growth metrhod gallium nitride single crystal.
Comparative example 2：This reference examples is substantially the same manner as Example 2, but instead of the activity after nitridation using commercially available activated carbon
Charcoal.
Embodiment 3：In the glove box of exhausted water anoxybiotic by mass ratio be 10：The gallium and metallic sodium of (11.0~15.0)
Mixed in crucible, then be separately added into the graphene after nitridation, CNT, graphite (addition is metallic sodium, gallium total amount
0.6~1.0mol%), gallium nitride seed crystal is added afterwards, is then transferred in epitaxial growth equipment, is 9~10MPa in pressure,
Under conditions of temperature is 950~1000 DEG C, the rheotaxial growth of flux growth metrhod gallium nitride single crystal is carried out.
Refer to Fig. 1-Fig. 2, it can be seen that by being nitrogenized in being added in the system of flux growth metrhod growing gallium nitride single crystal
Carbon material afterwards, as additive, can more effectively suppress gallium nitride polycrystalline as additive than using common carbon material
Formation, promote gallium nitride seed crystal rheotaxial growth, but also the seed crystal that can effectively reduce gallium nitride seeded growth early stage returns
It is molten.
It should be appreciated that the technical concepts and features of above-described embodiment only to illustrate the invention, its object is to allow be familiar with this
The personage of item technology can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention.It is all
The equivalent change or modification made according to spirit of the invention, it should all be included within the scope of the present invention.
Claims (10)
1. promote the method for seed crystal liquid phase epitaxy in a kind of flux growth metrhod growth GaN single crystal system, it is characterised in that including：With
During flux growth metrhod growing gallium nitride single crystal, in adding carbonaceous additive in the growth system of gallium nitride single crystal, the carbon adds
Agent is added to include the carbon material after nitridation.
2. promoting the method for seed crystal liquid phase epitaxy in flux growth metrhod growth GaN single crystal system according to claim 1, it is special
Sign is to include：In anhydrous and oxygen-free environment, metallic sodium, gallium, carbonaceous additive are uniformly mixed with gallium nitride seed crystal, afterwards
The rheotaxial growth of gallium nitride single crystal is carried out with flux growth metrhod.
3. promote the method for seed crystal liquid phase epitaxy in flux growth metrhod growth GaN single crystal system according to claim 1 or 2,
It is characterized in that：The dosage of the carbonaceous additive is metallic sodium and gallium total amount in gallium nitride single crystal growth system
0.005mol%~1.0mol%.
4. promoting the method for seed crystal liquid phase epitaxy in flux growth metrhod growth GaN single crystal system according to claim 2, it is special
Sign is：For the reaction temperature used in the flux growth metrhod for 700~1000 DEG C, reaction pressure is 3~10MPa.
5. promoting the method for seed crystal liquid phase epitaxy in flux growth metrhod growth GaN single crystal system according to claim 1, it is special
Sign is：The carbonaceous additive is using the carbon material after nitridation.
6. promoting the method for seed crystal liquid phase epitaxy in flux growth metrhod growth GaN single crystal system according to claim 1, it is special
Sign is：Carbon material after the nitridation includes appointing in graphite, graphene, activated carbon, CNT and the mesoporous carbon of nitridation
The combination for one or more of anticipating.
7. promoting the method for seed crystal liquid phase epitaxy in flux growth metrhod growth GaN single crystal system according to claim 1, it is special
Sign is to include：Carbon source is subjected to high-temperature ammonolysis processing, the carbon material formed after the nitridation in nitrogen containing atmosphere；Or will
Carbon source carries out high-temperature ammonolysis processing after being mixed with nitrogen source, obtains the carbon material after the nitridation.
8. promoting the method for seed crystal liquid phase epitaxy in flux growth metrhod growth GaN single crystal system according to claim 7, it is special
Sign is：The carbon source includes any one in graphite, graphene, activated carbon, CNT and mesoporous carbon or two or more
Combination；And/or the nitrogen source includes melamine；And/or the nitrogen containing atmosphere includes nitrogen or ammonia atmosphere.
9. promote the method for seed crystal liquid phase epitaxy in a kind of flux growth metrhod growth GaN single crystal system, it is characterised in that including：
In anhydrous and oxygen-free environment, metallic sodium is mixed with gallium, sequentially adds carbon material and gallium nitride after nitridation afterwards
Seed crystal, form the growth system of gallium nitride single crystal；
The growth system of the gallium nitride single crystal is transferred in epitaxial growth equipment, pressure be 3~10MPa, temperature 700
Under the conditions of~1000 DEG C, the rheotaxial growth of gallium nitride single crystal is carried out.
10. promote the method for seed crystal liquid phase epitaxy in flux growth metrhod growth GaN single crystal system according to claim 9, its
It is characterised by：The dosage of carbon material after the nitridation is metallic sodium and gallium total amount in gallium nitride single crystal growth system
0.005mol%~1.0mol%；And/or the carbon material after the nitridation includes graphite, graphene, activated carbon, the carbon of nitridation
Any one in nanotube and mesoporous carbon or two or more combinations.
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Cited By (7)
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|---|---|---|---|---|
| CN108796611A (en) * | 2018-07-06 | 2018-11-13 | 孟静 | Gallium nitride single crystal growing method |
| CN110735178A (en) * | 2018-07-19 | 2020-01-31 | 通用汽车环球科技运作有限责任公司 | System and method for binary single crystal growth |
| CN111434811A (en) * | 2019-01-14 | 2020-07-21 | 中国科学院苏州纳米技术与纳米仿生研究所 | Self-separating gallium nitride single crystal and growth method thereof by flux method |
| CN111434809A (en) * | 2019-01-14 | 2020-07-21 | 中国科学院苏州纳米技术与纳米仿生研究所 | Non-polar/semi-polar gallium nitride single crystal and growth method thereof by flux method |
| CN112899784A (en) * | 2021-01-20 | 2021-06-04 | 中国科学院苏州纳米技术与纳米仿生研究所 | Gallium nitride (11-22) single crystal substrate and method for producing same |
| CN113502544A (en) * | 2021-07-14 | 2021-10-15 | 东莞理工学院 | Large-size GaN crystal and preparation method thereof |
| CN114657640A (en) * | 2020-12-23 | 2022-06-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | High-quality gallium nitride single crystal and growth method and preparation system thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108796611A (en) * | 2018-07-06 | 2018-11-13 | 孟静 | Gallium nitride single crystal growing method |
| CN110735178A (en) * | 2018-07-19 | 2020-01-31 | 通用汽车环球科技运作有限责任公司 | System and method for binary single crystal growth |
| CN111434811A (en) * | 2019-01-14 | 2020-07-21 | 中国科学院苏州纳米技术与纳米仿生研究所 | Self-separating gallium nitride single crystal and growth method thereof by flux method |
| CN111434809A (en) * | 2019-01-14 | 2020-07-21 | 中国科学院苏州纳米技术与纳米仿生研究所 | Non-polar/semi-polar gallium nitride single crystal and growth method thereof by flux method |
| CN111434811B (en) * | 2019-01-14 | 2022-04-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Self-separating gallium nitride single crystal and growth method thereof by flux method |
| CN111434809B (en) * | 2019-01-14 | 2022-04-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Non-polar/semi-polar gallium nitride single crystal and growth method thereof by flux method |
| CN114657640A (en) * | 2020-12-23 | 2022-06-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | High-quality gallium nitride single crystal and growth method and preparation system thereof |
| CN112899784A (en) * | 2021-01-20 | 2021-06-04 | 中国科学院苏州纳米技术与纳米仿生研究所 | Gallium nitride (11-22) single crystal substrate and method for producing same |
| CN112899784B (en) * | 2021-01-20 | 2022-06-17 | 中国科学院苏州纳米技术与纳米仿生研究所 | Gallium nitride (11-22) single crystal substrate and method for producing same |
| CN113502544A (en) * | 2021-07-14 | 2021-10-15 | 东莞理工学院 | Large-size GaN crystal and preparation method thereof |
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