CN111434809A - Non-polar/semi-polar gallium nitride single crystal and growth method thereof by flux method - Google Patents
Non-polar/semi-polar gallium nitride single crystal and growth method thereof by flux method Download PDFInfo
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- CN111434809A CN111434809A CN201910038242.2A CN201910038242A CN111434809A CN 111434809 A CN111434809 A CN 111434809A CN 201910038242 A CN201910038242 A CN 201910038242A CN 111434809 A CN111434809 A CN 111434809A
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- 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
- C30B19/00—Liquid-phase epitaxial-layer growth
- C30B19/02—Liquid-phase epitaxial-layer growth using molten solvents, e.g. flux
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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
Abstract
The invention discloses a method for growing nonpolar/semipolar gallium nitride single crystals by a fluxing agent method, which comprises the following steps: cleaving the gallium nitride wafer along the selected cleavage plane, and arranging the obtained gallium nitride wafers into an array to obtain a cleaved-plane gallium nitride single crystal array; and taking the cleavage plane gallium nitride single crystal array as a seed crystal, and carrying out liquid phase epitaxy and combined growth by using a fluxing agent method to obtain the nonpolar/semipolar gallium nitride single crystal along the cleavage plane. Compared with the prior art, the method utilizes the nonpolar/semipolar gallium nitride single crystal array which has uniform quality and is used as seed crystal in the process of growing the gallium nitride by the fluxing agent method liquid phase epitaxy, obtains the nonpolar/semipolar gallium nitride single crystal with higher quality by the combined growth of the liquid phase epitaxy, and further adopts the gallium nitride single crystal to carry out the liquid phase epitaxy, thereby obtaining the nonpolar/semipolar gallium nitride single crystal.
Description
Technical Field
The invention relates to a preparation method of nitride single crystal, in particular to a method for growing nonpolar/semipolar gallium nitride single crystal by a fluxing agent method.
Background
Because gallium nitride single crystal is a strong polarization material, usually have polarization field in the growth direction (c-direction), the experiment proves, adopt gallium nitride material of the particular growth direction (nonpolar/semipolar direction), can avoid the influence that the polarization field brings in the material inside, further raise the performance of the device.
Taking m-plane (10-10) gallium nitride as an example, a common method for obtaining an m-plane gallium nitride single crystal is to obtain a c-plane (0001) gallium nitride single crystal with a centimeter-level thickness (1-5 cm) by a vapor phase method (mainly HVPE method), then an m-plane nonpolar/semipolar gallium nitride single crystal (as shown in fig. 1) is cut from the inside of the bulk single crystal perpendicular to the c-plane, however, the growth process of the c-plane gallium nitride bulk single crystal to obtain a centimeter-level thickness is difficult compared to the growth process of the c-plane gallium nitride wafer, and cutting m-plane gallium nitride from a single crystal of c-plane gallium nitride having a thickness of cm-order results in a high cost of the wafer, and further, since there is a quality unevenness of the gallium nitride bulk single crystal in the growth direction (for example, the crystal dislocation density gradually decreases as the growth thickness increases), there is an unevenness in the in-plane photoelectric properties of the obtained m-plane gallium nitride.
Disclosure of Invention
The invention mainly aims to provide a nonpolar/semipolar gallium nitride single crystal and a growth method thereof by a flux method, so as to overcome the defects in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a method for growing nonpolar/semipolar gallium nitride single crystals by a fluxing agent method, which comprises the following steps:
cleaving the gallium nitride wafer along the selected cleavage plane, and arranging the obtained gallium nitride wafers into an array to obtain a cleaved-plane gallium nitride single crystal array;
and taking the cleavage plane gallium nitride single crystal array as a seed crystal, and carrying out liquid phase epitaxy and combined growth by using a fluxing agent method to obtain the nonpolar/semipolar gallium nitride single crystal along the cleavage plane.
In some embodiments, the cleavage plane is a non-polar or semi-polar plane, preferably an m-planeBut is not limited thereto. Further, the method for growing the nonpolar/semipolar gallium nitride single crystal by the flux method specifically comprises the following steps: along the m-plane of the gallium nitride waferAnd (3) physically cleaving the gallium nitride wafer to obtain strip seed crystals with the width of 2-5 mm, and then arranging the obtained strip seed crystals into an array to obtain the m-plane gallium nitride single crystal array.
The embodiment of the invention also provides the nonpolar/semipolar gallium nitride single crystal prepared by any one of the methods.
Further, the nonpolar/semipolar gallium nitride single crystal is a high-quality m-plane or other nonpolar/semipolar gallium nitride single crystal. Compared with the prior art, the method utilizes the nonpolar/semipolar gallium nitride single crystal array which has uniform quality and is used as seed crystal in the process of growing the gallium nitride by the fluxing agent method liquid phase epitaxy, obtains the nonpolar/semipolar gallium nitride single crystal with higher quality by the combined growth of the liquid phase epitaxy, and further adopts the gallium nitride single crystal to carry out the liquid phase epitaxy, thereby obtaining the nonpolar/semipolar gallium nitride single crystal.
Drawings
FIG. 1 is a schematic view showing a process of obtaining a c-plane (0001) gallium nitride single crystal by a vapor phase method and then cutting an m-plane gallium nitride single crystal from the inside of the single crystal perpendicular to the c-plane in the prior art.
FIG. 2 is a schematic diagram of a process for growing a nonpolar/semipolar gallium nitride single crystal by a flux method according to an exemplary embodiment of the present invention.
FIG. 3a is an SEM image of a nonpolar/semipolar gallium nitride single crystal obtained in an exemplary embodiment of the invention.
FIG. 3b is a cathode fluorescence (C L) test chart of a nonpolar/semipolar gallium nitride single crystal obtained in an exemplary embodiment of the present invention.
Detailed Description
The flux method (NaFlux method) has many advantages as one of the mainstream growth methods for obtaining high-quality and large-size gallium nitride single crystals at present, and the inventor finds that the growth method can be used for obtaining high-quality m-plane or other nonpolar/semipolar gallium nitride single crystals by liquid phase epitaxy for a long time. Based on the discovery, the inventor provides a method for growing nonpolar/semipolar gallium nitride single crystals by a flux method, in the process of growing the gallium nitride by the flux method liquid phase epitaxy, a nonpolar/semipolar gallium nitride single crystal array which is uniform in quality and used as seed crystals is utilized, the nonpolar/semipolar gallium nitride single crystals with higher quality are obtained by liquid phase epitaxy combined growth, and the nonpolar/semipolar gallium nitride single crystals are further adopted for liquid phase epitaxy, so that nonpolar/semipolar gallium nitride body single crystals can be obtained.
More specifically, an aspect of the embodiments of the present invention provides a method for growing a nonpolar/semipolar gallium nitride single crystal by a flux method, including:
cleaving the gallium nitride wafer along the selected cleavage plane, and arranging the obtained gallium nitride wafers into an array to obtain a cleaved-plane gallium nitride single crystal array;
and taking the cleavage plane gallium nitride single crystal array as a seed crystal, and carrying out liquid phase epitaxy and combined growth by using a fluxing agent method to obtain the nonpolar/semipolar gallium nitride single crystal along the cleavage plane.
In some embodiments, the method of flux-growth of a nonpolar/semipolar gallium nitride single crystal further comprises: and further carrying out liquid phase epitaxial growth on the cleavage plane gallium nitride single crystal to obtain the nonpolar/semipolar gallium nitride single crystal.
In some embodiments, the flux method for growing a nonpolar/semipolar gallium nitride single crystal comprises: a free-standing gallium nitride wafer having a growth direction of c-direction was formed by vapor phase epitaxy (mainly HVPE).
Further, the size of the gallium nitride wafer is 2-6 inches.
Furthermore, the thickness of the gallium nitride wafer is 300-800 μm, wherein the maximum thickness of the 6-inch gallium nitride wafer can reach 800 μm.
In some embodiments, the cleavage plane may be a non-polar plane (e.g., m-plane) or a semi-polar plane, but is not limited thereto.
In a preferred embodiment, the method for growing the nonpolar/semipolar gallium nitride single crystal by the flux method specifically comprises the following steps: along the m-plane of the gallium nitride waferAnd (3) physically cleaving the gallium nitride wafer to obtain strip seed crystals with the width of 2-5 mm, and then arranging the obtained strip seed crystals into an array to obtain the m-plane gallium nitride single crystal array.
Further, the gap distance between two adjacent long-strip seed crystals is 0-500 μm.
Further, the m-plane gallium nitride single crystal array comprises more than two long-strip seed crystals.
Further, the size of the nonpolar/semipolar gallium nitride single crystal is 10mm × 10 mm-150 mm × 150mm, and the thickness is 0.5-5 mm.
In a preferred embodiment, the method for growing the nonpolar/semipolar gallium nitride single crystal by the flux method specifically comprises the following steps: in an anhydrous and oxygen-free environment, metal sodium, metal gallium and carbon nitride additives are uniformly mixed with an m-plane gallium nitride single crystal array serving as seed crystals, liquid phase epitaxy merging growth is firstly carried out by a fluxing agent method under the conditions of 3-10 MPa pressure and 700-1000 ℃, an m-plane gallium nitride single crystal film is obtained, and then m-plane nonpolar/semipolar gallium nitride single crystals are obtained by further liquid phase epitaxy growth.
Another aspect of an embodiment of the present invention provides a nonpolar/semipolar gallium nitride single crystal prepared by any one of the aforementioned methods.
In conclusion, in the process of growing gallium nitride by flux-method liquid phase epitaxy, the nonpolar/semipolar gallium nitride single crystal array which is uniform in quality and is used as seed crystal is utilized, the nonpolar/semipolar gallium nitride single crystal with higher quality is obtained by liquid phase epitaxy combined growth, and the nonpolar/semipolar gallium nitride single crystal can be obtained by further adopting the gallium nitride single crystal to carry out liquid phase epitaxy.
The technical solution of the present invention will be further explained with reference to the following examples.
Referring to fig. 2, taking m-plane gallium nitride (GaN) as an example, the method for growing a nonpolar/semipolar gallium nitride single crystal by the flux method according to the present embodiment includes the following steps:
the first step is as follows: selecting a self-supporting uniform epitaxial GaN wafer (growth direction is c direction) obtained by vapor phase epitaxy (mainly HVPE method), the size is 2-6 inches, the thickness is 300-800 μm, and then the GaN wafer is arranged along the m surfaceAnd physically cleaving to obtain long-strip seed crystals with the width of 2-5 mm, wherein the longer side surfaces (m surfaces) of the long-strip seed crystals are seed crystal surfaces to be subjected to liquid phase epitaxy, then arranging a plurality of seed crystals obtained in the manner into an array, wherein the gap distance between the two seed crystals is 0-500 mu m, and the m surfaces of the long-strip seed crystals obtained after cleaving are all placed upwards.
And secondly, taking the m-plane GaN single crystal array obtained in the mode as a seed crystal, and obtaining the m-plane GaN single crystal by utilizing a flux method liquid phase epitaxy merging growth, wherein as shown in fig. 3a and fig. 3b, 2 m-plane long GaN seed crystals are adopted, and the uniformity in the epitaxial crystal plane is better after the liquid phase epitaxy merging growth of the m-plane GaN single crystal, fig. 3a is an SEM (scanning electron microscope) diagram of the nonpolar/semipolar gallium nitride single crystal obtained in the embodiment, fig. 3b is a cathode fluorescence (C L) test diagram of the nonpolar/semipolar gallium nitride single crystal obtained in the embodiment, the number and the size of the long GaN seed crystals are further increased, and the m-plane GaN bulk single crystal (the thickness is 0.5-5 mm) with large size (10mm × 10 mm-150 mm × 150mm), high quality and uniform quality can be obtained.
In the second step, the process of growing the nonpolar/semipolar gallium nitride single crystal by liquid phase epitaxy specifically includes: putting metal sodium, metal gallium and a carbon nitride additive (the addition ratio is 0.005-1.0 mol% of the total amount of the metal sodium and the metal gallium) and a nonpolar/semipolar gallium nitride seed crystal array into a crucible in a glove box without water and oxygen, then transferring the crucible into liquid phase epitaxial growth equipment, firstly carrying out liquid phase epitaxy and growth under the conditions of 3-10 MPa pressure and 700-1000 ℃, obtaining an m-plane gallium nitride single crystal film, and then further carrying out liquid phase epitaxy growth to obtain an m-plane nonpolar/semipolar gallium nitride single crystal.
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, which are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and therefore, the protection scope of the present invention is not limited thereby. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. A method for growing nonpolar/semipolar gallium nitride single crystal by flux method is characterized by comprising:
cleaving the gallium nitride wafer along the selected cleavage plane, and arranging the obtained gallium nitride wafers into an array to obtain a cleaved-plane gallium nitride single crystal array;
and taking the cleavage plane gallium nitride single crystal array as a seed crystal, and carrying out liquid phase epitaxy and combined growth by using a fluxing agent method to obtain the nonpolar/semipolar gallium nitride single crystal along the cleavage plane.
2. The flux-assisted growth method of nonpolar/semipolar gallium nitride single crystal according to claim 1, further comprising: and further carrying out liquid phase epitaxial growth on the cleavage plane gallium nitride single crystal to obtain the nonpolar/semipolar gallium nitride single crystal.
3. The flux-based method for growing a nonpolar/semipolar gallium nitride single crystal according to claim 1, comprising: a self-supporting gallium nitride wafer with a growth direction of c-direction is formed by vapor phase epitaxy.
4. The flux-based method for growing a nonpolar/semipolar gallium nitride single crystal according to claim 3, wherein: the size of the gallium nitride wafer is 2-6 inches; and/or the thickness of the gallium nitride wafer is 300-800 μm.
5. The flux-based method for growing a nonpolar/semipolar gallium nitride single crystal according to claim 1, wherein: the cleavage surface is a nonpolar surface or a semipolar surface; preferably, the cleavage plane is an m-plane
Preferably, the method for growing the nonpolar/semipolar gallium nitride single crystal by the flux method specifically comprises the following steps: along the m-plane of the gallium nitride waferAnd (3) physically cleaving the gallium nitride wafer to obtain strip seed crystals with the width of 2-5 mm, and then arranging the obtained strip seed crystals into an array to obtain the m-plane gallium nitride single crystal array.
6. The flux-based method for growing a nonpolar/semipolar gallium nitride single crystal according to claim 5, wherein: the gap distance between two adjacent long-strip seed crystals is 0-500 mu m.
7. The flux-based method for growing a nonpolar/semipolar gallium nitride single crystal according to claim 5, wherein: the m-plane gallium nitride single crystal array comprises more than two long-strip seed crystals.
8. The method for growing the nonpolar/semipolar gallium nitride single crystal by the flux method according to claim 2, wherein the nonpolar/semipolar gallium nitride single crystal has a size of 10mm × 10 mm-150 mm × 150mm and a thickness of 0.5-5 mm.
9. The method for growing the nonpolar/semipolar gallium nitride single crystal by the flux method according to claim 5, which comprises: in an anhydrous and oxygen-free environment, metal sodium, metal gallium and carbon nitride additives are uniformly mixed with an m-plane gallium nitride single crystal array serving as seed crystals, liquid phase epitaxy merging growth is firstly carried out by a fluxing agent method under the conditions of 3-10 MPa pressure and 700-1000 ℃, an m-plane gallium nitride single crystal film is obtained, and then m-plane nonpolar/semipolar gallium nitride single crystals are obtained by further liquid phase epitaxy growth.
10. A non-polar/semi-polar gallium nitride single crystal prepared by the method of any one of claims 1-9.
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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 |
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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 |
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