CN111434811A - Self-separating gallium nitride single crystal and growth method thereof by flux method - Google Patents
Self-separating gallium nitride single crystal and growth method thereof by flux method Download PDFInfo
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- CN111434811A CN111434811A CN201910031985.7A CN201910031985A CN111434811A CN 111434811 A CN111434811 A CN 111434811A CN 201910031985 A CN201910031985 A CN 201910031985A CN 111434811 A CN111434811 A CN 111434811A
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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
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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
- C30B19/04—Liquid-phase epitaxial-layer growth using molten solvents, e.g. flux the solvent being a component of the crystal composition
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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
- 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
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Abstract
The invention discloses a method for growing self-separating gallium nitride single crystal by a fluxing agent method, which comprises the following steps: growing a microporous layer on the self-supporting gallium nitride by adopting a fluxing agent method and taking the self-supporting gallium nitride as a seed crystal; and growing the self-separation gallium nitride single crystal on the micropore layer by using a liquid phase epitaxy method. Compared with the prior art, the growth condition of growing the gallium nitride single crystal by the flux method is controlled, a microporous layer is grown firstly, the microporous layer can effectively release the stress in the seed crystal and inhibit most of dislocation in the seed crystal in the microporous layer, so that the stress cannot be introduced in the subsequent liquid phase epitaxial growth of the gallium nitride single crystal, and the self-separation phenomenon can occur in the layer after the growth, and the high-quality self-separation gallium nitride single crystal is further grown.
Description
Technical Field
The invention relates to a preparation method of nitride single crystals, in particular to a method for growing self-separation gallium nitride single crystals by a fluxing agent method.
Background
Flux method (Na Flux method) has many advantages as one of the mainstream growth methods for obtaining high-quality large-size gallium nitride (GaN) bulk single crystals at present. However, a bulk single crystal of gallium nitride is grown by flux method, and Free-standing GaN (HVPE) or MOCVD (metal organic chemical vapor deposition) gallium nitride (GaN is formed on sapphire) is generally used as a seed crystal. GaN by an HVPE method is taken as seed crystal, and because the seed crystal has larger stress, a GaN single crystal grown by a fluxing agent method also has larger stress, and crystal face warping can occur in serious cases; and because the thermal expansion coefficient between GaN and sapphire is different, the temperature reduction process of growing GaN single crystal by the fluxing agent method can generate larger thermal stress, and the crystal can generate microcracks in serious conditions. Therefore, the flux method is used for growing the gallium nitride single crystal, and the most ideal gallium nitride seed crystal is that the seed crystal is close to a stress-free state and does not have a substrate made of other materials (such as sapphire, SiC and the like), namely, no lattice mismatch or thermal mismatch exists between the seed crystal and the epitaxial single crystal. To date, there is no report in the industry, and this problem has been the direction of efforts of researchers in the industry for a long time.
Disclosure of Invention
The invention mainly aims to provide a self-separating 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 self-separation gallium nitride single crystals by a fluxing agent method, which comprises the following steps:
growing a microporous layer on the self-supporting gallium nitride by adopting a fluxing agent method and taking the self-supporting gallium nitride as a seed crystal; and
and growing a self-separation gallium nitride single crystal on the micropore layer by using a liquid phase epitaxy method.
In some embodiments, the flux method for growing a self-separating gallium nitride single crystal comprises: and growing a microporous layer on the self-supporting gallium nitride under the conditions that the pressure is 5-8 MPa and the temperature is 700-850 ℃.
In some embodiments, the flux method for growing a self-separating gallium nitride single crystal comprises: in an anhydrous and oxygen-free environment, uniformly mixing a metal sodium, a metal gallium and a carbon nitride additive with self-supporting gallium nitride prepared by an HVPE method, firstly growing a microporous layer under the conditions of 5-8 MPa of pressure and 700-850 ℃, and then further growing a gallium nitride single crystal by liquid phase epitaxy under the conditions of 3-10 MPa of pressure and 700-1000 ℃ to obtain the self-separating gallium nitride single crystal.
The embodiment of the invention also provides the self-separating gallium nitride single crystal prepared by any one of the methods.
Compared with the prior art, the growth condition of growing the gallium nitride single crystal by the flux method is controlled, a microporous layer is grown firstly, the microporous layer can effectively release the stress in the seed crystal and inhibit most of dislocation in the seed crystal in the microporous layer, so that the stress cannot be introduced in the subsequent liquid phase epitaxial growth of the gallium nitride single crystal, and the self-separation phenomenon can occur in the layer after the growth, and the high-quality self-separation gallium nitride single crystal is further grown.
Drawings
FIG. 1 is a schematic illustration of flux-grown self-segregated GaN single crystals using a self-growing microporous layer in an exemplary embodiment of the invention.
Fig. 2a and 2b are SEM images and cathodofluorescence (C L) test images of a cross-section of a self-segregated gallium nitride single crystal obtained in an exemplary embodiment of the present invention, respectively.
Fig. 3a and 3b are SEM images and cathode fluorescence (C L) test images of an interface after separation from a separated gallium nitride single crystal obtained in an exemplary embodiment of the present invention, respectively.
FIGS. 4a and 4b are photographs of a separated Na Flux-GaN and GaN seed crystal from a separated GaN single crystal according to an exemplary embodiment of the invention.
Detailed Description
The fluxing agent method is used for growing gallium nitride single crystal, and the most ideal gallium nitride seed crystal is that the seed crystal is close to a stress-free state and does not have a substrate made of other materials (such as sapphire, SiC and the like), namely, no lattice mismatch or thermal mismatch exists between the seed crystal and the epitaxial single crystal. In order to obtain relatively ideal seed crystals, the inventor finds that high-quality self-separation gallium nitride single crystals can be obtained by firstly growing a microporous layer and further growing by using HVPE self-supporting GaN as the seed crystal and controlling the growth conditions of the flux method for growing the gallium nitride single crystals. Based on this finding, the present inventors have proposed a method for obtaining a self-separating gallium nitride single crystal by growing a microporous layer.
More specifically, an aspect of the embodiments of the present invention provides a method for growing a self-separating gallium nitride single crystal by a flux method, including:
growing a microporous layer on the self-supporting gallium nitride by adopting a fluxing agent method and taking the self-supporting gallium nitride as a seed crystal; and
and growing a self-separation gallium nitride single crystal on the micropore layer by using a liquid phase epitaxy method.
In some embodiments, the flux method for growing a self-separating gallium nitride single crystal comprises: and preparing the self-supporting gallium nitride by using an HVPE method to serve as seed crystals.
In some embodiments, the method for growing a self-separating gallium nitride single crystal by the flux method specifically comprises the following steps: and growing a microporous layer on the self-supporting gallium nitride under the conditions that the pressure is 5-8 MPa and the temperature is 700-850 ℃.
Further, the thickness of the microporous layer is 30-150 μm.
Furthermore, the diameter of micropores contained in the micropore layer is 5 nm-1 mu m, and the porosity is 30-80%.
Further, the arrangement of the micropores is not limited, and the pores are distributed in the pore layer, are irregular pores and are naturally distributed, as long as self-separation can occur.
Furthermore, the microporous layer contains a large number of micropores (Micro-Void), the microporous layer can effectively release stress in seed crystals, so that stress cannot be introduced into subsequent liquid phase epitaxial growth of gallium nitride single crystals, and the microporous layer belongs to weak connection and can generate a self-separation phenomenon in the layer after growth.
In some embodiments, the method for growing a self-separating gallium nitride single crystal by the flux method specifically comprises the following steps: and growing the self-separation gallium nitride single crystal on the microporous layer by using a liquid phase epitaxy method under the conditions that the pressure is 3-10 MPa and the temperature is 700-1000 ℃.
Further, the thickness of the self-separating gallium nitride single crystal is more than 300 μm.
In a more preferred embodiment, the method for growing a self-separating gallium nitride single crystal by the flux method specifically includes: in an anhydrous and oxygen-free environment, uniformly mixing 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) with self-supporting gallium nitride prepared by an HVPE method, firstly growing a microporous layer under the conditions of 5-8 MPa of pressure and 700-850 ℃, and then further growing a gallium nitride single crystal by liquid phase epitaxy under the conditions of 3-10 MPa of pressure and 700-1000 ℃ to obtain the self-separating gallium nitride single crystal.
Further, the microporous layer fracture occurs self-separation during or after the growth of the gallium nitride single crystal.
Further, in the process of growing the gallium nitride single crystal, the pressure and temperature ranges are as described above, and natural separation is achieved by growing the void layer using weak connection of the void layer without external application conditions. The separation occurs during the growth process or during the cooling process, depending on the thickness of the growth of the interstitial layer.
Another aspect of an embodiment of the present invention provides a self-separating gallium nitride single crystal prepared by any one of the methods described above.
In summary, the present invention controls the growth conditions of the flux method for growing the gallium nitride single crystal, and firstly grows a microporous layer, which not only can effectively release the stress in the seed crystal, but also can inhibit most of dislocation in the seed crystal in the microporous layer, so that the stress can not be introduced in the subsequent liquid phase epitaxial growth of the gallium nitride single crystal, and also can generate the self-separation phenomenon in the layer after the growth, and further grow and obtain the high quality self-separation gallium nitride single crystal.
The technical solution of the present invention will be further explained with reference to the following examples.
Example 1
The method for growing the self-separation gallium nitride single crystal by the flux method comprises the following steps:
first, using flux method, using HVPE method self-supporting gallium nitride as seed crystal, by controlling the growth conditions of 5MPa pressure and 700 deg.C temperature, a microporous layer is grown on the seed crystal, the layer contains a large number of micropores, wherein the diameter of the micropores is 5nm, the thickness of the microporous layer is 30 μm, the porosity is 30%, the microporous layer not only can make the stress in the seed crystal effectively released, so that the stress will not be introduced in the subsequent liquid phase epitaxial growth single crystal, but also after the growth, the self-separation phenomenon (as shown in FIG. 1) can occur in the layer, further analysis shows that the self-separation occurs in the microporous layer because the microporous layer is weak connection, as shown in FIGS. 2a and 2b, the cross section C L of the single crystal GaN after flux method growth, the separated area shows that the self-separation occurs in the microporous layer, furthermore, the inventor found through the research on the separation that most of the seed crystal is suppressed in the microporous layer, and does not further extend into the epitaxial single crystal (as shown in FIGS. 3 a-3 b), the dislocation layer is visible in the black arrow mark of the microporous layer after the growth of the single crystal by flux method, the subsequent growth of the microporous layer, the epitaxial growth of the gallium nitride, the flux is not merged dislocation line, and the subsequent single crystal grown by the flux method.
The second step is that: high-quality self-separation gallium nitride single crystal can be obtained after further growth under the conditions of the pressure of 3MPa and the temperature of 800 ℃, for example, a picture of the gallium nitride single crystal by a flux method after separation is shown in figure 4a, and a picture of a GaN seed crystal is shown in figure 4 b.
The process of self-separating gallium nitride single crystal by liquid phase epitaxial growth specifically comprises the following steps: in a glove box without water and oxygen, metal sodium, metal gallium, a carbon nitride additive (the addition ratio is 0.005mol percent of the total amount of the metal sodium and the metal gallium) and gallium nitride seed crystals by an HVPE method are put into a crucible, then the crucible is transferred into liquid phase epitaxial growth equipment, a microporous layer is firstly grown under the conditions of the pressure of 5MPa and the temperature of 700 ℃, and then gallium nitride single crystals are further grown under the conditions of the pressure of 3MPa and the temperature of 800 ℃. After the growth is finished, the high-quality self-separation gallium nitride single crystal can be obtained.
Example 2
A fluxing agent method is adopted, metal sodium, metal gallium, carbon nitride additive (adding proportion: accounting for 0.1mol percent of the total amount of the metal sodium and the metal gallium) and HVPE method self-supporting gallium nitride seed crystal are placed in a crucible in a glove box without water and oxygen, and then transferred to liquid phase epitaxial growth equipment, and growth conditions are controlled as follows: a microporous layer is first grown on a seed crystal under a pressure of 6MPa and a temperature of 800 ℃, wherein the diameter of micropores is 100nm, the thickness of the microporous layer is 100 μm, the porosity is 60%, and then a gallium nitride single crystal is further grown under a pressure of 8MPa and a temperature of 700 ℃. After the growth is finished, the high-quality self-separation gallium nitride single crystal can be obtained.
Example 3
A fluxing agent method is adopted, metal sodium, metal gallium, carbon nitride additive (adding proportion: 1.0mol percent of the total amount of the metal sodium and the metal gallium) and HVPE method self-supporting gallium nitride seed crystal are placed in a crucible in a glove box without water and oxygen, and then transferred to liquid phase epitaxial growth equipment, and growth conditions are controlled as follows: a microporous layer is first grown on the seed crystal under a pressure of 8MPa and a temperature of 850 ℃, wherein the diameter of micropores is 1 μm, the thickness of the microporous layer is 150 μm, and the porosity is 80%, and then gallium nitride single crystals are further grown under a pressure of 10MPa and a temperature of 1000 ℃. After the growth is finished, the high-quality self-separation gallium nitride single crystal can be obtained.
In addition, the inventor also carries out corresponding experiments by using other raw materials and other process conditions listed above to replace various raw materials and corresponding process conditions in the examples 1 to 3, and can obtain high-quality self-separation gallium nitride single crystals, which are basically similar to the products of the example 1.
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 self-separating gallium nitride single crystal by a flux method is characterized by comprising the following steps:
growing a microporous layer on the self-supporting gallium nitride by adopting a fluxing agent method and taking the self-supporting gallium nitride as a seed crystal; and
and growing a self-separation gallium nitride single crystal on the micropore layer by using a liquid phase epitaxy method.
2. The flux-assisted growth method for a self-separating gallium nitride single crystal according to claim 1, characterized by comprising: the self-supporting gallium nitride is prepared by HVPE method.
3. The flux-assisted growth method for self-separating gallium nitride single crystals according to claim 1, characterized by specifically comprising: and growing a microporous layer on the self-supporting gallium nitride under the conditions that the pressure is 5-8 MPa and the temperature is 700-850 ℃.
4. The flux method for growing a self-separating gallium nitride single crystal according to claim 1 or 3, characterized in that: the thickness of the microporous layer is 30-150 mu m.
5. The flux method for growing a self-separating gallium nitride single crystal according to claim 1 or 3, characterized in that: the diameter of micropores contained in the microporous layer is 5 nm-1 mu m, and the porosity is 30-80%.
6. The flux-assisted growth method for self-separating gallium nitride single crystals according to claim 1, characterized by specifically comprising: and growing the self-separation gallium nitride single crystal on the microporous layer by using a liquid phase epitaxy method under the conditions that the pressure is 3-10 MPa and the temperature is 700-1000 ℃.
7. The flux-assisted growth method for self-separating gallium nitride single crystal according to claim 1, characterized in that: the thickness of the self-separating gallium nitride single crystal is more than 300 mu m.
8. The flux-assisted growth method for self-separating gallium nitride single crystals according to claim 1, characterized by specifically comprising: in an anhydrous and oxygen-free environment, uniformly mixing a metal sodium, a metal gallium and a carbon nitride additive with self-supporting gallium nitride prepared by an HVPE method, firstly growing a microporous layer under the conditions of 5-8 MPa of pressure and 700-850 ℃, and then further growing a gallium nitride single crystal by liquid phase epitaxy under the conditions of 3-10 MPa of pressure and 700-1000 ℃ to obtain the self-separating gallium nitride single crystal.
9. The flux-assisted growth method for self-separating gallium nitride single crystal according to claim 8, characterized in that: the microporous layer fracture self-separates during or after growth of the gallium nitride single crystal.
10. A self-separating gallium nitride single crystal produced by the method of any one of claims 1-9.
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