CN116607217A - Large-size low-stress nitride epitaxial material and preparation method thereof - Google Patents
Large-size low-stress nitride epitaxial material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 72
- 150000004767 nitrides Chemical class 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000010410 layer Substances 0.000 claims abstract description 102
- 239000000758 substrate Substances 0.000 claims abstract description 70
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims abstract description 62
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 62
- 239000010980 sapphire Substances 0.000 claims abstract description 62
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 35
- 238000005240 physical vapour deposition Methods 0.000 claims abstract description 34
- 239000002346 layers by function Substances 0.000 claims abstract description 25
- 238000000151 deposition Methods 0.000 claims abstract description 10
- 229910002601 GaN Inorganic materials 0.000 claims description 70
- 239000012159 carrier gas Substances 0.000 claims description 63
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 claims description 54
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 42
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 40
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 36
- 239000001257 hydrogen Substances 0.000 claims description 34
- 229910052739 hydrogen Inorganic materials 0.000 claims description 34
- 230000004888 barrier function Effects 0.000 claims description 32
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 claims description 30
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 24
- RNQKDQAVIXDKAG-UHFFFAOYSA-N aluminum gallium Chemical compound [Al].[Ga] RNQKDQAVIXDKAG-UHFFFAOYSA-N 0.000 claims description 24
- 238000004544 sputter deposition Methods 0.000 claims description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 claims description 18
- 229910052782 aluminium Inorganic materials 0.000 claims description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 12
- 229910002704 AlGaN Inorganic materials 0.000 claims description 10
- 238000005086 pumping Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 abstract description 6
- 230000001276 controlling effect Effects 0.000 description 18
- 238000005336 cracking Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000001534 heteroepitaxy Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- 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
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/183—Epitaxial-layer growth characterised by the substrate being provided with a buffer layer, e.g. a lattice matching layer
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- 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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Abstract
The invention discloses a large-size low-stress nitride epitaxial material and a preparation method thereof, wherein the preparation method comprises the steps of adopting a physical vapor deposition method to deposit and generate a first three-dimensional columnar structure on a C-plane sapphire substrate; placing the C-plane sapphire substrate in an MOCVD reaction cavity, and generating an aluminum nitride epitaxial structure on the first three-dimensional columnar structure by utilizing an MOCVD process; depositing on the aluminum nitride epitaxial structure by adopting a physical vapor deposition method to generate a second three-dimensional columnar structure; placing the C-plane sapphire substrate in an MOCVD reaction cavity, and generating an epitaxial functional layer on the second three-dimensional columnar structure by utilizing an MOCVD process; the thickness of the epitaxial structure is far smaller than that of the traditional epitaxial material, so that the preparation time and the preparation cost of the epitaxial structure are greatly saved, and the stress release layer and the high-voltage-resistant regulating layer are not required to be designed due to the small thickness of the epitaxial structure, so that the preparation process and the preparation cost are further reduced.
Description
Technical Field
The invention relates to the technical field of gallium nitride material preparation, in particular to a large-size low-stress nitride epitaxial material and a preparation method thereof.
Background
With the development of industrial technology, high-power, high-current-density and high-conversion-efficiency devices are increasingly in accordance with the social requirements of future green development. And the third-generation semiconductor gallium nitride material and the device have the advantages of high power density, strong field and the like, and are increasingly favored by the market.
Currently, gallium nitride materials and devices are mainly used in epitaxy and fabrication on heterogeneous substrates. The problem of heteroepitaxy is that it brings about extremely large internal epitaxial stress and curvature due to thermal mismatch with the substrate, which is likely to cause bending and cracking of gallium nitride materials and devices, and the curvature is more important for gallium nitride materials and devices with large size of 6 to 8 inches.
The gallium nitride material and the device are prepared on the existing large-size substrate by mainly adopting the following three substrate materials: silicon substrate, sapphire substrate and silicon carbide substrate.
The technical route of the epitaxial material in the prior art mainly comprises the following steps:
firstly, an MOCVD technology is adopted to grow an aluminum nitride buffer layer to be used as nucleation, and a thicker stress regulating layer (such as graded AlGaN, gaN/AlGaN superlattice and the like) is grown again. In order to improve the pressure resistance of the material, carbon element and iron-doped element growth are also carried out to form a doped pressure-resistant layer, and then structural growth of a gallium nitride channel layer, an aluminum gallium nitride barrier layer and a gallium nitride cap layer is carried out to obtain an epitaxial material structure.
The epitaxial structure has the common characteristics that the epitaxial internal stress is relatively large, and the problems of thermal mismatch and the like caused by the need of balancing the substrate are not easy to cause cracking of gallium nitride materials and devices, so that the problem of cracking can be reduced only by growing epitaxial materials with the thickness of more than 3 microns.
The stress regulation problem of the substrate with 6 to 8 inches is more prominent in the technical route of the epitaxial material in the prior art, the phenomenon of cracking is easy to occur in the preparation of the chip at the rear end due to the internal stress of the epitaxial material with large size, a great challenge is brought to the product yield, and the development of gallium nitride materials and devices is severely restricted.
Disclosure of Invention
The invention aims to provide a large-size low-stress nitride epitaxial material and a preparation method thereof, wherein the thickness of an epitaxial structure is far smaller than that of a traditional epitaxial material, so that the preparation time and the preparation cost of the epitaxial structure are greatly saved, and a stress release layer and a high-pressure-resistance regulating layer are not required to be designed due to the small thickness of the epitaxial structure, so that the preparation process and the preparation cost are further reduced.
In order to achieve the above object, the present invention discloses a method for preparing a large-sized low-stress nitride epitaxial material, comprising the steps of:
s1, depositing on a C-plane sapphire substrate by adopting a physical vapor deposition method to generate a first three-dimensional columnar structure;
s2, placing the C-plane sapphire substrate in an MOCVD reaction cavity, and generating an aluminum nitride epitaxial structure on the first three-dimensional columnar structure by utilizing an MOCVD process;
s3, depositing on the aluminum nitride epitaxial structure by adopting a physical vapor deposition method to generate a second three-dimensional columnar structure;
and S4, placing the C-plane sapphire substrate in an MOCVD reaction cavity, and generating an epitaxial functional layer on the second three-dimensional columnar structure by utilizing an MOCVD process.
Compared with the prior art, the method sequentially generates the first three-dimensional columnar structure, the aluminum nitride epitaxial structure, the second three-dimensional columnar structure and the epitaxial functional layer on the C-plane sapphire substrate, is suitable for effectively reducing the thickness of the aluminum nitride epitaxial structure and the thickness of the epitaxial functional layer by additionally arranging the first three-dimensional columnar structure and the second three-dimensional columnar structure so as to reduce the thickness of a finished product material, greatly saves the preparation time and the preparation cost of the epitaxial structure because the thickness of the epitaxial structure is far smaller than the thickness of the traditional epitaxial material, and does not need to design a stress release layer and a high pressure-resistant regulating layer because the thickness of the epitaxial structure is small, and further reduces the preparation procedure and the preparation cost.
Preferably, the step S1 specifically includes:
s11, placing the C-plane sapphire substrate in a physical vapor deposition reaction cavity;
s12, pumping the vacuum degree of the physical vapor deposition reaction cavity to 5 x 10 -5 Pa；
S13, introducing argon and nitrogen into the physical vapor deposition reaction chamber, wherein the flow ratio of the argon to the nitrogen is 8:1, and controlling the vacuum degree of the physical vapor deposition reaction chamber to be 1Pa;
s13, preheating the C-plane sapphire substrate and the aluminum target to 200 ℃;
s14, performing direct-current sputtering on the C-plane sapphire substrate, wherein the sputtering power is 300W, the sputtering rate is 0.1nm/S, and the sputtering time is 100.00S, so that a first three-dimensional columnar structure is formed on the C-plane sapphire substrate by deposition.
Preferably, the step S2 specifically includes:
s21, placing the C-plane sapphire substrate in an MOCVD reaction cavity;
s22, setting the temperature of the MOCVD reaction chamber to 1100 ℃ and the air pressure to 50mbar;
s23, taking hydrogen as carrier gas, and introducing trimethylaluminum and ammonia gas into the MOCVD reaction chamber, wherein the five-three ratio of the trimethylaluminum to the ammonia gas is 500, so as to generate an aluminum nitride epitaxial structure on the first three-dimensional columnar structure;
s24, controlling the carrier gas rate and carrier gas time of the hydrogen so as to control the growth rate of the aluminum nitride epitaxial structure to be 0.2nm/S and the growth time to be 50.00S.
Preferably, the step S3 specifically includes:
s31, placing the C-plane sapphire substrate in a physical vapor deposition reaction cavity;
s32, pumping the vacuum degree of the physical vapor deposition reaction cavity to 5 x 10 -5 Pa；
S33, introducing argon and nitrogen into the physical vapor deposition reaction chamber, wherein the flow ratio of the argon to the nitrogen is 8:1, and controlling the vacuum degree of the physical vapor deposition reaction chamber to be 1Pa;
s34, preheating the C-plane sapphire substrate and the aluminum target to 200 ℃;
s35, performing direct-current sputtering on the C-plane sapphire substrate, wherein the sputtering power is 300W, the sputtering rate is 0.1nm/S, and the sputtering time is 100.00S, so as to deposit and generate a second three-dimensional columnar structure on the aluminum nitride epitaxial structure.
Preferably, the step S4 specifically includes:
s411, placing the C-plane sapphire substrate in an MOCVD reaction cavity;
s412, setting the temperature of the MOCVD reaction chamber to 1080 ℃ and the air pressure to 100mbar;
s413, introducing trimethyl gallium and ammonia gas into the MOCVD reaction chamber by taking hydrogen as carrier gas, wherein the five-three ratio of the trimethyl gallium to the ammonia gas is 1500, so as to generate a gallium nitride channel layer on the second three-dimensional columnar structure;
s414, controlling the carrier gas rate and carrier gas time of the hydrogen so as to control the growth rate of the gallium nitride channel layer to be 0.6nm/S and the growth time to be 375.00S;
s415, taking hydrogen as carrier gas, and introducing trimethyl gallium, trimethyl aluminum and ammonia gas into the MOCVD reaction chamber, wherein the five-three ratio of the trimethyl gallium to the trimethyl aluminum to the ammonia gas is 800, so as to generate an aluminum gallium nitrogen barrier layer on the gallium nitride channel layer;
s416, controlling the carrier gas rate and carrier gas time of the hydrogen so as to control the growth rate of the AlGaN barrier layer to be 0.4nm/S and the growth time to be 62.50S;
s417, using hydrogen as carrier gas, and introducing trimethyl gallium and ammonia gas into the MOCVD reaction chamber to generate a gallium nitride cap layer on the aluminum gallium nitride barrier layer;
s418, controlling the carrier gas rate and carrier gas time of the hydrogen so as to control the growth rate of the gallium nitride cap layer to be 0.5nm/S and the growth time to be 4.00S.
Specifically, the aluminum component of the aluminum gallium nitride barrier layer is 25%.
Preferably, the step S4 specifically includes:
s421, placing the C-plane sapphire substrate in an MOCVD reaction cavity;
s422, setting the temperature of the MOCVD reaction chamber to 1110 ℃ and the air pressure to 70mbar;
s423, using hydrogen as carrier gas, and introducing trimethyl gallium and ammonia gas into the MOCVD reaction chamber, wherein the five-three ratio of the trimethyl gallium to the ammonia gas is 1500, so as to generate a gallium nitride channel layer on the second three-dimensional columnar structure;
s424, controlling the carrier gas rate and carrier gas time of the hydrogen so as to control the growth rate of the gallium nitride channel layer to be 0.6nm/S and the growth time to be 333.33S;
s425, taking hydrogen as carrier gas, and introducing trimethyl gallium, trimethyl aluminum and ammonia gas into the MOCVD reaction cavity, wherein the five-three ratio of the trimethyl gallium, the trimethyl aluminum and the ammonia gas is 600, so as to generate an aluminum gallium nitrogen barrier layer on the gallium nitride channel layer;
s426, controlling the carrier gas rate and carrier gas time of the hydrogen so as to control the growth rate of the AlGaN barrier layer to be 0.3nm/S and the growth time to be 66.67S;
s427, using hydrogen as carrier gas, and introducing trimethyl gallium and ammonia gas into the MOCVD reaction chamber to generate a gallium nitride cap layer on the aluminum gallium nitride barrier layer;
s428, controlling the carrier gas rate and carrier gas time of the hydrogen so as to control the growth rate of the gallium nitride cap layer to be 0.5nm/S and the growth time to be 3.00S.
Specifically, the aluminum component of the aluminum gallium nitride barrier layer is 30%.
Preferably, the C-plane sapphire substrate has a size of 6 to 8 inches.
Correspondingly, the invention also discloses a large-size low-stress nitride epitaxial material which is prepared by the preparation method of the large-size low-stress nitride epitaxial material, wherein the large-size low-stress nitride epitaxial material comprises a C-surface sapphire substrate, and a first three-dimensional columnar structure, an aluminum nitride epitaxial structure, a second three-dimensional columnar structure and an epitaxial functional layer which are sequentially epitaxially generated on the C-surface sapphire substrate, wherein the epitaxial functional layer sequentially epitaxially generates a gallium nitride channel layer, an aluminum gallium nitride barrier layer and a gallium nitride cap layer on the second three-dimensional columnar structure.
Drawings
FIG. 1 is a flow chart of a method of fabricating a large-size low-stress nitride epitaxial material of the present invention;
FIG. 2 is a schematic diagram of the structure of a large-sized low-stress nitride epitaxial material of the present invention;
FIG. 3 is a schematic view of a first three-dimensional columnar structure or a second three-dimensional columnar structure of the present invention;
FIG. 4 is a topography of an epitaxial functional layer of the present invention;
fig. 5 is a test chart of curvature test of an epitaxial structure of a large-sized low-stress nitride epitaxial material prepared by the preparation method of a large-sized low-stress nitride epitaxial material of the present invention.
Detailed Description
In order to describe the technical content, the constructional features, the achieved objects and effects of the present invention in detail, the following description is made in connection with the embodiments and the accompanying drawings.
Referring to fig. 1-5, the method for preparing a large-size low-stress nitride epitaxial material according to the present embodiment is used for preparing a large-size low-stress nitride epitaxial material, where the large-size low-stress nitride epitaxial material includes a C-plane sapphire substrate 1, and a first three-dimensional columnar structure 2, an aluminum nitride epitaxial structure 3, a second three-dimensional columnar structure 4 and an epitaxial functional layer sequentially epitaxially formed on the C-plane sapphire substrate 1, and the epitaxial functional layer sequentially epitaxially forms a gallium nitride channel layer 41, an aluminum gallium nitride barrier layer 42 and a gallium nitride cap layer 43 on the second three-dimensional columnar structure 4, and the aluminum nitride epitaxial structure 3 and the epitaxial functional layer are epitaxial structures of the large-size low-stress nitride epitaxial material.
It can be understood that the epitaxial structure grows on the three-dimensional columnar structure, is suitable for thinning the thickness of the epitaxial structure so as to reduce the thickness of a finished product material, greatly saves the preparation time and the preparation cost of the epitaxial structure because the thickness of the epitaxial structure is far smaller than that of a traditional epitaxial material, and further reduces the preparation process and the preparation cost because the thickness of the epitaxial structure is small without designing a stress release layer and a high-pressure-resistant regulating layer.
The preparation method of the large-size low-stress nitride epitaxial material comprises the following steps:
s1, depositing on a C-plane sapphire substrate 1 by adopting a physical vapor deposition method to generate a first three-dimensional columnar structure 2.
S2, placing the C-plane sapphire substrate 1 in an MOCVD reaction cavity, and generating an aluminum nitride epitaxial structure 3 on the first three-dimensional columnar structure 2 by utilizing an MOCVD process.
And S3, depositing on the aluminum nitride epitaxial structure 3 by adopting a physical vapor deposition method to generate a second three-dimensional columnar structure 4.
And S4, placing the C-plane sapphire substrate 1 in an MOCVD reaction cavity, and generating an epitaxial functional layer on the second three-dimensional columnar structure 4 by utilizing an MOCVD process.
The first three-dimensional columnar structure 2, the aluminum nitride epitaxial structure 3 and the second three-dimensional columnar structure 4 together constitute a three-dimensional epitaxial structure.
It will be appreciated that the large size nitride epitaxial materials on the market are mainly 6 to 8 inches in size, and correspondingly, the C-plane sapphire substrate 1 of 6 to 8 inches in size is required to be used for preparing the nitride epitaxial materials. The present embodiment is described taking a 6-inch nitride epitaxial material as an example, and the C-plane sapphire substrate 1 is 6 inches at this time, but of course, for a nitride epitaxial material having a size of 6 to 8 inches, the C-plane sapphire substrate 1 used is 6 to 8 inches. In addition, the preparation method of the large-size low-stress nitride epitaxial material provided by the embodiment is also applicable to other sizes of nitride epitaxial materials (such as nitride epitaxial materials smaller than 6 inches and nitride epitaxial materials larger than 8 inches).
Preferably, the step S1 specifically includes:
s11, placing the C-plane sapphire substrate 1 in a physical vapor deposition reaction cavity.
S12, pumping the vacuum degree of the physical vapor deposition reaction cavity to 5 x 10 -5 Pa。
And S13, introducing argon and nitrogen into the physical vapor deposition reaction chamber, wherein the flow ratio of the argon to the nitrogen is 8:1, and controlling the vacuum degree of the physical vapor deposition reaction chamber to be 1Pa.
S13, preheating the C-plane sapphire substrate 1 and the aluminum target to 200 ℃.
S14, performing direct-current sputtering on the C-plane sapphire substrate 1, wherein the sputtering power is 300W, the sputtering rate is 0.1nm/S, the sputtering time is 100.00S, so that a first three-dimensional columnar structure 2 is deposited and generated on the C-plane sapphire substrate 1, and the thickness of the obtained first three-dimensional columnar structure 2 is 10nm, and the obtained first three-dimensional columnar structure is actually an aluminum nitride three-dimensional epitaxial layer.
Preferably, the step S2 specifically includes:
s21, placing the C-plane sapphire substrate 1 in an MOCVD reaction cavity;
s22, setting the temperature of the MOCVD reaction chamber to 1100 ℃ and the air pressure to 50mbar;
s23, taking hydrogen as carrier gas, and introducing trimethylaluminum and ammonia gas into the MOCVD reaction chamber, wherein the five-three ratio of the trimethylaluminum to the ammonia gas is 500, so as to generate an aluminum nitride epitaxial structure 3 on the first three-dimensional columnar structure 2;
s24, controlling the carrier gas rate and the carrier gas time of the hydrogen to control the growth rate of the aluminum nitride epitaxial structure 3 to be 0.2nm/S and the growth time to be 50.00S, wherein the thickness of the obtained aluminum nitride epitaxial structure 3 is 10nm.
Preferably, the step S3 specifically includes:
s31, placing the C-plane sapphire substrate 1 in a physical vapor deposition reaction cavity;
s32, pumping the vacuum degree of the physical vapor deposition reaction cavity to 5 x 10 -5 Pa；
S33, introducing argon and nitrogen into the physical vapor deposition reaction chamber, wherein the flow ratio of the argon to the nitrogen is 8:1, and controlling the vacuum degree of the physical vapor deposition reaction chamber to be 1Pa;
s34, preheating the C-plane sapphire substrate 1 and an aluminum target to 200 ℃;
s35, performing direct current sputtering on the C-plane sapphire substrate 1, wherein the sputtering power is 300W, the sputtering rate is 0.1nm/S, the sputtering time is 100.00S, so as to deposit and generate a second three-dimensional columnar structure 4 on the aluminum nitride epitaxial structure 3, the thickness of the obtained second three-dimensional columnar structure 4 is 10nm, the second three-dimensional columnar structure is actually an aluminum nitride three-dimensional epitaxial layer, and fig. 3 shows the three-dimensional columnar morphology of the aluminum nitride three-dimensional epitaxial layer.
Preferably, the step S4 specifically includes:
s411, placing the C-plane sapphire substrate 1 in an MOCVD reaction cavity;
s412, setting the temperature of the MOCVD reaction chamber to 1080 ℃ and the air pressure to 100mbar;
s413, taking hydrogen as carrier gas, and introducing trimethyl gallium and ammonia gas into the MOCVD reaction chamber, wherein the five-three ratio of the trimethyl gallium to the ammonia gas is 1500, so as to generate a gallium nitride channel layer 41 on the second three-dimensional columnar structure 4, and the thickness of the gallium nitride channel layer 41 is 150nm;
s414, controlling the carrier gas rate and carrier gas time of the hydrogen gas to control the growth rate of the gallium nitride channel layer 41 to be 0.6nm/S and the growth time to be 375.00S;
s415, taking hydrogen as carrier gas, and introducing trimethyl gallium, trimethyl aluminum and ammonia gas into the MOCVD reaction chamber, wherein the five-three ratio of the trimethyl gallium, the trimethyl aluminum and the ammonia gas is 800, so as to generate an aluminum gallium nitrogen barrier layer 42 on the gallium nitride channel layer 41;
s416, controlling the carrier gas rate and carrier gas time of the hydrogen to control the growth rate of the AlGaN barrier layer 42 to be 0.4nm/S and the growth time to be 62.50S, wherein the thickness of the AlGaN barrier layer 42 is 25nm;
s417, using hydrogen as carrier gas, and introducing trimethyl gallium and ammonia gas into the MOCVD reaction chamber to generate a gallium nitride cap layer 43 on the aluminum gallium nitride barrier layer 42;
s418, controlling the carrier gas rate and carrier gas time of the hydrogen gas to control the growth rate of the gallium nitride cap layer 43 to be 0.5nm/S and the growth time to be 4.00S, wherein the thickness of the obtained gallium nitride cap layer 43 is 2nm.
Specifically, the aluminum component of the aluminum gallium nitride barrier layer 42 is 25%.
Through the steps, the epitaxial functional layer with the total thickness of 177nm is obtained, and the thickness of the second three-dimensional columnar structure 4, the aluminum nitride epitaxial structure 3 and the first three-dimensional columnar structure 2 is combined to obtain the epitaxial material with the total thickness of 207nm, wherein the epitaxial material is about one twentieth of the thickness of the conventional epitaxial material, the appearance of the epitaxial surface is shown as fig. 4, and as can be seen from fig. 4, the large-size low-stress nitride epitaxial material prepared by the embodiment basically realizes a relatively flat epitaxial surface.
Fig. 5 shows the test data of the epitaxial curvature test of the large-size low-stress nitride epitaxial material, and it can be seen from fig. 5 that TTV, WARP, etc. of the grown epitaxial material are all in the number of several micrometers, which is equivalent to the number of commercial 6-inch sapphire substrates, so that the state without epitaxial stress is basically realized.
In order to adapt the embodiment to the application of the radio frequency material, the parameters of step S4 of the embodiment may be adjusted so that the actually generated epitaxial functional layer is a radio frequency channel layer, where step S4 specifically includes:
s421, placing the C-plane sapphire substrate 1 in an MOCVD reaction cavity;
s422, setting the temperature of the MOCVD reaction chamber to 1110 ℃ and the air pressure to 70mbar;
s423, using hydrogen as carrier gas, and introducing trimethyl gallium and ammonia gas into the MOCVD reaction chamber, wherein the five-three ratio of the trimethyl gallium to the ammonia gas is 1500, so as to generate a gallium nitride channel layer 41 on the second three-dimensional columnar structure 4;
s424, controlling the carrier gas rate and carrier gas time of the hydrogen gas to control the growth rate of the gallium nitride channel layer 41 to be 0.6nm/S and the growth time to be 333.33S, wherein the thickness of the gallium nitride channel layer 41 is 200nm;
s425, taking hydrogen as carrier gas, and introducing trimethyl gallium, trimethyl aluminum and ammonia gas into the MOCVD reaction chamber, wherein the five-three ratio of the trimethyl gallium, the trimethyl aluminum and the ammonia gas is 600, so as to generate an aluminum gallium nitrogen barrier layer 42 on the gallium nitride channel layer 41;
s426, controlling the carrier gas rate and carrier gas time of the hydrogen so as to control the growth rate of the AlGaN barrier layer 42 to be 0.3nm/S and the growth time to be 66.67S, wherein the thickness of the AlGaN barrier layer 42 is 20nm;
s427, using hydrogen as carrier gas, and introducing trimethyl gallium and ammonia gas into the MOCVD reaction chamber to generate a gallium nitride cap layer 43 on the aluminum gallium nitride barrier layer 42;
s428, controlling the carrier gas rate and carrier gas time of the hydrogen gas to control the growth rate of the gallium nitride cap layer 43 to be 0.5nm/S and the growth time to be 3.00S, wherein the thickness of the obtained gallium nitride cap layer 43 is 1.5nm.
Specifically, the aluminum component of the aluminum gallium nitride barrier layer 42 is 30%.
Preferably, the C-plane sapphire substrate 1 has a size of 6 to 8 inches.
It can be understood that the invention combines the ideas of three-dimensional structure layer and epitaxial functional layer to solve the problems of large epitaxial internal stress and overlarge curvature. According to the invention, the epitaxial functional layer is directly prepared on the three-dimensional structure, and a stress regulation layer and a doped pressure-resistant layer of the traditional epitaxial structure are not needed, so that the thickness of the whole epitaxial material is thinner, the thickness of the common epitaxial material is less than 500nm, and the thin-layer structure is equivalent to realizing higher device performance. Because the thin epitaxial material structure is far smaller than the traditional structure (the traditional structure refers to an epitaxial material structure larger than 3 microns), the epitaxial stress of the whole material is smaller, so that the curvature is smaller, and the epitaxial chip preparation with higher yield is realized.
Corresponding to other types of large sizes, under the condition that the thickness of the aluminum nitride three-dimensional epitaxial layer is ensured to be 5-15nm and the thickness of the aluminum nitride epitaxial structure 3 is ensured to be 2-5nm, or the total thickness of the periodic structure design of the aluminum nitride three-dimensional epitaxial layer, the aluminum nitride epitaxial structure 3 and the aluminum nitride three-dimensional epitaxial layer is not more than 100nm, and under the condition that the total thickness of the epitaxial functional layer is not more than 500nm, the epitaxial material with larger size and thinner total thickness can be achieved.
With reference to fig. 1-5, the first three-dimensional columnar structure 2, the aluminum nitride epitaxial structure 3, the second three-dimensional columnar structure 4 and the epitaxial functional layer are sequentially generated on the C-plane sapphire substrate 1, and the thicknesses of the aluminum nitride epitaxial structure 3 and the epitaxial functional layer are reduced by adding the first three-dimensional columnar structure 2 and the second three-dimensional columnar structure 4, so that the thickness of a finished product material is reduced, the thickness of the epitaxial structure is far smaller than that of a traditional epitaxial material, the preparation time and the preparation cost of the epitaxial structure are greatly saved, and a stress release layer and a high-voltage-resistant regulating layer are not required to be designed due to the small thickness of the epitaxial structure, so that the preparation procedure and the preparation cost are further reduced.
The foregoing description of the preferred embodiments of the present invention is not intended to limit the scope of the claims, which follow, as defined in the claims.
Claims (10)
1. The preparation method of the large-size low-stress nitride epitaxial material is characterized by comprising the following steps of:
depositing on a C-plane sapphire substrate by adopting a physical vapor deposition method to generate a first three-dimensional columnar structure;
placing the C-plane sapphire substrate in an MOCVD reaction cavity, and generating an aluminum nitride epitaxial structure on the first three-dimensional columnar structure by utilizing an MOCVD process;
depositing on the aluminum nitride epitaxial structure by adopting a physical vapor deposition method to generate a second three-dimensional columnar structure;
and placing the C-plane sapphire substrate in an MOCVD reaction cavity, and generating an epitaxial functional layer on the second three-dimensional columnar structure by utilizing an MOCVD process.
2. The method for preparing a large-size low-stress nitride epitaxial material according to claim 1, wherein the physical vapor deposition method is used for depositing and generating a first three-dimensional columnar structure on a C-plane sapphire substrate, and specifically comprises the following steps:
placing the C-plane sapphire substrate in a physical vapor deposition reaction cavity;
pumping the vacuum degree of the physical vapor deposition reaction cavity to 5-10 -5 Pa；
Argon and nitrogen are introduced into the physical vapor deposition reaction chamber, wherein the flow ratio of the argon to the nitrogen is 8:1, and the vacuum degree of the physical vapor deposition reaction chamber is controlled to be 1Pa;
preheating a C-plane sapphire substrate and an aluminum target to 200 ℃;
and performing direct current sputtering on the C-plane sapphire substrate, wherein the sputtering power is 300W, the sputtering rate is 0.1nm/s, and the sputtering time is 100.00s, so as to deposit and generate a first three-dimensional columnar structure on the C-plane sapphire substrate.
3. The method for preparing a large-size low-stress nitride epitaxial material according to claim 1, wherein the step of placing the C-plane sapphire substrate in an MOCVD reaction chamber and generating an aluminum nitride epitaxial structure on the first three-dimensional columnar structure by using an MOCVD process specifically comprises:
placing the C-plane sapphire substrate in an MOCVD reaction cavity;
setting the temperature of the MOCVD reaction chamber to 1100 ℃ and the air pressure to 50mbar;
introducing trimethylaluminum and ammonia gas into the MOCVD reaction chamber by taking hydrogen as carrier gas, wherein the five-three ratio of the trimethylaluminum to the ammonia gas is 500, so as to generate an aluminum nitride epitaxial structure on the first three-dimensional columnar structure;
the carrier gas rate and carrier gas time of the hydrogen gas were controlled to control the growth rate of the aluminum nitride epitaxial structure to 0.2nm/s and the growth time to 50.00s.
4. The method for preparing a large-size low-stress nitride epitaxial material according to claim 1, wherein the physical vapor deposition method is used for depositing a second three-dimensional columnar structure on the aluminum nitride epitaxial structure, and the method specifically comprises the following steps:
placing the C-plane sapphire substrate in a physical vapor deposition reaction cavity;
pumping the vacuum degree of the physical vapor deposition reaction cavity to 5-10 -5 Pa；
Argon and nitrogen are introduced into the physical vapor deposition reaction chamber, wherein the flow ratio of the argon to the nitrogen is 8:1, and the vacuum degree of the physical vapor deposition reaction chamber is controlled to be 1Pa;
preheating a C-plane sapphire substrate and an aluminum target to 200 ℃;
and performing direct current sputtering on the C-plane sapphire substrate, wherein the sputtering power is 300W, the sputtering rate is 0.1nm/s, and the sputtering time is 100.00s, so as to deposit and generate a second three-dimensional columnar structure on the aluminum nitride epitaxial structure.
5. The method for preparing a large-size low-stress nitride epitaxial material according to claim 1, wherein the epitaxial functional layer comprises a gallium nitride channel layer, an aluminum gallium nitride barrier layer and a gallium nitride cap layer which are sequentially epitaxially grown on the second three-dimensional columnar structure, the C-plane sapphire substrate is placed in an MOCVD reaction chamber, and the epitaxial functional layer is grown on the second three-dimensional columnar structure by using an MOCVD process, and the method specifically comprises:
placing the C-plane sapphire substrate in an MOCVD reaction cavity;
setting the temperature of the MOCVD reaction chamber to 1080 ℃ and the air pressure to 100mbar;
introducing trimethyl gallium and ammonia gas into the MOCVD reaction cavity by taking hydrogen as carrier gas, wherein the five-three ratio of the trimethyl gallium to the ammonia gas is 1500, so as to generate a gallium nitride channel layer on the second three-dimensional columnar structure;
controlling the carrier gas rate and carrier gas time of the hydrogen to control the growth rate of the gallium nitride channel layer to be 0.6nm/s and the growth time to be 375.00s;
hydrogen is used as carrier gas, and trimethyl gallium, trimethyl aluminum and ammonia gas are introduced into the MOCVD reaction chamber, wherein the five-three ratio of the trimethyl gallium to the trimethyl aluminum to the ammonia gas is 800, so that an aluminum gallium nitrogen barrier layer is generated on the gallium nitride channel layer;
controlling the carrier gas rate and carrier gas time of the hydrogen to control the growth rate of the AlGaN barrier layer to be 0.4nm/s and the growth time to be 62.50s;
introducing trimethyl gallium and ammonia gas into the MOCVD reaction cavity by taking hydrogen as carrier gas to generate a gallium nitride cap layer on the aluminum gallium nitrogen barrier layer;
the carrier gas rate and carrier gas time of the hydrogen gas were controlled so as to control the growth rate of the gallium nitride cap layer to 0.5nm/s and the growth time to 4.00s.
6. The method of claim 5, wherein the aluminum component of the aluminum gallium nitride barrier layer is 25%.
7. The method for preparing a large-size low-stress nitride epitaxial material according to claim 1, wherein the epitaxial functional layer comprises a gallium nitride channel layer, an aluminum gallium nitride barrier layer and a gallium nitride cap layer which are sequentially arranged, the C-plane sapphire substrate is placed in an MOCVD reaction chamber, and the epitaxial functional layer is generated on the second three-dimensional columnar structure by using an MOCVD process, and the method specifically comprises:
placing the C-plane sapphire substrate in an MOCVD reaction cavity;
setting the temperature of the MOCVD reaction chamber to 1110 ℃ and the air pressure to 70mbar;
introducing trimethyl gallium and ammonia gas into the MOCVD reaction cavity by taking hydrogen as carrier gas, wherein the five-three ratio of the trimethyl gallium to the ammonia gas is 1500, so as to generate a gallium nitride channel layer on the second three-dimensional columnar structure;
controlling the carrier gas rate and carrier gas time of the hydrogen gas to control the growth rate of the gallium nitride channel layer to be 0.6nm/s and the growth time to be 333.33s;
hydrogen is used as carrier gas, and trimethyl gallium, trimethyl aluminum and ammonia gas are introduced into the MOCVD reaction chamber, wherein the five-three ratio of the trimethyl gallium, the trimethyl aluminum and the ammonia gas is 600, so that an aluminum gallium nitrogen barrier layer is generated on the gallium nitride channel layer;
controlling the carrier gas rate and carrier gas time of the hydrogen to control the growth rate of the AlGaN barrier layer to be 0.3nm/s and the growth time to be 66.67s;
introducing trimethyl gallium and ammonia gas into the MOCVD reaction cavity by taking hydrogen as carrier gas to generate a gallium nitride cap layer on the aluminum gallium nitrogen barrier layer;
the carrier gas rate and carrier gas time of the hydrogen gas were controlled so as to control the growth rate of the gallium nitride cap layer to 0.5nm/s and the growth time to 3.00s.
8. The method of fabricating a large-sized low-stress nitride epitaxial material according to claim 7, wherein the aluminum component of the aluminum gallium nitride barrier layer is 30%.
9. The method of fabricating a large-sized low-stress nitride epitaxial material according to claim 1, wherein the C-plane sapphire substrate has a size of 6 to 8 inches.
10. The large-size low-stress nitride epitaxial material is characterized by being prepared by a preparation method of the large-size low-stress nitride epitaxial material according to any one of claims 1-9, and comprises a C-plane sapphire substrate, a first three-dimensional columnar structure, an aluminum nitride epitaxial structure, a second three-dimensional columnar structure and an epitaxial functional layer, wherein the first three-dimensional columnar structure, the aluminum nitride epitaxial structure, the second three-dimensional columnar structure and the epitaxial functional layer are sequentially epitaxially generated on the C-plane sapphire substrate, and the gallium nitride channel layer, the aluminum gallium nitride barrier layer and the gallium nitride cap layer are sequentially epitaxially generated on the second three-dimensional columnar structure.
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