CN116288681A - Monocrystalline diamond AlN template for GaN power electronic device and preparation method thereof - Google Patents
Monocrystalline diamond AlN template for GaN power electronic device and preparation method thereof Download PDFInfo
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 84
- 239000010432 diamond Substances 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000013078 crystal Substances 0.000 claims abstract description 46
- 238000000407 epitaxy Methods 0.000 claims abstract description 42
- 229910052582 BN Inorganic materials 0.000 claims abstract description 33
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 33
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052741 iridium Inorganic materials 0.000 claims abstract description 21
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 17
- 239000010980 sapphire Substances 0.000 claims abstract description 17
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims description 62
- 238000000034 method Methods 0.000 claims description 40
- 238000000151 deposition Methods 0.000 claims description 36
- 230000008021 deposition Effects 0.000 claims description 36
- 238000004544 sputter deposition Methods 0.000 claims description 23
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 14
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 11
- 238000005566 electron beam evaporation Methods 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 7
- 238000012546 transfer Methods 0.000 abstract description 5
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 28
- 229910002601 GaN Inorganic materials 0.000 description 27
- 230000006872 improvement Effects 0.000 description 13
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 239000010408 film Substances 0.000 description 8
- 238000001878 scanning electron micrograph Methods 0.000 description 8
- 235000012431 wafers Nutrition 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000005259 measurement Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 3
- 238000005240 physical vapour deposition Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 238000000089 atomic force micrograph Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 230000001052 transient effect Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000004439 roughness measurement Methods 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
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- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
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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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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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
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Abstract
The invention provides a monocrystalline diamond AlN template for a GaN power electronic device and a preparation method thereof, comprising the following steps: s1, growing single crystal epitaxy of iridium on an A-plane sapphire; s2, growing a single crystal epitaxy of first cubic boron nitride on the single crystal epitaxy of iridium; s3, growing a diamond film on the monocrystal epitaxy of the cubic crystal boron nitride; s4, growing a single crystal epitaxy of second cubic boron nitride on the diamond film; s5, growing hexagonal boron nitride monocrystal epitaxy on the monocrystal epitaxy of the second cubic crystalline boron nitride; and S6, growing a hexagonal crystalline aluminum nitride layer on the hexagonal boron nitride monocrystal epitaxy. The single crystal diamond AlN template allows a high quality GaN epitaxial layer to be grown directly on top of the diamond AlN template without any additional bonding or transfer steps, reducing costs.
Description
Technical Field
The invention relates to a monocrystalline diamond AlN template for a GaN power electronic device and a preparation method thereof, belonging to the technical field of preparation of GaN power electronic devices.
Background
Gallium nitride is an inorganic substance, has a chemical formula of GaN, is a compound of nitrogen and gallium, is a direct bandgap (direct bond gap) semiconductor, and has been commonly used in light emitting diodes since 1990. The compound has a structure similar to wurtzite and high hardness. Gallium nitride has a wide energy gap of 3.4 ev, and can be used in high-power and high-speed photoelectric elements, for example, gallium nitride can be used in a laser Diode for ultraviolet light, and ultraviolet (405 nm) laser can be generated without using a nonlinear semiconductor pump solid-state laser (Diode-pumped solid-state laser). Gallium nitride (GaN) power electronics have attracted considerable attention in recent years due to their high power and high speed capabilities, but the large amount of heat generated during operation has adversely affected the performance of the device.
Diamond has its particular thermal conductivity and is considered a solution to the release of heat from gallium nitride power electronics. However, while the prior art has developed bonding methods that bond gallium nitride device layers to diamond layers, existing bonding techniques generally provide greater thermal boundary resistance than bulk growth, requiring additional bonding or transfer steps, increasing costs.
Disclosure of Invention
The invention provides a monocrystalline diamond AlN template for a GaN power electronic device and a preparation method thereof, which can effectively solve the problems
The invention is realized in the following way:
a preparation method of a monocrystal diamond AlN template comprises the following steps:
s1, growing single crystal epitaxy of iridium on an A-plane sapphire;
s2, growing a single crystal epitaxy of first cubic boron nitride on the single crystal epitaxy of iridium;
s3, growing a diamond film on the monocrystal epitaxy of the cubic crystal boron nitride;
s4, growing a single crystal epitaxy of second cubic boron nitride on the diamond film;
s5, growing hexagonal boron nitride monocrystal epitaxy on the monocrystal epitaxy of the second cubic crystalline boron nitride;
and S6, growing a hexagonal crystalline aluminum nitride layer on the hexagonal boron nitride monocrystal epitaxy.
As a further improvement, the growth in step S1 employs an electron beam evaporation method or a sputtering method; the deposition conditions of the electron beam evaporation method are as follows: the temperature of the substrate is 800-1000 ℃, and the vacuum degree is less than 10-9Torr; the sputtering method adopts a DC bias sputtering gun to sputter iridium, and the deposition conditions are as follows: vacuum degree <5mTorr, substrate temperature 800-1000 deg.C, and negative substrate bias voltage 50-300V.
As a further improvement, the growth in step S2 employs a sputtering method, and the deposition conditions are: the temperature of the substrate is fixed at 600-800 ℃, and a negative substrate bias voltage of 50-300V is applied.
As a further improvement, the growth in the step S3 adopts a microwave plasma enhanced chemical vapor deposition method, specifically: and (3) carrying out deposition on the substrate preheated to 700 ℃ in a mixed hydrogen methane atmosphere, and carrying out deposition at the deposition temperature of 800-1100 ℃ without applying substrate bias voltage.
As a further improvement, the growth in the step S4 adopts a sputtering method, a negative substrate bias voltage of 50-300V is applied, and the substrate temperature is fixed at 600-800 ℃.
As a further improvement, the growth in step S5 is performed by sputtering, the substrate temperature is fixed at 1000 ℃, and the substrate bias is not applied.
As a further improvement, the growth in step S6 employs a microwave plasma enhanced chemical vapor deposition method.
A single crystal diamond AlN template prepared by the method described above.
An application of the monocrystalline diamond AlN template in a GaN power electronic device.
The beneficial effects of the invention are as follows:
in the preparation of the single crystal diamond AlN template of the invention, h-BN and c-BN layers are introduced between AlN and diamond, which facilitates smooth transition of crystal structure, thereby forming an ordered and continuous AlN epitaxial layer. The entire stack shows excellent adhesion and compatibility between the different layers without breaking PVD vacuum, which allows high quality GaN epitaxial layers to be grown directly on top of the diamond AlN template without any additional bonding or transfer steps, reducing costs.
The preparation of the monocrystalline diamond AlN template adopts the diamond layer which has the highest heat conductivity coefficient, so that the heat generated by gallium nitride power electronic equipment is effectively released, and the performance of the device is improved.
In the preparation of the monocrystalline diamond AlN template, cubic boron nitride (c-BN) is introduced into the upper surface and the lower surface of the diamond as a buffer layer, the lattice constant of the c-BN layer is closer to that of the diamond, the lattice mismatch between a substrate and the diamond layer and between GaN and the diamond is reduced, the monocrystalline diamond AlN template can be used for producing large-area monocrystalline diamond with better quality and performance than that of the conventional method, and high-quality gallium nitride epitaxy is developed on the large-area monocrystalline diamond, so that the power of a gallium nitride power electronic device is improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic view of single crystal diamond AlN template growth provided in an embodiment of the present invention.
FIG. 2 is an X-ray diffraction chart of the sample obtained in step S3 in example 1 of the present invention.
FIG. 3 is an atomic force microscope image of the sample obtained in step S3 of example 1 of the present invention.
FIG. 4 is an SEM image of the h-BN/c-BN/diamond/c-BN/Ir/A planar sapphire surface of the sample obtained in step S5 of example 1 of the present invention.
FIG. 5 is one of XPS data graphs of the samples obtained in example 1 of the present invention.
FIG. 6 is a second XPS data plot of the sample obtained in example 1 of the present invention.
Fig. 7 is a photograph (a) of the sample of comparative example 1 of the present invention, SEM image (B) taken from the center of the sample, and SEM image (C) taken from the edge of the sample.
FIG. 8 is an X-ray diffraction (XRD) measurement pattern of a sample GaN/AlN/diamond heterostructure according to example 2 of the invention.
Fig. 9 is a graph of transient area thermal reflectance (TDTR) measurements of a sample of example 1 of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention. Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
As shown in fig. 1, the invention provides a preparation method of a monocrystalline diamond AlN template, comprising the following steps:
s1, growing single crystal epitaxy of iridium (Ir) on A-plane sapphire (A-plane sapphire);
s2, growing single crystal epitaxy of first cubic boron nitride (c-BN) on the single crystal epitaxy of iridium;
s3, growing a diamond film on single crystal epitaxy of cubic boron nitride (c-BN);
s4, growing single crystal epitaxy of second cubic boron nitride (c-BN) on the diamond film;
s5, growing hexagonal boron nitride (h-BN) monocrystal epitaxy on the monocrystal epitaxy of the second cubic boron nitride (c-BN);
s6, growing a hexagonal crystalline aluminum nitride layer (AlN) on the hexagonal boron nitride monocrystal (h-BN) epitaxy.
As a further improvement, the growth in step S1 employs an electron beam evaporation method or a sputtering method; the deposition conditions of the electron beam evaporation method are as follows: the temperature of the substrate is 800-1000 ℃ and the vacuum degree<10 -9 Torr; the sputtering method adopts a DC bias sputtering gun to sputter iridium, and the deposition conditions are as follows: vacuum degree<And 5mTorr, wherein the substrate temperature is 800-1000 ℃, and negative substrate bias voltage is applied for 50-300V, so that better crystal nucleus formation on the sapphire substrate is facilitated.
As a further improvement, the growth in step S2 employs a sputtering method, and since c-BN has a similar cubic crystal structure and lattice parameter, c-BN can be grown on the iridium layer by sputter deposition. The c-BN was grown using a pure iridium target and a substrate bias was applied. The application of a negative substrate bias voltage of 50-300V during deposition aids in the formation of a cubic crystal structure rather than hexagonal boron nitride. The substrate temperature was fixed at 600-800 c during deposition.
As a further improvement, the growth in step S3 employs a microwave plasma enhanced chemical vapor deposition (MPCVD). The microwave plasma enhanced chemical vapor deposition method comprises the following steps: and the deposition is carried out on the substrate preheated to 700 ℃ in the mixed hydrogen methane atmosphere, and then the deposition is carried out at the deposition temperature of 800-1100 ℃, so that the large-area monocrystalline diamond wafer with better quality and performance than the traditional method can be produced without applying a substrate direct current bias voltage, and the production cost and complexity are reduced.
Wherein the lattice constant difference between iridium and diamond is 7.03%, and wherein the lattice constant of iridium isThe lattice constant of diamond is +.>Since c-BN has->The lattice constant of the c-BN layer is closer to that of diamond, so that the addition of the c-BN insertion layer as a buffer layer between the iridium and diamond layers can gradually match the lattice constant, reducing the lattice mismatch between the substrate and the diamond layers. Furthermore, a key problem with using iridium as a substrate in conventional processes is that it has a higher Coefficient of Thermal Expansion (CTE) than diamond, which can lead to structural defects and degrade the quality of the diamond film over time. In this example, the Coefficient of Thermal Expansion (CTE) of c-BN is more similar to that of iridium than diamond, ensuring that the diamond film retains its integrity and quality over time. This method provides a practical and efficient way to produce large area single crystal diamond wafers of better quality and performance than conventional methods.
As a further improvement, the growth in step S4 is performed by sputtering, and c-BN can be grown on the diamond layer by sputter deposition due to its similar cubic crystal structure and lattice parameter. c-BN was grown on the diamond layer using a pure boron target. A negative substrate bias of 50-300V is used during deposition to form a cubic structure instead of hexagonal boron nitride. The substrate temperature was fixed at 600-800 ℃ during deposition.
As a further improvement, the growth in step S5 is performed by sputtering, the substrate temperature is fixed at 1000 ℃, and the substrate bias is not applied.
As a further improvement, the growth in step S6 employs a microwave plasma enhanced chemical vapor deposition method. The microwave plasma enhanced chemical vapor deposition method comprises the following steps: and (3) carrying out deposition on the substrate preheated to 700 ℃ in a mixed hydrogen methane atmosphere, and then carrying out deposition at the deposition temperature of 800-1100 ℃ without applying a substrate direct current bias voltage.
The invention also provides the monocrystalline diamond AlN template prepared by the method.
The invention also provides application of the monocrystalline diamond AlN template in a GaN power electronic device.
Example 1
The invention provides a preparation method of a monocrystalline diamond AlN template, which comprises the following steps:
s1, growing single crystal epitaxy of iridium on an A-plane sapphire; adopting an electron beam evaporation method; the deposition conditions are as follows: the temperature of the substrate is 950 ℃ and the vacuum degree<10 -9 Torr。
S2, growing a single crystal epitaxy of first cubic boron nitride on the single crystal epitaxy of iridium; the sputtering method is adopted, and the deposition conditions are as follows: the substrate temperature was fixed at 800 c and a negative substrate bias voltage of 200V was applied.
S3, growing a diamond film on the monocrystal epitaxy of the cubic crystal boron nitride; the microwave plasma enhanced chemical vapor deposition method is adopted, and concretely comprises the following steps: deposition was performed on a substrate preheated to 700 ℃ in a mixed hydrogen methane atmosphere, and then at a deposition temperature of 1100 ℃ without applying a substrate bias.
S4, growing a single crystal epitaxy of second cubic boron nitride on the diamond film; a negative substrate bias voltage 150 was applied by sputtering, and the substrate temperature was fixed at 600 ℃.
S5, growing hexagonal boron nitride monocrystal epitaxy on the monocrystal epitaxy of the second cubic crystalline boron nitride; the sputtering method was used, the substrate temperature was fixed at 1000 ℃, and no substrate bias was applied.
S6, growing a hexagonal crystalline aluminum nitride layer on the hexagonal boron nitride monocrystal epitaxy, and adopting a microwave plasma enhanced chemical vapor deposition method, wherein the method specifically comprises the following steps: deposition was performed on a substrate preheated to 700 ℃ in a mixed hydrogen methane atmosphere, and then at a deposition temperature of 1100 ℃ without applying a substrate bias.
Example 2
On the basis of example 1, a GaN layer was grown on a hexagonal crystalline aluminum nitride layer, and the other operations were the same as in example 1. The GaN layer is grown by adopting a microwave plasma enhanced chemical vapor deposition method. The method comprises the following steps: deposition was performed on a substrate preheated to 700 ℃ in a mixed hydrogen methane atmosphere, and then at a deposition temperature of 1100 ℃ without applying a substrate bias.
Comparative example 1
The difference from example 1 is that there are no steps S4 and S5, and the other operations are the same as example 1.
The performance tests of the samples of examples 1-2 and comparative example 1 are shown in fig. 2 to 9.
As shown in fig. 2, fig. 2 is an X-ray diffraction (XRD) pattern of the sample obtained in step S3 of example 1 of the present invention, showing crystallization peaks of materials for producing a large-area single crystal diamond wafer, including sapphire (1120), ir (002), c-BN (200) and Ir (111). The location, strength and shape of each peak provides important information about the crystal structure and orientation of each material, which is critical to determining the optimal growth conditions for the diamond layer and ensuring good alignment of the crystal structure of the diamond layer with the underlying substrate and buffer layer. The peak of sapphire (1120) was observed at 37.5 degrees, the peak of Ir (002) was observed at 47.5 degrees, the peak of c-BN (200) was observed at 43 degrees, and the peak of iridium (111) was observed at 41.6 degrees. The presence of distinct peaks for each material indicated that the crystal structure of each layer was well aligned with the underlying layer, indicating that the c-BN/Ir/sapphire structure could be successfully grown and used as a substrate for producing large area single crystal diamond wafers. In general, XRD data supports the effectiveness of the methods presented in this invention, providing valuable information for optimizing the growth process and ensuring the quality and performance of the final diamond product.
As shown in FIG. 3, an Atomic Force Microscope (AFM) image of the sample obtained in step S3 in example 1 of the present invention is shown. The data of this figure provides important information about the surface morphology and roughness of cBN/Ir/sapphire structures used as substrates for producing large area single crystal diamond wafers. AFM data showed well-defined step flow on cBN/Ir/sapphire structure surface, which followed a 7 degree cut of the a-plane sapphire substrate. Further, the average value of the surface roughness measured by AFM was 0.815nm. These features are important parameters for producing large area single crystal diamond wafers because they affect the quality and performance of the diamond layer. A smooth and uniform substrate surface is desirable because it minimizes defects and dislocations in the diamond layer, resulting in a higher quality and more reliable end product. AFM data, including step flow and surface roughness measurements, support the effectiveness of the methods presented in this invention, providing valuable information for optimizing the growth process and ensuring the quality and performance of the final diamond product.
As shown in FIG. 4, an SEM image of the h-BN/c-BN/diamond/c-BN/Ir/A planar sapphire surface of the sample obtained in step S5 of example 1 of the present invention, which shows a smooth and uniform surface morphology with no visible cracks or flaws. This image demonstrates that the growth of the individual layers in the stack was successful and that the resulting surface was suitable for further growth of high quality AlN epitaxial layers. A smooth surface is very important for achieving good adhesion and crystal quality of subsequent layers, which is critical for the performance of the final device.
As shown in fig. 5, one of XPS data graphs of the sample obtained in example 1 of the present invention. The figure shows the proven successful deposition of boron and nitride material obtained by AlN/h-BN/c-BN stack. The presence of Al peaks in XPS spectra also indicates the deposition of an aluminum nitride layer. The fact that the entire stack is grown monolithically without breaking the PVD vacuum demonstrates the excellent adhesion and compatibility of the different layers in the stack. This is an important achievement because it allows high quality GaN epitaxial layers to be grown directly on top of the AlN/h-BN/c-BN stack without any additional bonding or transfer steps. XPS data confirm that successful deposition of the various layers is a critical step in achieving high performance GaN-based power electronics.
As shown in fig. 6, the second XRD data pattern obtained for the sample of example 1 of the present invention. Sample AlN/h-BN/c-BN/diamond/c-BN/Ir/A planar sapphire XRD data patterns confirm successful growth of AlN on diamond. A sharp and intense AlN (002) peak occurs at about 35 degrees and a clear diamond (111) peak occurs at about 42 degrees, clearly indicating epitaxial growth of an AlN layer on a diamond substrate with high crystalline quality. This is due to the introduction of h-BN and c-BN layers between AlN and diamond, which facilitates a smooth transition of the crystal structure, resulting in an ordered and continuous AlN epitaxial layer. Observations of Al, B and N peaks in XPS data further confirm successful growth of AlN on diamond/c-BN/Ir/A planar sapphire without breaking the vacuum of PVD, thus forming a monolithic structure. These results demonstrate the effectiveness of the new method proposed in the present invention, which allows the growth of high quality AlN epitaxy on diamond substrates for various applications in the power electronics field.
As shown in fig. 7, a photograph (a) of the sample of comparative example 1 of the present invention, an SEM image (B) taken from the center of the sample, and an SEM image (C) taken from the edge of the sample are shown. The photograph of the AlN template sample as in fig. 7A shows a round wafer with a smooth surface and uniform color. SEM images taken from the center of the sample (fig. 7B) showed a highly uniform and smooth surface, with no obvious pinholes or defects, indicating high quality of the AlN template layer. In contrast, SEM images taken from the edges of the samples (FIG. 7C) showed amorphous morphology, which may be due to the lack of h-BN/C-BN layer. During growth, the edges are blocked by the sample holder, preventing deposition of the h-BN/c-BN layer and resulting in a lower quality morphology.
As shown in FIG. 8, an X-ray diffraction (XRD) measurement chart was carried out on the GaN/AlN/diamond heterostructure sample of example 2 of the present invention. XRD data reveals clear and sharp peaks corresponding to the (002) plane of GaN and AlN and the (111) plane of diamond. The presence of these peaks confirms successful growth of high quality GaN and AlN epitaxial layers on the diamond substrate. Furthermore, sharp peaks in the diamond (111) plane indicate a high crystalline quality and orientation of the diamond layer. These results demonstrate the effectiveness of the methods described in the examples of the present invention to grow high quality GaN and AlN layers on diamond substrates.
As shown in fig. 9, a transient area thermal reflectance (TDTR) measurement graph of the sample of example 1 of the present invention is shown. The TDTR method is a non-destructive technique capable of accurately measuring the heat transfer properties of a thin film with high resolution. TDTR measurements showed that the thermal conductivity of the diamond layer of example 1 was 2265W/(m.k), significantly higher than the thermal conductivity of other materials used in the power electronics. This high thermal conductivity of the diamond layer of example 1 makes it an excellent material for releasing heat generated by GaN power electrons.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, and various modifications and variations may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The preparation method of the monocrystalline diamond AlN template is characterized by comprising the following steps of:
s1, growing single crystal epitaxy of iridium on an A-plane sapphire;
s2, growing a single crystal epitaxy of first cubic boron nitride on the single crystal epitaxy of iridium;
s3, growing a diamond film on the monocrystal epitaxy of the cubic crystal boron nitride;
s4, growing a single crystal epitaxy of second cubic boron nitride on the diamond film;
s5, growing hexagonal boron nitride monocrystal epitaxy on the monocrystal epitaxy of the second cubic crystalline boron nitride;
and S6, growing a hexagonal crystalline aluminum nitride layer on the hexagonal boron nitride monocrystal epitaxy.
2. The method according to claim 1, wherein the growing in step S1 employs an electron beam evaporation method or a sputtering method; the deposition conditions of the electron beam evaporation method are as follows: the temperature of the substrate is 800-1000 ℃ and the vacuum degree<10 -9 Torr; the sputtering method adopts a DC bias sputtering gun to sputter iridium, and the deposition conditions are as follows: vacuum degree<5mTorr, the substrate temperature is 800-1000 ℃, and a negative substrate bias voltage of 50-300V is applied.
3. The method according to claim 1, wherein the growing in step S2 is performed by sputtering under the following deposition conditions: the temperature of the substrate is fixed at 600-800 ℃, and a negative substrate bias voltage of 50-300V is applied.
4. The method according to claim 1, wherein the growing in step S3 is performed by a microwave plasma enhanced chemical vapor deposition method, specifically: and (3) carrying out deposition on the substrate preheated to 700 ℃ in a mixed hydrogen methane atmosphere, and carrying out deposition at the deposition temperature of 800-1100 ℃ without applying substrate bias voltage.
5. The method according to claim 1, wherein the growth in step S4 is performed by sputtering, a negative substrate bias voltage of 50-300V is applied, and the substrate temperature is fixed at 600-800 ℃.
6. The method according to claim 1, wherein the growth in step S5 is performed by sputtering, the substrate temperature is fixed at 1000 ℃, and the substrate bias is not applied.
7. The method according to claim 1, wherein the growing in step S6 is performed by microwave plasma enhanced chemical vapor deposition.
8. A single crystal diamond AlN template prepared by the method of any one of claims 1 to 7.
9. Use of the single crystal diamond AlN template of claim 8 in a GaN power electronic device.
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