CN117133639A - Method for producing a group III nitride layer and use thereof - Google Patents

Method for producing a group III nitride layer and use thereof Download PDF

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CN117133639A
CN117133639A CN202210555451.6A CN202210555451A CN117133639A CN 117133639 A CN117133639 A CN 117133639A CN 202210555451 A CN202210555451 A CN 202210555451A CN 117133639 A CN117133639 A CN 117133639A
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layer
nitride
dimensional material
nitride layer
substrate
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魏同波
高雅琦
王军喜
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Institute of Semiconductors of CAS
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Abstract

The present disclosure discloses a method for preparing a group III nitride layer and applications thereof, wherein the method for preparing a group III nitride layer comprises: growing a two-dimensional material layer on a substrate; growing a nucleation layer on the two-dimensional material layer, wherein the two-dimensional material layer and the nucleation layer form a composite substrate for growing a III-nitride layer; a group III nitride layer is epitaxially grown on the composite substrate.

Description

Method for producing a group III nitride layer and use thereof
Technical Field
The present disclosure relates to the field of semiconductor technology, and in particular, to a method for preparing a group III nitride layer and applications thereof.
Background
The third generation semiconductors represented by gallium nitride and aluminum nitride are important development directions of research at present, and have wide application prospects and research values in the photoelectric fields of optical display, optical storage and the like. Silicon-based electronics are of enormous scale and functionality, combining higher quality nitride devices with silicon-based integrated circuits is critical to the application of optoelectronics and electronic power devices.
At present, nitride-based semiconductor materials are grown on heterogeneous substrates, but because of larger lattice mismatch and thermal mismatch between the nitride materials and the substrates, dislocation, warping, cracks and the like are easy to generate on the nitride materials epitaxially grown on the substrates, and the reliability, the product qualification rate and the working efficiency of devices are seriously affected; further, if the crystal orientation at the time of nitride growth is arbitrary, it is difficult to form a high quality thin film, thereby affecting the performance of the semiconductor device.
The flexible electronic device has wide application prospect in the fields of daily life, medical treatment, military, energy sources, computers and the like due to the unique ductility, portability, high efficiency and low cost manufacturing process. The application field and the background of the nitride-based optoelectronic device can be further widened by combining the nitride material with the flexible wearable device. In order to develop the flexible nitride photoelectric device, the problem that the flexible substrate is difficult to bear the high temperature (> 800 ℃) in the preparation process of nitride is firstly needed to be overcome, and in order to solve the problem, most researchers choose to strip and transfer the nitride epitaxially grown on the substrate by using laser, and the laser stripping cost is high, and meanwhile, the nitride is damaged.
Therefore, how to grow a higher quality group III nitride layer on a substrate and to completely strip the group III nitride layer is a problem that needs to be solved.
Disclosure of Invention
In view of the above, the present disclosure provides a method for preparing a group III nitride layer and application thereof, in order to at least partially solve the above-mentioned technical problems.
In order to solve the above technical problems, as one aspect of the present disclosure, there is provided a method for preparing a group III nitride layer, including:
growing a two-dimensional material layer on a substrate;
growing a nucleation layer on the two-dimensional material layer, wherein the two-dimensional material layer and the nucleation layer form a composite substrate for growing a III-nitride layer;
and epitaxially growing a III-nitride layer on the composite substrate.
In one embodiment, the above preparation method further includes:
after growing a III-nitride layer on the composite substrate, etching the surface of the substrate by adopting a wet etching method, and stripping and transferring the composite substrate and the III-nitride layer by adopting an adhesive tape.
In one embodiment, a substrate comprises: a silicon substrate.
In one embodiment, the two-dimensional material comprises any one of the following:
graphene, tungsten disulfide, molybdenum disulfide, tungsten diselenide, tungsten ditelluride, molybdenum ditelluride;
the thickness of the two-dimensional material includes: single layer or multiple layers, wherein the multiple layers are 2-10 layers.
In one embodiment, the nucleation layer is an aluminum nitride layer;
the aluminum nitride nucleation layer is obtained through the following steps:
adopting nitrogen or ammonia gas to treat the surface of the two-dimensional material layer, and then introducing ammonia gas and trimethylaluminum to grow an aluminum nitride nucleation layer on the surface of the treated two-dimensional material layer;
the thickness of the aluminum nitride nucleation layer comprises: 20-40nm.
In one embodiment, the epitaxial growth includes molecular beam epitaxy, metal organic chemical vapor deposition, hydride vapor phase epitaxy.
In one embodiment, the group III nitride layer grown on the composite substrate includes at least one of:
gallium nitride, aluminum nitride, indium nitride, in x Ga 1-x N、In x Al 1-x N、Al x Ga 1-x N，0<x<1；
The thickness of the group III nitride layer is 2-5 μm.
In one embodiment, the tape comprises: heat release tape or conductive copper tape.
In one embodiment, the composite substrate and the group III nitride layer are peeled and transferred using an adhesive tape, comprising:
depositing a metal electrode on the surface of the III-nitride layer, and then stripping and transferring the III-nitride layer with the metal electrode and the composite substrate by adopting a conductive copper tape to obtain a conductive copper tape, a III-nitride layer with the metal electrode, a nucleation layer and a two-dimensional material layer which are sequentially stacked from top to bottom;
taking the conductive copper tape as a lower electrode of an electronic device, and placing metal indium on the surface of the two-dimensional material layer as an upper electrode of the electronic device; or (b)
And transferring the stripped composite substrate and the III-nitride layer onto a target substrate by adopting a heat release adhesive tape to obtain the electronic device.
As another aspect of the present disclosure, there is provided an electronic device, wherein the electronic device includes a group III nitride layer prepared using the method in the above-described embodiments.
As can be seen from the above technical solutions, the method and application for preparing a group III nitride layer of the present disclosure have at least one of the following beneficial effects:
(1) In the embodiment of the disclosure, the two-dimensional material is grown on the substrate, the two-dimensional material is combined with the substrate, the III-nitride is epitaxially grown on the two-dimensional material in a van der Waals force combination mode, so that the lattice mismatch between the III-nitride and the substrate is weakened, the interface stress is released, and the atom migration and the stripping and transfer of the film can be promoted by utilizing the two-dimensional material.
(2) In the embodiment of the disclosure, the nucleation layer is grown on the surface of the two-dimensional material, so that the arbitrary orientation of the III-nitride crystal can be reduced, and the crystal quality of the III-nitride layer is improved.
Drawings
FIG. 1 is a flow chart of a method for preparing a group III-nitride layer in an embodiment of the present disclosure;
FIG. 2a is a schematic diagram of a structure for growing a two-dimensional material layer on a substrate in an embodiment of the disclosure;
FIG. 2b is a schematic diagram of a structure for growing a nucleation layer on a two-dimensional material layer in an embodiment of the present disclosure;
FIG. 2c is a schematic diagram of the structure of epitaxially growing a group III-nitride layer on a composite substrate in an embodiment of the present disclosure;
FIG. 3a is a schematic diagram of a structure for stripping group III-nitride using wet chemical etching in an embodiment of the present disclosure;
FIG. 3b is a schematic diagram of a structure for transferring a group III nitride layer onto a flexible substrate using a heat release tape in an embodiment of the present disclosure;
FIG. 3c is a schematic diagram of a structure after stripping and transferring a group III nitride layer using a conductive copper tape in an embodiment of the present disclosure;
fig. 4 is an atomic force microscope image of a final gallium nitride epitaxial layer in an embodiment of the disclosure.
[ reference numerals description ]
(1): substrate and method for manufacturing the same
(2): natural oxide layer
(3): two-dimensional material layer
(4): nucleation layer
(5): group III nitride layer
(6): adhesive tape
(7): flexible substrate
(8): metal electrode
(9): indium metal
Detailed Description
For the purposes of promoting an understanding of the principles and advantages of the disclosure, reference will now be made to the embodiments illustrated in the drawings and specific language will be used to describe the same.
The quality of the group III nitride layer has a large impact on the performance of the optoelectronic device it is composed of. In the prior art, the growing nitride-based semiconductor material is based on an epitaxial technology grown on a heterogeneous substrate, the heterogeneous substrate mainly comprises sapphire, silicon nitride, silicon and the like, and the substrate has the advantages of large size, good heat dissipation, low price, capability of realizing photoelectric integration and the like, and has more mature development and application in the field of microelectronics, so that the preparation of III-group nitride on the heterogeneous substrate also becomes a research hot spot in recent years. However, there are also problems of larger thermal mismatch and lattice mismatch between the hetero-substrate and the nitride, and it is more difficult to grow a higher quality group III nitride layer, thereby affecting its application in the electronics field, especially in the flexible electronics field.
Fig. 1 is a flow chart of a method for preparing a group III nitride layer in an embodiment of the present disclosure.
As shown in fig. 1, the method for preparing a group III nitride layer includes steps S101 to S103.
Step S101: a layer of two-dimensional material is grown on a substrate.
Step S102: and growing a nucleation layer on the two-dimensional material layer, and forming a composite substrate for growing the III-nitride layer by the two-dimensional material layer and the nucleation layer.
Step S103: a group III nitride layer is epitaxially grown on the composite substrate.
According to the embodiment of the disclosure, the two-dimensional material is grown on the silicon substrate, the two-dimensional material is combined with the silicon substrate, so that the III-nitride is epitaxially grown on the two-dimensional material in a van der Waals force combination mode, lattice mismatch between the III-nitride and the substrate is weakened, interface stress is released, and atomic migration and stripping and transferring of a film can be promoted by utilizing the two-dimensional material; then, a nucleation layer is grown on the surface of the two-dimensional material, the two-dimensional material and the nucleation layer are used as a composite substrate, and the crystal orientation randomness of the nitride can be reduced by growing the III-nitride on the composite substrate, so that the crystal quality of the III-nitride film is improved.
According to an embodiment of the present disclosure, in step S101, a substrate includes: a silicon substrate such as Si (100), si (111), or other crystal plane index silicon substrate.
Fig. 2a is a schematic diagram of a structure for growing a two-dimensional material layer on a substrate in an embodiment of the disclosure.
According to an embodiment of the disclosure, as shown in fig. 2a, a two-dimensional material layer (3) is grown on a substrate (1) and a natural oxide layer (2) thereof by Chemical Vapor Deposition (CVD), wherein the substrate includes a layer of natural oxide layer (2), and in the case of a silicon substrate, the natural oxide layer is silicon dioxide.
Through the embodiment of the disclosure, the interaction between the nitride and the substrate can be reduced by utilizing the two-dimensional material layer, the lattice mismatch between the III-nitride and the substrate is weakened, the atomic diffusion is assisted, and the stripping and the transfer of the film can be promoted;
according to an embodiment of the present disclosure, in step S101, the two-dimensional material includes any one of the following: graphene, tungsten disulfide, molybdenum disulfide, tungsten diselenide, tungsten ditelluride, molybdenum ditelluride.
According to an embodiment of the present disclosure, the thickness of the two-dimensional material includes: single layer or multiple layers, wherein the multiple layers are 2-10 layers.
According to embodiments of the present disclosure, when the two-dimensional material is a single layer, the crystal quality of the grown nitride material is higher; when the two-dimensional material is in a plurality of layers, the thickness of the two-dimensional material layer is too thick, so that the induction force of the substrate to the nitride layer is reduced, the growth quality of the nitride material is slightly poorer than that of the nitride material when the two-dimensional material layer is in a single layer, but the bonding force with the substrate can be better reduced when the two-dimensional material layer is in a plurality of layers, and the stripping difficulty is reduced.
Fig. 2b is a schematic diagram of a structure for growing a nucleation layer on a two-dimensional material layer in an embodiment of the present disclosure.
According to an embodiment of the present disclosure, as shown in fig. 2b, since the surface chemical reactivity of the two-dimensional material is low, there is a problem in that it is difficult to nucleate when growing nitride directly on the surface thereof, and it is difficult to form high quality group III nitride, a nucleation layer (4) is prepared on the two-dimensional material layer (3) using Metal Organic Chemical Vapor Deposition (MOCVD) in step S102.
According to an embodiment of the present disclosure, the nucleation layer thickness includes: the crystal quality of the group III nitride layer is affected by both the excessively thin and thick nucleation layers of 20-40nm.
In embodiments of the present disclosure, the nucleation layer is an AlN nucleation layer for reducing the randomness of crystal orientations and improving the crystal quality of the nitride thin film.
According to an embodiment of the present disclosure, an AlN nucleation layer is obtained by: and (3) treating the surface of the two-dimensional material layer by adopting nitrogen or ammonia, and then introducing ammonia and trimethylaluminum on the surface of the treated two-dimensional material layer to grow an aluminum nitride nucleation layer.
According to an embodiment of the present disclosure, the condition parameters for treating the surface of the two-dimensional material layer with nitrogen or ammonia include: the power of the treatment is 50-100W, the nitrogen flow is 100-300sccm, or ammonia is introduced into the MOCVD epitaxial growth at 1010 ℃ for pretreatment for 2-4 minutes, and the two-dimensional material layer is treated by introducing nitrogen or ammonia, so that a suspension bond is formed on the surface of the two-dimensional material layer, and the suspension bond can be combined with Al atoms in aluminum nitride for nucleation, thereby facilitating the formation of an AlN nucleation layer.
According to embodiments of the present disclosure, an AlN nucleation layer is grown at 1200-1400 ℃.
Fig. 2c is a schematic diagram of a structure for epitaxially growing a group III nitride layer on a composite substrate in an embodiment of the present disclosure.
In accordance with an embodiment of the present disclosure, in step S103, epitaxial growth includes growth using a method of Molecular Beam Epitaxy (MBE), metal Organic Chemical Vapor Deposition (MOCVD), hydride Vapor Phase Epitaxy (HVPE).
In accordance with an embodiment of the present disclosure, a group III nitride material grown on a composite substrate includes at least one of:
gallium nitride, aluminum nitride, indium nitride, in x Ga 1-x N、In x Al 1-x N、Al x Ga 1-x N, wherein 0<x<1, a step of; wherein the thickness of the III-nitride layer is 2-5 μm, and the thickness of the III-nitride layer can meet the requirements of flexible electronic devices.
According to the embodiment of the disclosure, the growth temperature of the grown gallium nitride is 1040-1080 ℃, and the V/III ratio is 550-1500; the conditions for growing aluminum nitride are generally 1200 ℃, and the V/III ratio is 580-1154; the temperature of the growing ternary alloy is 750-1000 ℃, and the flow of the two organic metal sources can be changed according to the components for the growing ternary alloy, wherein V represents ammonia; III represents an organometallic source such as trimethylaluminum, trimethylgallium.
Fig. 3a is a schematic diagram of a structure for stripping group III nitride using wet chemical etching in an embodiment of the present disclosure.
According to another embodiment of the present disclosure, the method for preparing a group III nitride layer further includes etching the substrate surface to etch away the native oxide layer using a wet etching method after growing the group III nitride layer (5) on the composite substrate. Then, the composite substrate and the group III nitride layer were peeled off and transferred using an adhesive tape (6), and the specific structure is shown in fig. 3 a.
In accordance with an embodiment of the present disclosure, a wet etching process is used to etch a substrate surface, including, using a BOE solution (NH 4 F, etching the substrate (1) and the natural oxide layer (2) for 1-2 h by HF=6:1, and removing the natural oxide layer on the surface of the substrate.
According to an embodiment of the present disclosure, the tape (6) comprises a heat release tape or a conductive copper tape.
By the embodiment of the disclosure, the III-nitride layer is stripped and transferred by utilizing a wet chemical etching method and an adhesive tape, and the method can simply and conveniently realize large-area stripping and transferring of the III-nitride layer on the substrate without influencing the crystal quality of the III-nitride layer.
Fig. 3b is a schematic diagram of a structure for transferring a group III nitride layer onto a flexible substrate using a heat release tape in an embodiment of the present disclosure.
According to an embodiment of the present disclosure, as shown in fig. 3b, the composite substrate and the group III nitride layer are peeled off with a heat release tape and transferred onto a flexible substrate (7) for the preparation of a flexible device.
Fig. 3c is a schematic diagram of a structure after stripping and transferring a group III nitride layer using a conductive copper tape in an embodiment of the present disclosure.
According to another embodiment of the present disclosure, as shown in fig. 3c, a metal electrode (8) is prepared on a group III nitride layer (5) by electron beam evaporation, and a composite substrate and the group III nitride layer (5) with the metal electrode are peeled off and transferred by an adhesive tape (6) using a conductive copper adhesive tape, so as to obtain a conductive copper adhesive tape, the group III nitride layer (5) with the metal electrode, a nucleation layer (4) and a two-dimensional material layer (3) which are stacked in sequence from top to bottom. The conductive copper tape is used as a lower electrode of an electronic device, and metal indium (9) is placed on the stripping surface of the two-dimensional material layer (3) and can be used as an upper electrode of the electronic device, wherein the metal electrode comprises nickel or gold, and the nucleation layer is aluminum nitride.
According to the embodiment of the disclosure, the conductive copper tape is adopted to strip and transfer the composite substrate and the III-nitride layer with the metal electrode, so that the photoelectric device with the vertical structure can be directly manufactured, and the photoelectric device is not limited in size and high in flexibility.
There is also provided, in accordance with an embodiment of the present disclosure, an electronic device, wherein the electronic device includes epitaxially growing a group III nitride layer on a composite substrate through the above steps.
According to the embodiment of the disclosure, the conductive copper tape is used for stripping the composite substrate and the III-nitride layer, the conductive copper tape can be used as a lower electrode to form good contact with the metal semiconductor, and the metal indium is placed on the stripping surface of the two-dimensional material layer to be used as an upper electrode, so that the flexible photoelectric device can be obtained.
The technical scheme of the present disclosure is further explained below by specific embodiments and with reference to the accompanying drawings. It should be noted that the following specific examples are given by way of illustration only, and the scope of the present disclosure is not limited thereto.
A graphene film of a two-dimensional material is grown on a silicon substrate having silicon dioxide by Chemical Vapor Deposition (CVD), wherein the graphene film has a single-layer or double-layer structure, the silicon substrate has a (100) crystal plane, and silicon substrates having other crystal planes can be used.
And then the graphene film is placed into an MOCVD chamber, ammonia gas is introduced at 1010 ℃ for pretreatment for 2 minutes, and a dangling bond is formed on the surface of the two-dimensional material, so that nucleation sites are provided for the growth of a nucleation layer. Next, an AlN nucleation layer was grown on the graphene film using Metal Organic Chemical Vapor Deposition (MOCVD), with an AlN growth temperature of 1200 ℃, a pressure of 50torr, v/III 1155, and a growth time of 2 minutes.
Then, a gallium nitride layer was grown by Metal Organic Chemical Vapor Deposition (MOCVD) on a composite substrate composed of a graphene thin film and an AlN nucleation layer at 50Torr under a V/III of 1102 at 1200 ℃ for 1.5 hours and a final growth thickness of 3 μm, wherein the grown nitride was not limited to gallium nitride, but the method was also applicable to other grown nitrides.
Fig. 4 is an atomic force microscope image of a final gallium nitride epitaxial layer in an embodiment of the disclosure.
As shown in fig. 4, it can be seen that the surface step flow of the gallium nitride layer is remarkable, and the RMS (root mean square roughness) is only 0.437nm, which indicates that the crystal quality and flatness of the gallium nitride layer are good.
Then, BOE solution (NH) 4 F, HF=6:1) is used for corroding the surface of the composite substrate for 1 to 2 hours at normal temperature, and the composite substrate and the gallium nitride layer can be stripped by adopting the heat release adhesive tape. And transferring the stripped composite substrate and the gallium nitride layer onto a flexible substrate for forming a flexible device.
The nickel/gold electrode (the thickness of the electrode is 20nm/200 nm) can also be prepared on the gallium nitride layer by adopting an electron beam evaporation method, then the natural oxide layer on the substrate is removed by adopting a corrosion process, and the composite substrate and the III-nitride layer with the metal electrode are stripped and transferred by adopting a conductive copper tape. And taking the conductive copper tape as a lower electrode, and placing metal indium on the stripping surface of the graphene film (two-dimensional material layer) as an upper electrode to obtain the flexible photoelectric device.
In summary, since the crystal orientation during the growth of the nitride layer is arbitrary, it is difficult to grow a high quality nitride film by the whole epitaxy. By combining the two-dimensional material with the substrate, and growing the aluminum nitride nucleation layer on the surface of the two-dimensional material, the III-nitride can be epitaxially grown on the two-dimensional material in a van der Waals force combination manner. The AlN nucleation layer can reduce the random orientation of nitride crystals and improve the crystal quality of the nitride film. On the other hand, large-area stripping and transfer of nitride material on a substrate can be achieved by wet chemical etching without damaging the quality of the nitride film, and the transferred nitride film can be used for the fabrication of electronic devices, particularly flexible electronic devices.
While the foregoing is directed to embodiments of the present disclosure, other and further details of the invention may be had by the present application, it is to be understood that the foregoing description is merely exemplary of the present disclosure and that no limitations are intended to the scope of the disclosure, except insofar as modifications, equivalents, improvements or modifications may be made without departing from the spirit and principles of the present disclosure.

Claims (10)

1. A method for preparing a group III nitride layer, comprising:
growing a two-dimensional material layer on a substrate;
growing a nucleation layer on the two-dimensional material layer, wherein the two-dimensional material layer and the nucleation layer form a composite substrate for growing a III-nitride layer;
and epitaxially growing a group III nitride layer on the composite substrate.
2. The method of claim 1, wherein the method further comprises:
and after growing the III-nitride layer on the composite substrate, etching the surface of the substrate by adopting a wet etching method, and stripping and transferring the composite substrate and the III-nitride layer by adopting an adhesive tape.
3. The method of claim 1, wherein the substrate comprises: a silicon substrate.
4. The method of claim 1, wherein the two-dimensional material comprises any one of:
graphene, tungsten disulfide, molybdenum disulfide, tungsten diselenide, tungsten ditelluride, molybdenum ditelluride;
the thickness of the two-dimensional material includes: single layer or multiple layers, wherein the multiple layers are 2-10 layers.
5. The method of claim 1, wherein the nucleation layer is an aluminum nitride layer;
the aluminum nitride nucleation layer is obtained through the following steps:
adopting nitrogen or ammonia gas to treat the surface of the two-dimensional material layer, and then introducing ammonia gas and trimethylaluminum to grow an aluminum nitride nucleation layer on the surface of the treated two-dimensional material layer;
the thickness of the aluminum nitride nucleation layer comprises: 20-40nm.
6. The method of claim 1, wherein,
the epitaxial growth comprises molecular beam epitaxy, metal organic chemical vapor deposition and hydride vapor phase epitaxy.
7. The method of claim 1, wherein the group III nitride layer grown on the composite substrate comprises at least one of:
gallium nitride, aluminum nitride, indium nitride, in x Ga 1-x N、In x Al 1-x N、Al x Ga 1-x N, wherein 0<x<1；
The thickness of the III-nitride layer is 2-5 μm.
8. The method of claim 2, wherein the tape comprises: heat release tape or conductive copper tape.
9. The method of claim 2, wherein the taping the composite substrate and the group III nitride layer comprises:
depositing a metal electrode on the surface of the III-nitride layer, and then stripping and transferring the III-nitride layer with the metal electrode and the composite substrate by adopting a conductive copper tape to obtain a conductive copper tape, a III-nitride layer with the metal electrode, a nucleation layer and a two-dimensional material layer which are sequentially stacked from top to bottom;
taking the conductive copper tape as a lower electrode of an electronic device, and placing metal indium on the surface of the two-dimensional material layer as an upper electrode of the electronic device; or (b)
And transferring the stripped composite substrate and the stripped III-nitride layer to a target substrate by adopting a heat release adhesive tape to obtain the electronic device.
10. An electronic device, wherein the electronic device comprises a group III nitride layer prepared by the method of any of claims 1-9.
CN202210555451.6A 2022-05-19 2022-05-19 Method for producing a group III nitride layer and use thereof Pending CN117133639A (en)

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