CN113628967A - In-situ processing method for nitride epitaxial substrate and substrate - Google Patents

In-situ processing method for nitride epitaxial substrate and substrate Download PDF

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CN113628967A
CN113628967A CN202110677351.6A CN202110677351A CN113628967A CN 113628967 A CN113628967 A CN 113628967A CN 202110677351 A CN202110677351 A CN 202110677351A CN 113628967 A CN113628967 A CN 113628967A
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nitride
substrate
nitride film
processing method
mask layer
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郭艳敏
尹甲运
李佳
王波
张志荣
芦伟立
高楠
房玉龙
冯志红
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CETC 13 Research Institute
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Abstract

The invention is applicable to the technical field of nitride material preparation methods, and provides an in-situ processing method for a nitride epitaxial substrate and the substrate. The processing method comprises the following steps: providing a substrate, wherein the substrate is arranged in an MOCVD reaction chamber; growing a nitride film: introducing hydrogen, an MO source and ammonia gas into the reaction chamber at a first preset temperature, growing an island-shaped nitride film on the first surface of the substrate, and closing the MO source and the ammonia gas when the grown nitride film reaches a first preset thickness; and (3) etching the nitride film: raising the temperature to a second preset temperature within a first preset time, continuously introducing hydrogen to etch the surface of the nitride film, and decomposing the nitride at the junction between the island and the island; and circularly performing the steps of growing the nitride film and etching the nitride film to form a patterned mask layer with an opening, wherein the patterned mask layer is used for growing nitride epitaxy. The growth method of the nitride epitaxial material is simple, and dislocation density can be effectively reduced.

Description

In-situ processing method for nitride epitaxial substrate and substrate
Technical Field
The invention belongs to the technical field of nitride material preparation methods, and particularly relates to an in-situ processing method for a nitride epitaxial substrate and the substrate.
Background
Group III nitrides composed of GaN, AlN, InN, etc. are direct bandgap semiconductors whose bandgap width can be continuously tunable from 0.7eV for InN to 6.2eV for AlN, whose wavelength can cover the red, yellow, green, to ultraviolet spectral range, and whose large bandgap differences make heterojunctions, quantum wells, superlattices, etc. prepared using group III nitrides have superior device characteristics, and therefore group III nitrides composed of GaN, AlN, InN, etc. are of great significance for manufacturing new semiconductor devices.
Currently, GaN-based semiconductor materials are mainly heteroepitaxially grown on sapphire, Si, SiC, and other substrates. In order to reduce the dislocation density due to lattice mismatch between the hetero-substrate and the epitaxial layer, techniques such as lateral Epitaxy (ELOG) and Selective Area Growth (SAG) are widely used in the epitaxy of nitride materials.
However, the conventional ELOG and SAG technologies require complex semiconductor process technologies such as dielectric deposition, photolithography and etching, and have complex processes and high cost, thereby restricting the wide application of the technologies. Therefore, how to simplify the process becomes a key to the wide application of technologies such as lateral epitaxy and selective area growth in the field of nitride material epitaxy.
Disclosure of Invention
In view of the above, the present invention provides an in-situ processing method for a nitride epitaxial substrate and a substrate, and aims to solve the problems that the prior art is complex in process and cannot improve the quality of nitride epitaxy. A patterned nitride thin film layer is prepared on a substrate in advance and is used as a mask layer, and the dislocation density in an epitaxial layer is reduced by utilizing the characteristic of selectivity of epitaxial growth of nitride.
To achieve the above object, in a first aspect, the present invention provides an in-situ processing method for a nitride epitaxial substrate, comprising:
providing a substrate, wherein the substrate is arranged in an MOCVD reaction chamber;
growing a nitride film: introducing hydrogen, an MO source and ammonia gas into the reaction chamber at a first preset temperature, growing an island-shaped nitride film on the first surface of the substrate, and closing the MO source and the ammonia gas when the grown nitride film reaches a first preset thickness;
and (3) etching the nitride film: raising the temperature to a second preset temperature within a first preset time, continuously introducing hydrogen to etch the surface of the nitride film, and decomposing the nitride at the junction between the island and the island; wherein the second preset temperature is higher than the first preset temperature;
and circularly performing the steps of growing the nitride film and etching the nitride film to form a patterned mask layer with an opening, wherein the substrate with the patterned mask layer is used for growing the nitride epitaxial material.
According to the in-situ processing method for the nitride epitaxial substrate, the island-shaped nitride film grows on the surface of the substrate, and then the nitride film is etched at high temperature by utilizing hydrogen, so that the nitride film is decomposed at the junction of the island-shaped nitride film and the island-shaped nitride film, and the substrate at the decomposition position is exposed. And repeating the growth and the etching of the nitride film to obtain the patterned mask layer with randomly distributed openings, namely, the nitride film does not exist on the substrate of a part of the area, and the nitride film is arranged on the substrate of the part of the area. Wherein, the nitride film left on the substrate can be used as a mask layer for subsequent epitaxial growth. The region without the nitride film is a window region, and due to the difference of surface energy, subsequent epitaxial materials can grow rapidly in the window region. The treatment method has simple process and can be widely used.
In a possible implementation manner, the material of the grown nitride thin film is one or a combination of several of GaN, AlN, BN, InN, AlGaN, InGaN, BGaN, or BAlN.
In some embodiments, the first predetermined thickness is in a range of 10nm to 200 nm.
In one possible implementation, the first preset temperature ranges from 700 ℃ to 1200 ℃.
In one possible implementation, the second preset temperature ranges from 1000 ℃ to 1600 ℃.
In some embodiments, the first predetermined time is in the range of 1 to 20 minutes.
In one possible implementation, the thickness of the patterned mask layer is in a range of 200nm to 1000 μm.
In one possible implementation, the growth pressure of the nitride film is in the range of 50mbar to 500 mbar.
In a possible implementation manner, the material of the nitride epitaxy is one or a combination of several of GaN, AlN, BN, InN, AlGaN, InGaN, BGaN, or BAlN.
On the other hand, the invention also provides a substrate for the nitride epitaxial material, which comprises a substrate body and a patterned mask layer grown on the first surface of the substrate body, wherein the patterned mask layer is prepared by adopting any one of the methods.
The substrate provided by the embodiment of the application is prepared by adopting the in-situ processing method of the nitride epitaxial substrate. Firstly, a patterned mask layer with unevenly distributed openings on the surface is grown on the first surface of the substrate, and then an epitaxial layer is grown on the patterned mask layer. The epitaxial material will preferentially grow in the window area of the nitride film without the patterned mask layer and then combine with the epitaxial material grown on the mask layer provided with the nitride film to finally form a flat epitaxial layer surface. The method has the advantages that the selective growth is realized on the substrate with the patterned mask layer by utilizing the characteristic that the epitaxial growth of the nitride material has selectivity, a large number of dislocation defects are stopped at the interface of the mask layer and the epitaxial layer, the dislocation density in the nitride film of the epitaxial layer is effectively reduced, the crystal quality is not improved to the greatest extent, the treatment process is simple, and the method is convenient to widely use.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise.
Fig. 1 is a schematic view of an in-situ processing method for a nitride epitaxial substrate according to an embodiment of the present invention;
in the figure: 1-substrate, 2-nitride film, 3-nitride epitaxy.
Detailed Description
In the following description, for purposes of explanation and not limitation, specific details are set forth, such as particular system structures, techniques, etc. in order to provide a thorough understanding of the embodiments of the invention. It will be apparent, however, to one skilled in the art that the present invention may be practiced in other embodiments that depart from these specific details. In other instances, detailed descriptions of well-known systems, devices, circuits, and methods are omitted so as not to obscure the description of the present invention with unnecessary detail.
In order to explain the technical means of the present invention, the following description will be given by way of specific examples.
Since nitride epitaxial growth typically employs heteroepitaxy on other substrate materials, the quality of the resulting epitaxial layers is generally poor due to differences in lattice and thermal expansion coefficients and due to interface chemistry problems. However, the crystal quality of the epitaxial layer is poor, the development of photoelectric and electronic devices is severely restricted, and the improvement of the epitaxial growth technology plays a key role in improving the crystal quality of the epitaxial layer.
Referring to fig. 1, an in-situ processing method for a nitride epitaxial substrate in the present embodiment includes:
firstly, placing a substrate 1 in an MOCVD reaction chamber, and secondly, growing a nitride thin film 2 includes: at a first preset temperature, hydrogen is taken as carrier gas in a reaction chamber, and an MO source and ammonia gas are introduced, wherein the MO source and the ammonia gas can grow on the first surface of the substrate 1 to form an island-shaped nitride film 2. When the thickness of the grown nitride thin film 2 reaches the first preset thickness, the MO source and ammonia gas are turned off, and the growth of the nitride thin film 2 is stopped.
Then, etching the nitride thin film 2 includes: and within the first preset time, raising the temperature to a second preset temperature, wherein the second preset temperature is higher than the first preset temperature, the continuously introduced hydrogen can etch the surface of the nitride film 2, and the nitride film 2 can start to decompose from the junction between the islands to leak out of the first surface of the substrate 1. The steps of growing the nitride film 2 and etching the nitride film 2 are performed cyclically until a patterned mask layer having openings is formed on the first surface of the substrate 1. The patterned mask layer described above may be used to grow nitride epitaxy. These patterned mask layers may function as a microregion mask.
Finally, nitride epitaxy 3 is grown on the upper surface of the nitride film 2 of the patterned mask layer with randomly distributed openings, wherein the nitride epitaxy 3 is an epitaxial material. At this time, the nitride epitaxy 3 is first nucleated on the surface without the patterned mask layer, and the nucleated particles gradually grow and merge with each other to finally form a flat surface.
According to the in-situ processing method for the nitride epitaxial substrate, the island-shaped nitride film grows on the surface of the substrate, and then the nitride film is etched at high temperature by utilizing hydrogen, so that the nitride film is decomposed at the junction of the island-shaped nitride film and the island-shaped nitride film, and the substrate at the decomposition position is exposed. And repeating the growth and the etching of the nitride film to obtain the patterned mask layer with randomly distributed openings, namely, the nitride film does not exist on the substrate of a part of the area, and the nitride film is arranged on the substrate of the part of the area. Wherein, the nitride film left on the substrate can be used as a mask layer for subsequent epitaxial growth. The region without the nitride film is a window region, and due to the difference of surface energy, subsequent epitaxial materials can grow rapidly in the window region. Therefore, the nucleation layer of the nitride epitaxial material can be prevented from directly growing on the substrate, dislocation is avoided, and the epitaxial quality is improved.
In some embodiments, the material of the nitride thin film 2 is one or a combination of GaN, AlN, BN, InN, AlGaN, InGaN, BGaN, or BAlN. Nitride films 2 of different materials can be grown on the first surface of the substrate 1 according to device requirements.
Specifically, the first predetermined thickness is in a range of 10nm to 200 nm. When the thickness of the nitride thin film 2 reaches 10nm to 200nm, the specific thickness can be set as required, the MO source and ammonia gas are turned off, and the growth of the nitride thin film 2 is stopped.
In some possible implementations, the first preset temperature ranges from 700 ℃ to 1200 ℃. When the temperature is raised to a first predetermined temperature, the nitride thin film 2 starts to grow.
In some embodiments, the second predetermined temperature is in the range of 1000 ℃ to 1600 ℃, and the second predetermined temperature is higher than the first predetermined temperature. When the temperature rises to a second preset temperature, the island-shaped nitride film 2 is etched by hydrogen at a high temperature, so that part of the nitride film 2 starts to be decomposed at the junction between the island and the island, and leaks out of the first surface of the substrate 1 at the lower part of the nitride film 2.
In some embodiments, the first predetermined time is in the range of 1-20 minutes. And in the first preset time, the hydrogen can etch the nitride film 2 at high temperature all the time, and after the first preset time is reached, the temperature is reduced, and the etching is stopped.
In some possible implementations, the second predetermined thickness is in a range of 200nm to 1000 μm. When the total thickness of the nitride film 2 layer reaches the second preset thickness, the nitride film 2 growth and etching are stopped from being repeatedly performed. At this point a patterned mask layer, i.e. a layer of nitride film 2 with randomly distributed openings, has been formed on the first surface of the substrate 1.
Specifically, the pressure range during the growth of the entire nitride thin film 2 is 50mbar to 500 mbar.
In some possible implementations, the material of the nitride epitaxy 3 is one or a combination of GaN, AlN, BN, InN, AlGaN, InGaN, BGaN, or BAlN.
In the embodiment of the invention, a nitride film 2 layer with randomly distributed openings is grown on the first surface of a substrate 1 to be used as a patterned mask layer. Thereby, the nitride film 2 is not formed on the partial area substrate 1, and the nitride film 2 is provided on the partial area substrate 1. Therefore, the selective growth can be realized on the substrate 1 with the patterned mask layer by utilizing the characteristic that the epitaxial growth of the nitride epitaxial 3 material has growth selectivity, a large number of dislocation defects are stopped at the interface of the patterned mask layer and the nitride layer, the epitaxial dislocation density is effectively reduced, and the crystal quality is improved.
The invention also provides a substrate for the nitride epitaxial material, which comprises a substrate 1 and a nitride film 2. A patterned mask layer is grown on the first surface of the substrate 1. The patterned mask layer is the nitride film 2 prepared by the method, and uneven openings are distributed on the surface of the patterned mask layer. Wherein a nitride film 2 is arranged on the substrate of a partial region, and the nitride film 2 is not arranged on the substrate of the partial region. A nitride epitaxy 3 is provided on the surface of the nitride thin film 2. The nitride epitaxy 3 may be a nucleation layer of nitride epitaxial material.
The substrate provided by the embodiment of the application is prepared by adopting the in-situ processing method for the nitride epitaxial substrate. Firstly, growing a nitride film with unevenly distributed openings on the surface on the first surface of the substrate as a patterned mask layer, and then growing an epitaxial layer on the patterned mask layer. The epitaxial material will preferentially grow in the window area without the nitride film and then combine with the epitaxial material grown on the mask layer provided with the nitride film to finally form a flat epitaxial layer surface. According to the method, the selective growth is realized on the substrate with the patterned mask layer by utilizing the characteristic that the epitaxial growth of the nitride material has selectivity, a large number of dislocation defects are stopped at the interface of the mask layer and the epitaxial layer, the dislocation density in the nitride film of the epitaxial layer is effectively reduced, and the crystal quality is improved. Meanwhile, the method can be carried out in situ in nitride deposition equipment, is economical and economical, is simple and feasible, has good epitaxial material performance, and is an effective solution for realizing the high-quality and low-cost growth of the nitride film.
On the other hand, the embodiment of the invention also provides a preparation method of the GaN HEMT on the high-quality sapphire substrate. The method specifically comprises the following steps:
first, a 20nm island-shaped GaN mask layer was grown on a sapphire substrate using MOCVD equipment. Wherein the growth temperature is 800 ℃, the pressure is 100mbar, the flow of TMGa is 100sccm, the ammonia gas is 30L, and the carrier gas is hydrogen gas 50L. And secondly, closing the TMGa source and ammonia gas, heating to 1100 ℃, and carrying out high-temperature etching for 5 minutes by using hydrogen gas. And repeatedly growing the island-shaped GaN mask layer and etching the island-shaped GaN mask layer by hydrogen at high temperature for three times. Then, a 1200nm GaN buffer layer was grown on the finally grown GaN mask layer with randomly distributed openings. Wherein the temperature is 1000 ℃, the pressure is 200mbar, the flow rate of TMGa is 200sccm, the ammonia gas is 20L, and the carrier gas adopts 30L of hydrogen gas. Subsequently, a 100nm thick GaN channel layer and a 20nm thick AlGaN barrier layer, in which the Al composition was 20%, were sequentially grown on the GaN buffer layer. Thereby preparing the GaN HEMT on the high-quality sapphire substrate.
In the above embodiments, the descriptions of the respective embodiments have respective emphasis, and reference may be made to the related descriptions of other embodiments for parts that are not described or illustrated in a certain embodiment.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not substantially depart from the spirit and scope of the embodiments of the present invention, and are intended to be included within the scope of the present invention.

Claims (10)

1. An in-situ processing method for a nitride epitaxial substrate, comprising:
providing a substrate, wherein the substrate is arranged in an MOCVD reaction chamber;
growing a nitride film: introducing hydrogen, an MO source and ammonia gas into the reaction chamber at a first preset temperature, growing an island-shaped nitride film on the first surface of the substrate, and closing the MO source and the ammonia gas when the grown nitride film reaches a first preset thickness;
and (3) etching the nitride film: raising the temperature to a second preset temperature within a first preset time, continuously introducing hydrogen to etch the surface of the nitride film, and decomposing the nitride at the junction between the island and the island; wherein the second preset temperature is higher than the first preset temperature;
and circularly performing the steps of growing the nitride film and etching the nitride film to form a patterned mask layer with an opening, wherein the substrate with the patterned mask layer is used for growing the nitride epitaxial material.
2. The in-situ processing method for a nitride epitaxial substrate according to claim 1 wherein the grown nitride thin film is one or a combination of several of GaN, AlN, BN, InN, AlGaN, InGaN, BGaN or BAlN.
3. The in-situ processing method for a nitride epitaxial substrate according to claim 2, characterized in that the first predetermined thickness is in the range of 10nm to 200 nm.
4. The in-situ processing method for a nitride epitaxial substrate according to claim 1 wherein the first preset temperature is 700 ℃ -1200 ℃.
5. The in-situ processing method for a nitride epitaxial substrate according to claim 4, characterized in that the second predetermined temperature is 1000 ℃ -1600 ℃.
6. The in-situ processing method for a nitride epitaxial substrate according to claim 5 wherein the first predetermined time is 1 to 20 minutes.
7. The in-situ processing method for a nitride epitaxial substrate according to claim 1, wherein the thickness of the patterned mask layer is 200nm-1000 μ ι η.
8. The in-situ processing method for a nitride epitaxial substrate according to claim 1, characterized in that the growth pressure range of the nitride thin film is 50mbar-500 mbar.
9. The in-situ processing method for the nitride epitaxial substrate according to claim 1, characterized in that the material of the nitride epitaxy is one or a combination of several of GaN, AlN, BN, InN, AlGaN, InGaN, BGaN or BAlN.
10. A substrate for a nitride epitaxial material, comprising a substrate body and a patterned mask layer grown on a first surface of the substrate body, the patterned mask layer being prepared by the method of any one of claims 1 to 9.
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CN112820626A (en) * 2020-12-30 2021-05-18 中国科学院长春光学精密机械与物理研究所 Epitaxial growth method of nitride semiconductor material

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CN104393125A (en) * 2014-12-17 2015-03-04 安徽三安光电有限公司 Method for preparing light emitting element
CN107919392A (en) * 2017-11-09 2018-04-17 中国电子科技集团公司第五十五研究所 Gallium nitride base nitride high electronic migration rate transmistor epitaxial structure and growing method
CN112820626A (en) * 2020-12-30 2021-05-18 中国科学院长春光学精密机械与物理研究所 Epitaxial growth method of nitride semiconductor material

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