CN111933513A - Method for preparing nitride semiconductor material - Google Patents
Method for preparing nitride semiconductor material Download PDFInfo
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- CN111933513A CN111933513A CN201910392871.5A CN201910392871A CN111933513A CN 111933513 A CN111933513 A CN 111933513A CN 201910392871 A CN201910392871 A CN 201910392871A CN 111933513 A CN111933513 A CN 111933513A
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
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- H01L21/02538—Group 13/15 materials
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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Abstract
The invention provides a method for preparing a nitride semiconductor material, which comprises the following steps: (1) forming a high absorption layer on one surface of a substrate; (2) depositing a nitride semiconductor material by means of microwave heating on the highly absorbing layer or on another surface of the substrate opposite to the highly absorbing layer; the high absorption layer is formed of a material having a dielectric loss tangent of not less than 0.01. By the method of the present invention, uniform heat conduction to the nitride semiconductor material can be achieved. Meanwhile, the method has higher energy utilization efficiency. In the method, the energy is intensively absorbed by the material to be heated, so that the cavity of the vacuum deposition equipment is not heated, and the maintenance and the use of the equipment are prolonged.
Description
Technical Field
The invention relates to the field of semiconductor materials. In particular, the present invention relates to a method for producing a nitride semiconductor material.
Background
With the progress of semiconductor production and manufacturing technology, and the progress of technology and social development, the application field of semiconductors is more and more extensive, and the requirements for the performance of semiconductors are higher and higher. The semiconductor material not only has great application in the photoelectric field, but also is a cornerstone in the power electronic field. Especially group iii-v semiconductor materials.
High temperature processes must be performed during the growth of the semiconductor material, even after the growth of the structure is complete, to achieve the final function. The high temperature process serves to promote the growth of the material, activate elements, release stress and the like. At present, in material growth equipment (such as MOCVD and MBE), a resistance wire heating method or an infrared heating method is mainly adopted. The strength of the resistance wire is low in a high-temperature environment, the plasticity of the heating wire can be enhanced along with the increase of the temperature, the resistance wire is easy to deform at high temperature, and the resistance wire is not easy to repair after deformation. The infrared heating reaction is too fast, and the temperature rise is too fast.
The main advantages of microwave heating include: instantaneous application and withdrawal of energy; directly heating the material instead of thermally conducting, both the interior and the surface of the material being heated; the structure can be selectively heated, so that the grown structure can be independently heated instead of the cavity of the whole equipment, the growth of the material is simpler and easier, for example, when gallium nitride is grown on sapphire, because the microwave only heats the gallium nitride and does not heat the sapphire, the thermal stress can be more simply regulated and controlled. Moreover, since the gallium nitride material can absorb microwave energy in the whole, the gallium nitride material can be heated more uniformly.
Disclosure of Invention
In order to overcome the disadvantages of the prior art, the present invention provides a novel method for preparing a nitride semiconductor material. The novel method for preparing the nitride semiconductor material is carried out in a microwave heating mode. By the method of the present invention, uniform heat conduction to the nitride semiconductor material can be achieved. Meanwhile, the method has higher energy utilization efficiency.
The above object of the present invention is achieved by the following means.
The invention provides a method for preparing a nitride semiconductor material, which comprises the following steps:
(1) forming a high absorption layer on one surface of a substrate;
(2) depositing a nitride semiconductor material by means of microwave heating on the highly absorbing layer or on another surface of the substrate opposite to the highly absorbing layer;
the high absorption layer is formed of a material having a dielectric loss tangent of not less than 0.01.
Preferably, in the method of the present invention, the substrate is a sapphire, silicon or silicon carbide substrate.
Preferably, in the method of the present invention, the high absorption layer is made of GaO, ZnO, TiO2And formula AlxGa(1-x)One or more of N compounds, wherein x is more than or equal to 0 and less than or equal to 1.
Preferably, in the method of the present invention, the high absorption layer is formed of GaN and/or AlN.
Preferably, in the method of the present invention, the thickness of the high absorption layer is 50nm to 2 μm.
Preferably, in the method of the present invention, the forming of the high absorption layer in the step (1) is performed by physical or chemical deposition.
Preferably, in the method of the present invention, the physical or chemical deposition is performed by sputtering, evaporation, chemical vapor deposition, atomic layer deposition or molecular beam epitaxy.
Preferably, in the method of the present invention, the method further includes a step of patterning the high absorption layer after the step (1) and before the step (2).
Preferably, in the method of the present invention, the microwave heating is performed under the following conditions: the frequency of the microwave heating source is controlled to be 2GHz-20GHz in the vacuum deposition chamber.
The invention has the beneficial effects that:
(1) the method has wide application range: in the present invention, the nitride semiconductor material includes, but is not limited to, group III-V semiconductor materials and metal oxide semiconductor materials thereof. For example, a gallium nitride-based LED structure, a gallium nitride-based HEMT structure, or a gallium nitride-based detector structure can be fabricated using the method of the present invention.
(2) The method of the invention can realize uniform heat conduction to the nitride semiconductor material by virtue of the high absorption effect of the high absorption layer on the microwave. Meanwhile, the method has higher energy utilization efficiency. In the method, the energy is intensively absorbed by the material to be heated, so that the cavity of the vacuum deposition equipment is not heated, and the maintenance and the use of the equipment are prolonged.
Drawings
Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a flow chart of the method of example 1 of the present invention;
FIG. 2 is a flow chart of a method of embodiment 2 of the present invention;
FIG. 3 is a flow chart of a method of embodiment 3 of the present invention;
FIG. 4 is a flow chart of a method of embodiment 4 of the present invention;
fig. 5 is a schematic sectional view of the structure of a nitride semiconductor material prepared on a high absorption layer by microwave heating in example 1 of the present invention;
fig. 6 is a schematic sectional view showing the structure of a nitride semiconductor material prepared on a patterned high absorption layer by microwave heating in example 2 of the present invention;
fig. 7 is a schematic sectional view of the structure of a nitride semiconductor material prepared on the other surface of the substrate opposite to the high absorption layer by microwave heating in embodiment 3 of the present invention;
fig. 8 is a schematic sectional view showing the structure of a nitride semiconductor material prepared on a high absorption layer by microwave heating in example 4 of the present invention;
FIG. 9 is a SEM scan of a cross section of a material prepared in example 4 of the present invention;
FIG. 10 is an AFM scan of a material prepared in example 4 of the present invention;
FIG. 11 shows the current-voltage characteristics of an LED device fabricated with the structure grown in example 4 of the present invention;
wherein the reference numbers are as follows:
1 substrate
2 high absorption layer
3 nitride semiconductor material.
Detailed Description
The present invention is described in further detail below with reference to specific embodiments, which are given for the purpose of illustration only and are not intended to limit the scope of the invention.
Example 1
The embodiment relates to a method for preparing a nitride semiconductor material by microwave heating, and the specific flow is shown in figure 1, and the method comprises the following steps:
(1) providing a 2-inch sapphire substrate required for growth;
(2) growing a layer of aluminum nitride (AlN) on a surface of a substrate;
the AlN material is prepared by a sputtering method, the substrate temperature is 200 ℃, and N is2The flow ratio of/Ar is 1: 2, the working pressure is 0.1Pa, and the thickness of the grown AlN material is 100 nm;
(3) on an AlN material, preparing a nitride semiconductor material by microwave heating in an MOCVD chamber with the vacuum degree of 400mbar to form a GaN-based LED;
in the process of growing the nitride semiconductor material, at least one microwave emitting source is used for heating the AlN layer, the frequency of the microwave source is 2.4GHz, and the AlN is heated to 1150 ℃ to grow the nitride semiconductor material. By means of the high absorption effect of AlN on microwaves, on one hand, uniform heat conduction on nitride semiconductor materials is guaranteed, and the problem of low non-contact efficiency is solved; on the other hand, since the area of AlN corresponds to the nitride semiconductor material, the efficiency of energy utilization is improved. Firstly, growing a GaN buffer layer with the thickness of about 600nm on the surface of AlN; the substrate is then heated to 1050 ℃ by microwaves; then 4um N-type GaN is deposited, the substrate is cooled to 800 ℃, and then a GaN/InGaN multiple quantum well structure is deposited; and then raising the temperature to 900 ℃, and growing the P-type Mg-doped GaN on the surface of the quantum well to finish the growth of the structure. Fig. 5 is a schematic cross-sectional view illustrating a structure of a nitride semiconductor material fabricated on a high absorption layer by microwave heating according to the present embodiment.
Example 2
The embodiment relates to a method for preparing a semiconductor material by microwave heating, and the specific flow is shown in figure 2, and the method comprises the following steps:
(1) providing a 2-inch silicon substrate required for growth;
(2) growing a layer of aluminum nitride (AlN) material on a surface of the substrate;
the AlN material is prepared by a sputtering method, the substrate temperature is 200 ℃, and N is2The flow ratio of/Ar is 1: 2, the working pressure is 0.1Pa, and the thickness of the grown AlN material is 1.5 mu m;
(3) patterning the aluminum nitride material;
preparing a photoresist pattern with a periodic structure by using methods such as ultraviolet exposure or nano-imprinting, and the like, and then transferring the pattern to AlN by using an etching method to prepare a pattern with the depth of 100 nm;
(4) on an AlN material, preparing a nitride semiconductor material by microwave heating in an MOCVD chamber with the vacuum degree of 400mbar to form a GaN-based LED;
in the process of growing the nitride semiconductor material, the aluminum nitride layer is heated by at least one microwave emitting source with the microwave power of 6.5GHz, and the nitride semiconductor material is grown by specifically heating AlN to 1150 ℃. By means of the high absorption effect of AlN on microwaves, on one hand, uniform heat conduction on nitride semiconductor materials is guaranteed, and the problem of low non-contact efficiency is solved; on the other hand, since the area of the aluminum nitride corresponds to the nitride semiconductor material, the utilization efficiency of energy is improved. Firstly, growing a GaN buffer layer with the thickness of about 500nm on the surface of AlN; the substrate is then heated to 1050 ℃ by microwaves; then 4um N-type GaN is deposited, the substrate is cooled to 800 ℃, and then a GaN/InGaN multiple quantum well structure is deposited; and then raising the temperature to 900 ℃, and growing the P-type Mg-doped GaN on the surface of the quantum well to finish the growth of the structure. Fig. 6 is a schematic cross-sectional view illustrating a structure of a nitride semiconductor material fabricated on a patterned high absorption layer by microwave heating according to the present embodiment.
Example 3
The embodiment relates to a method for preparing a semiconductor material by microwave heating, and the specific flow is shown in fig. 3, and the method comprises the following steps:
(1) providing a 2-inch sapphire substrate required for growth;
(2) growing a layer of titanium dioxide (TiO) on a surface of a substrate2);
TiO2The material is prepared by a sputtering method, the substrate temperature is 200 ℃, and N is2The flow ratio of/Ar is 1: 2, working pressure of 0.1Pa, growing TiO2The thickness of the material is 100 nm;
(3) preparing a nitride semiconductor material to form a GaN-based LED by microwave heating in a cavity with a vacuum degree of 400 mbarr on the other surface of the substrate opposite to the titanium dioxide;
in the process of growing the nitride semiconductor material, the titanium dioxide layer is heated by at least one microwave emitting source with the microwave frequency of 16GHz, and the growth of the nitride semiconductor material is carried out by specifically heating the titanium dioxide to 1150 ℃. By means of the high microwave absorption of titanium dioxide, uniform heat conduction to the nitride semiconductor material is ensured on one hand; on the other hand, since the area of titanium dioxide corresponds to the nitride semiconductor material, the utilization efficiency of energy is improved. Firstly, growing a GaN buffer layer with the thickness of about 700nm on the surface of a substrate opposite to titanium dioxide; the substrate is then heated to 1050 ℃ by microwaves; then 4um N-type GaN is deposited, the substrate is cooled to 800 ℃, and then a GaN/InGaN multiple quantum well structure is deposited; and then raising the temperature to 900 ℃, and growing the P-type Mg-doped GaN on the surface of the quantum well to finish the growth of the structure. Fig. 7 is a schematic sectional view showing the structure of a nitride semiconductor material of the present embodiment prepared on the other surface of the substrate opposite to the high absorption layer by microwave heating.
Example 4
The embodiment relates to a method for preparing a semiconductor material by microwave heating, and the specific flow is shown in fig. 4, and the method comprises the following steps:
(1) providing a 2-inch sapphire substrate required for growth;
(2) growing a layer of GaN material on one surface of the substrate;
the GaN material is grown in a resistance heating mode, the substrate is heated to 1150 ℃ in a resistance wire heating mode, the growth of a GaN buffer layer is carried out in an MOCVD chamber with the vacuum degree of 400mbar, and the thickness of the grown GaN material is 200 nm;
(3) on a GaN material, preparing a nitride semiconductor material by microwave heating in a cavity with the vacuum degree of 400 mbarr MOCVD so as to form a GaN-based LED;
in the process of growing the nitride semiconductor material, the GaN buffer layer is heated by not less than one microwave emitting source, the microwave frequency is 2.56GHz, and the growth of the nitride semiconductor material is performed by specifically heating GaN to a suitable temperature. By means of the high absorption effect of GaN on microwave, uniform heat conduction on nitride semiconductor materials is ensured, and the problem of low non-contact efficiency is solved; on the other hand, since the area of the aluminum nitride corresponds to the nitride semiconductor material, the utilization efficiency of energy is improved. Heating the substrate to 1050 ℃ by microwaves; then 4um N-type GaN is deposited, the substrate is cooled to 800 ℃, and then a GaN/InGaN multiple quantum well structure is deposited; and then raising the temperature to 900 ℃, and growing the P-type Mg-doped GaN on the surface of the quantum well to finish the growth of the structure. Fig. 8 is a schematic sectional view showing the structure of the nitride semiconductor material prepared on the high absorption layer by microwave heating in the present embodiment. FIG. 9 is a SEM scan of a cross section of the material prepared in this example. Fig. 9 shows a clear layered structure, and a clear interface between the nitride semiconductor material and the sapphire substrate. FIG. 10 is an AFM scan of the material prepared in this example. Fig. 10 shows that the morphology of the surface of the resulting material conforms to the morphology of a normal nitride material. Fig. 11 shows the current-voltage characteristics of the LED device fabricated by using the structure grown in this example, and it can be seen that the LED device fabricated by the present invention has normal performance.
Claims (9)
1. A method of preparing a nitride semiconductor material, comprising the steps of:
(1) forming a high absorption layer on one surface of a substrate;
(2) depositing a nitride semiconductor material by means of microwave heating on the highly absorbing layer or on another surface of the substrate opposite to the highly absorbing layer;
the high absorption layer is formed of a material having a dielectric loss tangent of not less than 0.01.
2. The method of claim 1, wherein the substrate is a sapphire, silicon, or silicon carbide substrate.
3. The method of claim 1, wherein the high absorption layer is made of GaO, ZnO, TiO2And formula AlxGa(1-x)One or more of N compounds, wherein x is more than or equal to 0 and less than or equal to 1.
4. The method of claim 3, wherein the high absorption layer is formed of GaN and/or AlN.
5. The method of claim 1, wherein the thickness of the high absorption layer is 50nm-2 μ ι η.
6. The method according to claim 1, wherein the forming of the high absorption layer in the step (1) is performed by physical or chemical deposition.
7. The method of claim 6, wherein the physical or chemical deposition is by sputtering, evaporation, chemical vapor deposition, atomic layer deposition, or molecular beam epitaxy deposition.
8. The method of claim 1, further comprising, after step (1) and before step (2), the step of patterning the superabsorbent layer.
9. The method of claim 1, wherein the microwave heating is performed under the following conditions: the frequency of the microwave heating source is controlled to be 2GHz-20GHz in the vacuum deposition chamber.
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CN112635323A (en) * | 2020-12-15 | 2021-04-09 | 中国科学院上海微系统与信息技术研究所 | Preparation method of SiC-based heterogeneous integrated gallium nitride film and HEMT device |
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CN112635323A (en) * | 2020-12-15 | 2021-04-09 | 中国科学院上海微系统与信息技术研究所 | Preparation method of SiC-based heterogeneous integrated gallium nitride film and HEMT device |
CN112635323B (en) * | 2020-12-15 | 2021-12-28 | 中国科学院上海微系统与信息技术研究所 | Preparation method of SiC-based heterogeneous integrated gallium nitride film and HEMT device |
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