CN113437186A - Preparation method of AlGaN film - Google Patents

Preparation method of AlGaN film Download PDF

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CN113437186A
CN113437186A CN202110715925.4A CN202110715925A CN113437186A CN 113437186 A CN113437186 A CN 113437186A CN 202110715925 A CN202110715925 A CN 202110715925A CN 113437186 A CN113437186 A CN 113437186A
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thin film
algan
aln
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porous
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王军喜
张睿洁
郭亚楠
刘志彬
闫建昌
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Institute of Semiconductors of CAS
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    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005—Processes
    • H01L33/0062—Processes for devices with an active region comprising only III-V compounds
    • H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
    • H01L33/007—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
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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
    • H01L21/02436—Intermediate layers between substrates and deposited layers
    • H01L21/02439—Materials
    • H01L21/02455—Group 13/15 materials
    • H01L21/02458—Nitrides
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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
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    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
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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
    • H01L21/02656—Special treatments
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    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S5/00—Semiconductor lasers
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    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
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Abstract

The present disclosure provides a method for preparing an AlGaN thin film, including: carrying out heat treatment on the substrate to enable the growth surface of the substrate to be converted into an island-shaped fluctuation structure; growing a porous AlN thin film on the growth surface; and growing an AlGaN film with a combined surface on the porous AlN film. The method can not only improve the crystal quality of the epitaxial layer, but also effectively relieve the stress of the epitaxial layer through the porous structure, thereby preparing the high-quality AlGaN film.

Description

Preparation method of AlGaN film
Technical Field
The disclosure relates to the technical field of semiconductor materials, in particular to a preparation method of an AlGaN film.
Background
The energy gap of the AlGaN material can be continuously adjusted between 3.4-6.2eV, an ultraviolet light emitting diode (UV LED) and an ultraviolet laser (UV LD) prepared by the material can cover a wavelength interval of 200-365 nm, and a light emitting interval covers UV-A, UV-B and UV-C wave bands, so that the AlGaN material has the advantages of low power consumption, low voltage, no mercury, environmental protection, portability, flexibility, easy adjustment of wavelength, high reliability and the like.
The material quality of AlGaN is one of the main factors affecting the performance of the ultraviolet photoelectric device. Because large-size, low defect density AlN single crystal substrates are difficult to obtain, AlGaN materials are typically epitaxially grown on heterogeneous substrates such as sapphire, silicon carbide, and the like. The silicon carbide substrate is applied to sapphire as a substrate material to a wide extent, and has the advantages of good chemical stability, good electrical conductivity, good heat conductivity and the like. The lattice mismatch between the silicon carbide substrate and AlGaN is small, but there is still a high thermal mismatch between the two. The silicon carbide substrate has a thermal expansion coefficient of about 3.07 x 10-6The AlGaN has a high coefficient of thermal expansion (4.2 to 5.59X 10)-6at/DEG C), high-density defects and even cracking are easily generated when AlN and AlGaN epitaxial layers are subjected to strong tensile stress in the epitaxial and cooling processes.
BRIEF SUMMARY OF THE PRESENT DISCLOSURE
Based on this, the present disclosure provides a method for preparing an AlGaN thin film, including: carrying out heat treatment on the substrate to enable the growth surface of the substrate to be converted into an island-shaped fluctuation structure; growing a porous AlN thin film on the growth surface; and growing the AlGaN film with the combined surface on the porous AlN film.
According to an embodiment of the present disclosure, wherein thermally treating the substrate comprises: placing the substrate in a gas atmosphere, heating to a predetermined temperature range and maintaining the temperature for a predetermined period of time, wherein the gas atmosphere comprises pure H2Atmosphere or H2/NH3And (3) mixing the gas atmosphere, wherein the preset temperature range is 800-1500 ℃, and the preset time period range is 30s-60 min.
According to an embodiment of the present disclosure, wherein growing the porous AlN thin film on the growth surface includes: and growing the porous AlN thin film on the growth surface by adopting a one-step method or a two-step method.
According to an embodiment of the present disclosure, wherein growing a porous AlN thin film on a growth surface using a one-step method includes: and introducing an Al source and an N source, and setting the growth temperature to 900-1300 ℃ to grow the porous AlN thin film.
According to an embodiment of the present disclosure, wherein growing the porous AlN thin film on the growth surface using a two-step method includes: introducing an Al source and an N source, and setting the growth temperature to 600-1100 ℃ to grow the AlN nucleating layer; and raising the temperature to 1000-1350 ℃ to grow an AlN high-temperature layer on the AlN nucleating layer, wherein the surface of the AlN high-temperature layer is of a porous structure.
According to an embodiment of the present disclosure, growing a surface-merged AlGaN thin film on a porous AlN thin film includes: and introducing an Al source, a Ga source and an N source, and setting the growth temperature to 1000-1150 ℃ to grow the AlGaN film.
According to an embodiment of the present disclosure, wherein the substrate is a silicon carbide substrate and the growth surface is a silicon surface.
According to an embodiment of the present disclosure, before growing the surface-merged AlGaN thin film on the porous AlN thin film, the method further includes: growing an insertion layer on the porous AlN thin film, and growing the AlGaN thin film on the insertion layer, wherein the insertion layer comprises a composition gradually-changed structure or AlxGal-xN/AlyGal-yN superlattice or an intermediate composition layer or an intermediate temperature layer, x is more than or equal to 0, y is less than or equal to 1, and x is not equal to y.
According to an embodiment of the present disclosure, prior to thermally treating the substrate, the method further comprises: sequentially putting the substrate into a concentrated sulfuric acid/hydrogen peroxide mixed solution, a hydrofluoric acid solution and deionized water for cleaning; or sequentially putting the substrate into an acetone organic solution, an isopropanol organic solution, deionized water, a hydrofluoric acid solution and deionized water for cleaning.
According to the embodiment of the present disclosure, the average pore diameter of the AlN thin film is 10 to 500 nm.
Drawings
The above and other objects, features and advantages of the present disclosure will become more apparent from the following description of embodiments of the present disclosure with reference to the accompanying drawings, in which:
fig. 1 schematically shows a flow chart of a method for fabricating an AlGaN thin film according to an embodiment of the present disclosure;
fig. 2 schematically illustrates an epitaxial structure of an AlGaN thin film according to an embodiment of the present disclosure;
fig. 3 schematically illustrates an epitaxial structure of an AlGaN thin film according to another embodiment of the present disclosure;
FIG. 4 schematically shows a scanning electron micrograph of a porous AlN thin film of an embodiment of the present disclosure;
fig. 5 schematically shows a flow chart of a method for fabricating an AlGaN thin film according to another embodiment of the present disclosure;
fig. 6 schematically shows a flowchart of a method for preparing an AlGaN thin film according to still another embodiment of the present disclosure.
Detailed Description
For the purpose of promoting a better understanding of the objects, aspects and advantages of the present disclosure, reference is made to the following detailed description taken in conjunction with the accompanying drawings. It is to be understood that the described embodiments are only a few, and not all, of the disclosed embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments disclosed herein without making any creative effort, shall fall within the protection scope of the present disclosure.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure. The terms "comprises," "comprising," and the like, as used herein, specify the presence of stated features, steps, operations, and/or components, but do not preclude the presence or addition of one or more other features, steps, operations, or components.
In the present disclosure, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integral; can be mechanically connected, electrically connected or can communicate with each other; either directly or indirectly through intervening media, either internally or in any other suitable relationship. The specific meaning of the above terms in the present disclosure can be understood by those of ordinary skill in the art as appropriate.
In the description of the present disclosure, it is to be understood that the terms "longitudinal," "length," "circumferential," "front," "rear," "left," "right," "top," "bottom," "inner," "outer," and the like are used in the orientation or positional relationship indicated in the drawings for convenience in describing the present disclosure and for simplicity in description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed in a particular orientation, and be operated in a particular manner, and therefore should not be construed as limiting the present disclosure.
Throughout the drawings, like elements are represented by like or similar reference numerals. Conventional structures or constructions will be omitted when they may obscure the understanding of the present disclosure. And the shapes, sizes and positional relationships of the components in the drawings do not reflect the actual sizes, proportions and actual positional relationships. Furthermore, in the claims, any reference signs placed between parentheses shall not be construed as limiting the claim.
Similarly, in the above description of exemplary embodiments of the disclosure, various features of the disclosure are sometimes grouped together in a single embodiment, figure, or description thereof for the purpose of streamlining the disclosure and aiding in the understanding of one or more of the various disclosed aspects. Reference to the description of the terms "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the disclosure. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present disclosure, "a plurality" means at least two, e.g., two, three, etc., unless explicitly specifically limited otherwise.
Fig. 1 schematically shows a flowchart of a method for preparing an AlGaN thin film according to an embodiment of the present disclosure.
As shown in fig. 1, the method may include, for example, operations S101 to S103.
In operation S101, the substrate is heat-treated to transform the growth surface of the substrate into an island-like relief structure.
In an embodiment of the present disclosure, the substrate may be placed in a gas atmosphere, heated to a predetermined temperature range and maintained for a predetermined period of time to achieve the thermal treatment, wherein the gas atmosphere may comprise pure H2 atmosphere or H2/NH3The preset temperature range of the mixed gas atmosphere can be 800-1500 ℃, and the preset time period range can be 30s-60 min. One specific embodiment may be as follows: the substrate may be heat treated using a Metal Organic Chemical Vapor Deposition (MOCVD) technique. Specifically, the chamber pressure in the MOCVD equipment is set to a preset pressure, for example, 50 Torr. Introducing H with the flow rate of 5000sccm2Heating the substrate to 800-1500 deg.c for 30s-60min, and heat treating the substrate. After the heat treatment, the appearance of the growth surface of the substrate is changed, and the surface with the island-shaped fluctuation is changed from a remarkable atomic step flow surface, so that the island-shaped fluctuation surface is beneficial to the next step of forming the porous AlN thin film.
In an embodiment of the present disclosure, in order to better ensure the quality of the prepared AlGaN thin film, the substrate is preferably a silicon carbide substrate (4H-SiC), and the corresponding growth surface is preferably a silicon surface.
In operation S102, a porous AlN thin film is grown on the growth surface.
In an embodiment of the present disclosure, a one-step method may be used to grow a porous AlN film on the growth surface.
Specifically, growing a porous AlN film on a growth surface using a one-step method may include, for example: the chamber pressure in the MOCVD tool is set to a preset pressure, for example, 50 Torr. And introducing an Al source and an N source into a chamber in the MOCVD equipment, and setting the growth temperature to 900-1300 ℃ to grow the porous AlN thin film. The porous AlN thin film may have a thickness of, for example, 100-500nm and an average pore diameter of 10-500 nm. Among them, TMAl and NH may be used3As an Al source and an N source, respectively.
In another embodiment of the present disclosure, a two-step method may be used to grow a porous AlN film on the growth surface.
Specifically, growing a porous AlN film on a growth surface using a two-step method may include, for example: the chamber pressure in the MOCVD tool is set to a preset pressure, for example, 50 Torr. And introducing an Al source and an N source into a chamber in the MOCVD equipment, firstly setting the growth temperature to 600-1100 ℃ to grow the AlN nucleating layer, and then raising the growth temperature to 1000-1350 ℃ to grow the AlN high-temperature layer on the AlN nucleating layer, wherein the surface of the AlN high-temperature layer is of a porous structure. The AlN nucleation layer may have a thickness of, for example, 5 to 200nm, the AlN high-temperature layer may have a thickness of, for example, 100 to 2000nm, and the porous structure of the surface of the AlN high-temperature layer may have an average pore diameter of 10 to 500 nm.
According to the embodiment of the present disclosure, the heat treatment time, the heat treatment temperature, the pressure, H2 or H2/NH can be adjusted3The molar ratio of Al to N, and the like, so as to flexibly regulate and control the pore size and the density of the porous AlN thin film.
In operation S103, a surface-merged AlGaN thin film is grown on the porous AlN thin film.
In the embodiment of the disclosure, the chamber pressure in the MOCVD apparatus may be kept at a preset pressure, for example, 50Torr, the Al source, the Ga source and the N source are introduced, and the growth temperature is set to 1000-. Here, the surface merge may mean that the surface of the AlGaN thin film has no void and is continuous. The aperture of the porous structure of the porous AlN film is not higher than 500nm, and the size of the porous AlN film is small, so that the AlGaN film on the porous AlN film is short in transverse combination length, the component segregation phenomenon is not obvious, and the whole components are uniformly distributed. The epitaxial structure of the prepared AlGaN thin film is shown in fig. 2 and 3, wherein fig. 2 schematically shows a schematic view of the epitaxial structure of the AlGaN thin film according to an embodiment of the present disclosure, in which the porous AlN thin film epitaxial layer is prepared by a one-step method, and fig. 3 schematically shows a schematic view of the epitaxial structure of the AlGaN thin film according to another embodiment of the present disclosure, in which the porous AlN thin film epitaxial layer is prepared by a two-step method. Fig. 4 schematically shows a scanning electron micrograph of the porous AlN thin film according to an embodiment of the present disclosure, and as can be seen from fig. 2 to 4, the pore distribution of the porous AlN thin film is uniform.
According to the embodiment of the disclosure, the substrate is subjected to heat treatment by setting reasonable heat treatment conditions, so that the appearance of the growth surface of the substrate is changed from a remarkable atomic step flow surface into an island-shaped fluctuated surface, and the porous AlN thin film with adjustable aperture and porosity can be well formed on the basis of the island-shaped fluctuated surface, so that when the AlGaN thin film is prepared on the porous AlN thin film, partial dislocation of the AlGaN thin film is bent to reduce the dislocation density, meanwhile, the stress in the AlGaN layer is fully released by controlling the aperture size and the porosity of the porous AlN thin film and the merging speed of the AlGaN layer, the merging thickness of subsequent AlGaN layers is reduced, the AlGaN component is prevented from being remarkably and unevenly distributed, and the high-quality AlGaN thin film is finally obtained. In addition, the preparation process is simple and controllable, the repeatability is good, the porous AlN epitaxial template grows in situ, pollution caused by taking out a sample wafer in the growth process is avoided, the manufacturing period is shortened, and the cost is reduced.
Fig. 5 schematically shows a flowchart of a method for preparing an AlGaN thin film according to another embodiment of the present disclosure.
As shown in fig. 5, the method may further include, for example, operation S501 before the heat treatment of the substrate, in addition to operation S101 to operation S103.
In operation S501, a substrate is cleaned.
In an embodiment of the present disclosure, the substrate may be sequentially placed in a concentrated sulfuric acid/hydrogen peroxide mixed solution, deionized water, a hydrofluoric acid solution, and deionized water to be cleaned, organic contaminants and inorganic metal particles on the surface are removed, and finally, the substrate is dried by a nitrogen gun.
In another embodiment of the present disclosure, the substrate may be sequentially placed in an acetone organic solution, an isopropanol organic solution, deionized water, a hydrofluoric acid solution, and deionized water to be cleaned, to remove organic contaminants and inorganic metal particles on the surface, and finally dried by a nitrogen gun.
According to the embodiment of the disclosure, the substrate is cleaned by selecting a reasonable solvent and a reasonable mode, and organic pollutants and inorganic metal particles on the surface are removed on the basis of not damaging the structure of the substrate, so that the quality of the AlGaN film is further improved.
Fig. 6 schematically shows a flowchart of a method for preparing an AlGaN thin film according to still another embodiment of the present disclosure.
As shown in fig. 6, the method may further include operation S601, for example, before growing the surface-merged AlGaN thin film on the porous AlN thin film, in addition to operation S501, operation S101 to operation S103.
In operation S601, an insertion layer is grown on the porous AlN film.
In one embodiment of the present disclosure, an insertion layer is grown on the porous AlN film, and then an AlGaN film is grown on the insertion layer. Wherein, the insertion layer comprises a component gradual change structure or AlxGal-xN/AlyGal-yN superlattice or an intermediate component layer or an intermediate temperature layer, x is more than or equal to 0, y is less than or equal to 1, and x is not equal to y.
According to the embodiment of the disclosure, the existence of the insertion layer can further relieve the stress borne by the AlGaN film, and further improve the quality of the AlGaN film.
The above-mentioned embodiments are intended to illustrate the objects, aspects and advantages of the present disclosure in further detail, and it should be understood that the above-mentioned embodiments are only illustrative of the present disclosure and are not intended to limit the present disclosure, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present disclosure should be included in the scope of the present disclosure.

Claims (9)

1. A preparation method of the AlGaN film comprises the following steps:
carrying out heat treatment on the substrate to enable the growth surface of the substrate to be converted into an island-shaped fluctuation structure;
growing a porous AlN thin film on the growth surface;
and growing an AlGaN film with a combined surface on the porous AlN film.
2. The method of manufacturing an AlGaN thin film according to claim 1, wherein the heat treatment of the substrate includes:
placing the substrate in a gas atmosphere, heating to a preset temperature range and preserving heat for a preset time period,wherein the gas atmosphere comprises pure H2Atmosphere or H2/NH3And (3) mixing the gas atmosphere, wherein the preset temperature range is 800-1500 ℃, and the preset time period range is 30s-60 min.
3. The method of producing an AlGaN thin film according to claim 1, wherein the growing a porous AlN thin film on the growth surface includes:
and growing a porous AlN thin film on the growth surface by adopting a one-step method or a two-step method.
4. The method of claim 3, wherein the growing a porous AlN thin film on the growth surface using a one-step method comprises:
and introducing an Al source and an N source, and setting the growth temperature to 900-1300 ℃ to grow the porous AlN thin film.
5. The method of claim 3, wherein the growing a porous AlN thin film on the growth surface in a two-step method comprises:
introducing an Al source and an N source, and setting the growth temperature to 600-1100 ℃ to grow the AlN nucleating layer;
and raising the temperature to 1000-1350 ℃ to grow an AlN high-temperature layer on the AlN nucleating layer, wherein the surface of the AlN high-temperature layer is of a porous structure.
6. The method of producing an AlGaN thin film according to claim 1, wherein the growing a surface-merged AlGaN thin film on the porous AlN film includes:
and introducing an Al source, a Ga source and an N source, and setting the growth temperature to 1000-1150 ℃ to grow the AlGaN film.
7. The method according to claim 1, wherein the substrate is a silicon carbide substrate, and the growth surface is a silicon surface.
8. The method of producing an AlGaN film according to claim 1, further comprising, before growing a surface-merged AlGaN film on the porous AlN film:
growing an insertion layer on the porous AlN thin film, and growing the AlGaN thin film on the insertion layer, wherein the insertion layer comprises a composition gradient structure or AlxGal-xN/AlyGa1-yN superlattice or an intermediate composition layer or an intermediate temperature layer, x is more than or equal to 0, y is less than or equal to 1, and x is not equal to y.
9. The method of producing an AlGaN thin film according to claim 1, wherein the AlN thin film has an average pore diameter of 10 to 500 nm.
CN202110715925.4A 2021-06-25 2021-06-25 Preparation method of AlGaN film Pending CN113437186A (en)

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