CN116190507A - Patterned substrate based on composite material film, preparation method and LED epitaxial wafer - Google Patents

Patterned substrate based on composite material film, preparation method and LED epitaxial wafer Download PDF

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Publication number
CN116190507A
CN116190507A CN202310175665.5A CN202310175665A CN116190507A CN 116190507 A CN116190507 A CN 116190507A CN 202310175665 A CN202310175665 A CN 202310175665A CN 116190507 A CN116190507 A CN 116190507A
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gas
oxide layer
inorganic oxide
inorganic
layer
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曾广艺
王子荣
卢建航
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Guangdong Zhongtu Semiconductor Technology Co ltd
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Guangdong Zhongtu Semiconductor Technology Co ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/401—Oxides containing silicon
    • C23C16/402—Silicon dioxide
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/56—After-treatment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
    • H01L33/20—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a particular shape, e.g. curved or truncated substrate
    • H01L33/22—Roughened surfaces, e.g. at the interface between epitaxial layers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The embodiment of the invention discloses a patterned substrate based on a composite material film layer, a preparation method and an LED epitaxial wafer, wherein the preparation method of the patterned substrate based on the composite material film layer comprises the following steps: providing a flat sapphire substrate; forming a first inorganic oxide layer on the flat sapphire substrate through a first plasma enhanced chemical vapor deposition process; and forming a second inorganic oxide layer on the first inorganic oxide layer through a second plasma enhanced chemical vapor deposition process, wherein the oxygen content of the second inorganic oxide layer is smaller than that of the first inorganic oxide layer. By using the method, the adhesiveness of the second inorganic oxide layer to the photoresist is improved, so that the photoresist uniformity yield of the photoresist film layer is improved, the steps of surface modification and tackifying treatment of the film layer are reduced, the time limit in the photoresist uniformity process is reduced, the degumming defect of the patterned substrate is avoided, the preparation efficiency of the patterned substrate is improved, and the production cost of the patterned substrate is reduced.

Description

Patterned substrate based on composite material film, preparation method and LED epitaxial wafer
Technical Field
The embodiment of the invention relates to the technical field of semiconductor manufacturing, in particular to a patterned substrate based on a composite material film layer, a preparation method and an LED epitaxial wafer.
Background
Pursuing higher light extraction efficiency is an important direction of substrate material research, and one of the main principles of the composite substrate capable of improving light extraction efficiency is to introduce a heterogeneous material with a low refractive index, and the low refractive index film material can form a larger total reflection angle critical value at a material interface in LED light extraction, which is beneficial to total emission and emission extraction of light in an LED device. Among them, oxygen content is a main factor affecting the refractive index of the hetero material, and also a main factor affecting the adhesion between the hetero material and the photoresist.
Low refractive index requires low oxygen content, which means that the adhesion of the material surface is also low, so in the spin coating process after obtaining the low refractive index film layer, people often need to perform surface modification and adhesion promotion treatment of the film layer, and the film layer is limited by timeliness, and the film layer will fail after being placed too long after the surface modification and adhesion promotion treatment, and the uncertainty and the cost of corresponding steps are increased.
Disclosure of Invention
The embodiment of the invention provides a patterned substrate based on a composite material film, a preparation method and an LED epitaxial wafer, which are used for improving the spin coating yield of the film, reducing the steps of surface modification and tackifying treatment of the film and avoiding the degumming defect of the patterned substrate.
In a first aspect, an embodiment of the present invention provides a method for preparing a patterned substrate based on a composite film layer, including:
providing a flat sapphire substrate;
forming a first inorganic oxide layer on the flat piece sapphire substrate through a first plasma enhanced chemical vapor deposition process;
and forming a second inorganic oxide layer on the first inorganic oxide layer through a second plasma enhanced chemical vapor deposition process, wherein the oxygen content of the second inorganic oxide layer is smaller than that of the first inorganic oxide layer.
Optionally, forming a first inorganic oxide layer on the flat piece sapphire substrate by a first plasma enhanced chemical vapor deposition process, comprising:
performing chemical vapor deposition by adopting inorganic gas and oxide gas according to a first flow ratio to obtain the first inorganic oxide layer, wherein the inorganic gas is gas containing inorganic chemical components of the first inorganic oxide layer, and the oxide gas is gas containing oxygen element chemical components;
forming a second inorganic oxide layer on the first inorganic oxide by a second plasma enhanced chemical vapor deposition process, comprising:
and performing chemical vapor deposition by adopting the inorganic gas and the oxide gas in a second flow ratio to obtain the second inorganic oxide layer, wherein the first flow ratio and the second flow ratio are proportional relations between the flow of the inorganic gas and the flow of the oxide gas, and the first flow ratio is smaller than the second flow ratio.
Optionally, performing chemical vapor deposition with an inorganic gas and an oxide gas at a first flow ratio to obtain the first inorganic oxide layer, and further including:
depositing the first inorganic oxide layer in nitrogen gas using the nitrogen gas as a carrier gas;
and performing chemical vapor deposition by adopting the inorganic gas and the oxide gas in a second flow ratio to obtain the second inorganic oxide layer, and further comprising:
the second inorganic oxide layer is deposited in the nitrogen gas using the nitrogen gas as a carrier gas.
Optionally, depositing the second inorganic oxide layer in the nitrogen gas using the nitrogen gas as a carrier gas, further comprising:
there is a multiple relationship A between the gas amount of the nitrogen gas and the total gas amount of the inorganic gas and the oxide gas, wherein A < 1.5 < 3.
Optionally, the first inorganic oxide layer comprises a first silicon dioxide layer, the second inorganic oxide layer comprises a second silicon dioxide layer, the inorganic gas comprises silane, and the oxide gas comprises laughing gas;
performing chemical vapor deposition by using an inorganic gas and an oxide gas at a first flow ratio to obtain the first inorganic oxide layer, including:
carrying out chemical vapor deposition by adopting the silane and the laughing gas to obtain the first silicon dioxide layer, wherein the flow ratio of the silane to the laughing gas is 1:40;
performing chemical vapor deposition with the inorganic gas and the oxide gas at a second flow ratio to obtain the second inorganic oxide layer, including:
and carrying out chemical vapor deposition by adopting the silane and the laughing gas to obtain the second silicon dioxide layer, wherein the flow ratio of the silane to the laughing gas is 9:10.
Optionally, the deposition thickness of the first inorganic oxide layer ranges from 1.0um to 2.4um, and the deposition thickness of the second inorganic oxide layer ranges from 50nm to 180nm.
Optionally, the method further comprises: and coating photoresist on the second inorganic oxide layer through a photoresist homogenizing process to form a photoresist layer.
Optionally, after coating a photoresist on the second inorganic oxide layer by a photoresist uniformizing process, forming a photoresist layer, the method further includes:
forming a pattern structure on the photoresist layer through exposure and development;
transferring the graphic structure to the second inorganic oxide layer and the first inorganic oxide layer;
and removing the second inorganic oxide layer through an over-etching process to obtain a patterned substrate based on the composite material film layer, wherein the patterned substrate is formed with the pattern structure, and the pattern structure is prepared from the first inorganic oxide layer.
In a second aspect, an embodiment of the present invention further provides a patterned substrate based on a composite film, which is prepared by using the method for preparing a patterned substrate based on a composite film according to any one of the first aspect.
In a third aspect, an embodiment of the present invention further provides an LED epitaxial wafer, including the patterned substrate based on the composite film layer according to any one of the second aspects.
The embodiment of the invention provides a patterned substrate based on a composite material film layer, a preparation method and an LED epitaxial wafer, wherein the preparation method of the patterned substrate based on the composite material film layer comprises the following steps: providing a flat sapphire substrate; forming a first inorganic oxide layer on the flat sapphire substrate through a first plasma enhanced chemical vapor deposition process; and forming a second inorganic oxide layer on the first inorganic oxide layer through a second plasma enhanced chemical vapor deposition process, wherein the oxygen content of the second inorganic oxide layer is smaller than that of the first inorganic oxide layer. By using the method, the oxygen content of the second inorganic oxide layer is smaller than that of the first inorganic oxide layer, so that the adhesiveness of the second inorganic oxide layer to photoresist is improved, the photoresist homogenizing yield of the photoresist film layer is improved, the steps of surface modification and tackifying treatment of the film layer are reduced, the limitation of time limitation in the photoresist homogenizing process is reduced, the degumming defect of the patterned substrate is avoided, the preparation efficiency of the patterned substrate is improved, and the production cost of the patterned substrate is reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of a method for preparing a patterned substrate based on a composite material film layer according to an embodiment of the present invention;
FIG. 2 is a structural flow diagram of a method of fabricating the patterned substrate based on the composite film layer shown in FIG. 1;
FIG. 3 is a schematic flow chart of another method for preparing a patterned substrate based on a composite film layer according to an embodiment of the present invention;
FIG. 4 is a schematic flow chart of another method for preparing a patterned substrate based on a composite film layer according to an embodiment of the present invention;
FIG. 5 is a schematic flow chart of another method for preparing a patterned substrate based on a composite film layer according to an embodiment of the present invention;
FIG. 6 is a structural flow diagram of a method of fabricating the patterned substrate based on the composite film layer shown in FIG. 5;
FIG. 7 is a graphical substrate based on a composite film layer provided by an embodiment of the present invention;
fig. 8 is a schematic structural diagram of an LED epitaxial wafer according to an embodiment of the present invention.
Detailed Description
The invention is described in further detail below with reference to the drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting thereof. It should be further noted that, for convenience of description, only some, but not all of the structures related to the present invention are shown in the drawings.
The terminology used in the embodiments of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. It should be noted that, the terms "upper", "lower", "left", "right", and the like in the embodiments of the present invention are described in terms of the angles shown in the drawings, and should not be construed as limiting the embodiments of the present invention. In addition, in the context, it will also be understood that when an element is referred to as being formed "on" or "under" another element, it can be directly formed "on" or "under" the other element or be indirectly formed "on" or "under" the other element through intervening elements. The terms "first," "second," and the like, are used for descriptive purposes only and not for any order, quantity, or importance, but rather are used to distinguish between different components. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
The term "comprising" and variants thereof as used herein is intended to be open ended, i.e., including, but not limited to. The term "based on" is based at least in part on. The term "one embodiment" means "at least one embodiment".
It should be noted that the terms "first," "second," and the like herein are merely used for distinguishing between corresponding contents and not for defining a sequential or interdependent relationship.
It should be noted that references to "one", "a plurality" and "a plurality" in this disclosure are intended to be illustrative rather than limiting, and those skilled in the art will appreciate that "one or more" is intended to be construed as "one or more" unless the context clearly indicates otherwise.
Fig. 1 is a flow chart of a method for preparing a patterned substrate based on a composite material film layer according to an embodiment of the present invention, and fig. 2 is a structural flow chart of the method for preparing a patterned substrate based on a composite material film layer shown in fig. 1, and as shown in fig. 1 and fig. 2, the method for preparing a patterned substrate based on a composite material film layer includes:
s110, providing a flat sapphire substrate.
Specifically, referring to fig. 2 a), the flat sapphire substrate 10 is a substrate having a flat surface, which is smoothly polished, that is, the flat sapphire substrate 10 has a C-plane of good quality, which can contribute to nucleation and growth of epitaxial crystals into an epitaxial layer. In addition, before the epitaxial layer or the hetero layer is subsequently grown, the flat piece sapphire substrate 10 is further required to be subjected to a cleaning and drying pretreatment, and for example, the flat piece sapphire substrate 10 may be subjected to a wet cleaning in an SPM solution (a mixed solution of sulfuric acid and hydrogen peroxide in a ratio of 6:1) at 90 ℃ to 150 ℃ for 20 minutes, and the flat piece sapphire substrate 10 is rinsed with deionized water, and finally the flat piece sapphire substrate 10 is rotated to be subjected to a drying treatment.
S120, forming a first inorganic oxide layer on the flat piece sapphire substrate through a first plasma enhanced chemical vapor deposition process.
Specifically, referring to fig. 2 b), the first inorganic oxide layer 20 is a film layer made of an inorganic oxide material that is substantially opposite to the flat sapphire substrate 10 and an epitaxial layer material such as gallium nitride, i.e., a material different from the flat sapphire substrate 10 and the epitaxial material, and may be, for example, silicon dioxide (SiO 2 ) Indium Tin Oxide (ITO), tin oxide (Sn O) 2 ) And silver oxide (AgO), and the like.
S130, forming a second inorganic oxide layer on the first inorganic oxide layer through a second plasma enhanced chemical vapor deposition process, wherein the oxygen content of the second inorganic oxide layer is smaller than that of the first inorganic oxide layer.
Specifically, referring to fig. 2 c), the second inorganic oxide layer 30 is a film layer made of an inorganic oxide material substantially opposite to the flat sapphire substrate 10 and the epitaxial layer material such as gallium nitride, i.e., different from the flat sapphire substrate 10 and the epitaxial material, and may be silicon dioxide (SiO 2 ) Indium Tin Oxide (ITO), tin oxide (Sn O) 2 ) And silver oxide (AgO), and the like. It should be noted that, the inorganic oxide materials used in the first inorganic oxide layer 20 and the second inorganic oxide layer 30 may be the same or different, but the oxygen content of the second inorganic oxide layer 30 is smaller than that of the first inorganic oxide layer 20, which can effectively regulate the polarity of the surface of the whole film layer, so that the surface property of the hydrophilic first inorganic oxide layer 20 is converted into the surface property of the hydrophobic second inorganic oxide layer 30, the adhesion property of the second inorganic oxide layer 30 is higher than that of the first inorganic oxide layer 20, and the surface property of the whole formed flat sapphire substrate 10, the first inorganic oxide layer 20 and the second inorganic oxide layer 30 is hydrophobic, so that the whole adhesion property is stronger, and convenience is provided for the subsequent step of coating the photoresist layer.
According to the technical scheme, a flat sapphire substrate is provided; then forming a first inorganic oxide layer on the flat sapphire substrate through a first plasma enhanced chemical vapor deposition process; and finally, forming a second inorganic oxide layer on the first inorganic oxide layer through a second plasma enhanced chemical vapor deposition process, wherein the oxygen content of the second inorganic oxide layer is smaller than that of the first inorganic oxide layer. By using the method, the oxygen content of the second inorganic oxide layer is smaller than that of the first inorganic oxide layer, so that the adhesiveness of the second inorganic oxide layer to photoresist is improved, the photoresist homogenizing yield of the photoresist film layer is improved, the steps of surface modification and tackifying treatment of the film layer are reduced, the limitation of time limitation in the photoresist homogenizing process is reduced, the degumming defect of the patterned substrate is avoided, the preparation efficiency of the patterned substrate is improved, and the production cost of the patterned substrate is reduced.
Fig. 3 is a schematic flow chart of another method for preparing a patterned substrate based on a composite film layer according to an embodiment of the present invention, where the method is optimized based on the foregoing embodiment. Optionally, forming a first inorganic oxide layer on the flat piece sapphire substrate by a first plasma enhanced chemical vapor deposition process, comprising:
performing chemical vapor deposition by adopting inorganic gas and oxide gas according to a first flow ratio to obtain a first inorganic oxide layer, wherein the inorganic gas is gas containing inorganic chemical components of the first inorganic oxide layer, and the oxide gas is gas containing oxygen element chemical components;
forming a second inorganic oxide layer on the first inorganic oxide by a second plasma enhanced chemical vapor deposition process, comprising:
and performing chemical vapor deposition by adopting inorganic gas and oxide gas at a second flow rate ratio to obtain a second inorganic oxide layer, wherein the first flow rate ratio and the second flow rate ratio are proportional relations between the flow rate of the inorganic gas and the flow rate of the oxide gas, and the first flow rate ratio is smaller than the second flow rate ratio.
For details not yet described in this embodiment, refer to the above embodiment, as shown in fig. 3, the method for preparing a patterned substrate based on a composite film layer includes:
s210, providing a flat sapphire substrate.
S220, performing chemical vapor deposition by adopting inorganic gas and oxide gas according to a first flow ratio to obtain a first inorganic oxide layer, wherein the inorganic gas is gas containing inorganic chemical components of the first inorganic oxide layer, and the oxide gas is gas containing oxygen chemical components.
Specifically, with continued reference to fig. 2 b), chemical vapor deposition may be performed using an inorganic gas and an oxide gas through a first plasma enhanced chemical vapor deposition process, a first inorganic oxide layer 20 may be formed on the flat sheet sapphire substrate 10, and the amount of oxygen content of the formed first inorganic oxide layer 20 may be varied by controlling a first flow ratio between the inorganic gas and the oxide gas.
Optionally, with continued reference to fig. 2 b), chemical vapor deposition is performed using an inorganic gas and an oxide gas at a first flow ratio to obtain a first inorganic oxide layer 20, and further comprising: the first inorganic oxide layer 20 is deposited in nitrogen using nitrogen as a carrier gas. Specifically, nitrogen can be used as carrier gas, or high-purity nitrogen can be used as carrier gas, the high-purity nitrogen has high purity, extremely low water content and oxygen content, high reliability and is colorless and odorless inert gas at normal temperature and normal pressure. The first inorganic oxide layer 20 is deposited in nitrogen, so that the film surface of the first inorganic oxide layer 20 obtained by performing chemical vapor deposition on the inorganic gas and the oxide gas is more uniform, and the adhesiveness of the first inorganic oxide layer 20 can be changed to a certain extent by the nitrogen. Alternatively, the first inorganic oxide layer 20 may be deposited to a thickness in the range of 1.0um to 2.4um.
S230, performing chemical vapor deposition by adopting inorganic gas and oxide gas at a second flow rate ratio to obtain a second inorganic oxide layer, wherein the first flow rate ratio and the second flow rate ratio are both proportional relations of the flow rate of the inorganic gas and the flow rate of the oxide gas, and the first flow rate ratio is smaller than the second flow rate ratio.
Specifically, with continued reference to fig. 2 c), chemical vapor deposition may be performed using an inorganic gas and an oxide gas through a second plasma enhanced chemical vapor deposition process, a second inorganic oxide layer 30 may be formed on the first inorganic oxide layer 20, and the amount of oxygen content of the formed second inorganic oxide layer 30 may be changed by controlling a second flow ratio between the inorganic gas and the oxide gas. It should be noted that, if the first flow ratio is smaller than the second flow ratio, the proportion of the oxide gas in the deposition process is from large to small, so that the oxygen content of the second inorganic oxide layer 30 obtained by deposition is smaller than that of the first inorganic oxide layer 20.
Optionally, with continued reference to fig. 2 c), chemical vapor deposition is performed using an inorganic gas and an oxide gas at a second flow ratio to obtain a second inorganic oxide layer 30, further comprising: the second inorganic oxide layer 30 is deposited in nitrogen using nitrogen as a carrier gas. Further, the second inorganic oxide layer 30 is deposited in nitrogen using nitrogen as a carrier gas, further comprising: there is a multiple relation A between the gas amount of nitrogen and the total gas amount of inorganic gas and oxide gas, wherein A is more than 1.5 and less than 3. Specifically, nitrogen can be used as carrier gas, or high-purity nitrogen can be used as carrier gas, the high-purity nitrogen has high purity, extremely low water content and oxygen content, high reliability and is colorless and odorless inert gas at normal temperature and normal pressure. The second inorganic oxide layer 30 is deposited in nitrogen, so that the film surface of the second inorganic oxide layer 30 obtained by performing chemical vapor deposition on the inorganic gas and the oxide gas is more uniform, and the adhesiveness of the second inorganic oxide layer 30 can be changed by nitrogen to a certain extent. In addition, the adhesion of the film surface is affected by both the oxygen content of the film and the nature of the nitrogen. In order to ensure that the oxygen content is in a lower range (the oxygen content of the second inorganic oxide layer 30 is smaller than that of the first inorganic oxide layer 20) and that the adhesion performance of the film surface of the second inorganic oxide layer 30 is higher (the adhesion of the second inorganic oxide layer 30 is greater than that of the first inorganic oxide layer 20) during the deposition of the second inorganic oxide layer 30, the gas amount of nitrogen should be greater than the total gas amount of inorganic gas and oxide gas, and a multiple relationship a exists between the gas amount of nitrogen and the total gas amount of inorganic gas and oxide gas, wherein 1.5 < a < 3, and the gas amount of nitrogen may be 2 times the total gas amount of inorganic gas and oxide gas, for example. Alternatively, the deposition thickness of the second inorganic oxide layer 30 may range from 50nm to 180nm, and the deposition thickness of the second inorganic oxide layer 30 is smaller than the deposition thickness of the first inorganic oxide layer 20.
According to the technical scheme provided by the embodiment of the invention, the oxygen content in the first inorganic oxide layer and the second inorganic oxide layer obtained by deposition can be effectively regulated and controlled by changing the flow ratio of the inorganic gas to the oxide gas in the chemical vapor deposition process, so that the purpose of regulating and controlling the film surface adhesion of the first inorganic oxide layer and the second inorganic oxide layer is achieved, the adhesion of the integral film layer is improved, the phenomenon of abnormal degumming of the integral film layer is avoided, and the spin-coating yield is improved.
In a specific embodiment, fig. 4 is a schematic flow chart of another method for preparing a patterned substrate based on a composite film according to an embodiment of the present invention, where the method is optimized based on the foregoing embodiment. Optionally, the first inorganic oxide layer comprises a first silicon dioxide layer, the second inorganic oxide layer comprises a second silicon dioxide layer, the inorganic gas comprises silane, and the oxide gas comprises laughing gas;
performing chemical vapor deposition by using inorganic gas and oxide gas at a first flow ratio to obtain a first inorganic oxide layer, including:
carrying out chemical vapor deposition by adopting silane and laughing gas to obtain a first silicon dioxide layer, wherein the flow ratio of the silane to the laughing gas is 1:40;
performing chemical vapor deposition with an inorganic gas and an oxide gas at a second flow ratio to obtain a second inorganic oxide layer, comprising:
and carrying out chemical vapor deposition by adopting silane and laughing gas to obtain a second silicon dioxide layer, wherein the flow ratio of the silane to the laughing gas is 9:10.
For details not yet described in this embodiment, refer to the above embodiment, as shown in fig. 4, the method for preparing a patterned substrate based on a composite film layer includes:
s310, providing a flat sapphire substrate.
S320, performing chemical vapor deposition by using silane and laughing gas to obtain a first silicon dioxide layer, wherein the flow ratio of the silane to the laughing gas is 1:40.
Specifically, with continued reference to fig. 2 b), the first inorganic oxide layer 20 may be a first silicon dioxide layer 21 and the inorganic gas may be Silane (SiH) 4 ) The oxide gas may be laughing gas (N) 2 O). By the first plasma enhanced chemical vapor deposition process, chemical vapor deposition may be performed using silane and laughing gas, and nitrogen gas is used as a carrier gas, to form the first silicon dioxide layer 21 on the flat sapphire substrate 10, and illustratively, the flow ratio of silane and laughing gas may be 1:40, and 1:40 is a first flow ratio, which may effectively regulate and control the oxygen content of the first silicon dioxide layer 21. In addition, during the deposition of the first silicon dioxide layer 21, it specifically includes: the flat sapphire substrate 10 is placed on an aluminum stage of a chamber of a plasma enhanced chemical vapor deposition process, the temperature of the aluminum stage is set to 180-280 ℃, the pressure of the chamber is pumped to 160-80pa, and the first silicon dioxide layer 21 is deposited in an atmosphere of nitrogen, silane and laughing gas, and the deposition thickness of the first silicon dioxide layer 21 may be 2.1um, for example.
S330, performing chemical vapor deposition by adopting silane and laughing gas to obtain a second silicon dioxide layer, wherein the flow ratio of the silane to the laughing gas is 9:10.
Specifically, with continued reference to fig. 2 c), the second inorganic oxide layer 30 may be the second silicon dioxide layer 31, the inorganic gas may be silane, and the oxide gas may be laughing gas. By the second plasma enhanced chemical vapor deposition process, chemical vapor deposition may be performed by using silane and laughing gas, and nitrogen gas is used as a carrier gas, and the second silicon dioxide layer 31 is formed on the first silicon dioxide layer 21, and illustratively, the flow ratio of silane to laughing gas may be 9:10, and 9:10 may be a second flow ratio, which may effectively regulate the oxygen content of the second silicon dioxide layer 31, and the second flow ratio may be greater than the first flow ratio, and the oxygen content of the second silicon dioxide layer 31 may be less than the oxygen content of the first silicon dioxide layer 21. In addition, during the deposition of the second silicon dioxide layer 31, it specifically includes: after the deposition of the first silicon oxide layer 21 is completed, the radio frequency energy is turned off and adjusted to increase the flow ratio of silane and laughing gas, and after the process of stably depositing the second silicon oxide layer 31 for 15 seconds, the radio frequency energy is turned back on to deposit the second silicon oxide layer 31 in an atmosphere of nitrogen, silane and laughing gas, and the gas amount of nitrogen is 2 times the total gas amount of silane and laughing gas, and the deposition thickness of the second silicon oxide layer 31 may be 60nm, for example.
According to the technical scheme provided by the embodiment of the invention, a specific method for respectively depositing the first silicon dioxide layer and the second silicon dioxide layer is provided, so that the oxygen content of the first silicon dioxide layer can be effectively regulated and controlled to be larger than that of the second silicon dioxide layer, the adhesion performance of the surfaces of the finally formed flat sapphire substrate, the integrated film layers of the first silicon dioxide layer and the second silicon dioxide layer is improved, the photoresist uniformity yield of the photoresist film layer is improved, the degumming defect of the patterned substrate is avoided, the preparation efficiency of the patterned substrate is improved, and the production cost of the patterned substrate is reduced.
Fig. 5 is a flow chart of another method for preparing a patterned substrate based on a composite film according to an embodiment of the present invention, and fig. 6 is a structural flow chart of the method for preparing a patterned substrate based on a composite film shown in fig. 5, where the embodiment is optimized based on the foregoing embodiment. Optionally, the method further comprises: and coating photoresist on the second inorganic oxide layer through a photoresist homogenizing process to form a photoresist layer. Further, after coating a photoresist on the second inorganic oxide layer by a photoresist uniformizing process to form a photoresist layer, the method further comprises:
forming a pattern structure on the photoresist layer through exposure and development;
transferring the pattern structure to the second inorganic oxide layer and the first inorganic oxide layer;
and removing the second inorganic oxide layer through an over-etching process to obtain the patterned substrate based on the composite material film layer with the pattern structure, wherein the pattern structure is prepared from the first inorganic oxide layer.
For details not yet described in this embodiment, please refer to the above embodiment, as shown in fig. 6 and fig. 7, the method for preparing a patterned substrate based on a composite film layer includes:
s410, providing a flat piece of sapphire substrate.
S420, forming a first inorganic oxide layer on the flat piece sapphire substrate through a first plasma enhanced chemical vapor deposition process.
S430, forming a second inorganic oxide layer on the first inorganic oxide layer through a second plasma enhanced chemical vapor deposition process, wherein the oxygen content of the second inorganic oxide layer is smaller than that of the first inorganic oxide layer.
S440, coating photoresist on the second inorganic oxide layer through a photoresist homogenizing process to form a photoresist layer.
Specifically, referring to d) of fig. 6, the first inorganic oxide layer 20 and the second inorganic oxide layer 30 are respectively deposited in a nitrogen atmosphere, so that the surfaces of the first inorganic oxide layer 20 and the second inorganic oxide layer 30 may be more uniform and flat, the photoresist layer 40 formed may be more flat and may have a more uniform thickness by coating the photoresist on the flat surface of the second inorganic oxide layer 30 through a photoresist-homogenizing process, and for example, the photoresist layer 40 may be selected as a positive photoresist or a negative photoresist when the photoresist layer 40 is prepared, the photoresist layer 40 may be prepared by a spin-coating or spray-coating process, and the thickness thereof may be set to be 0.3 μm to 5 μm, and for example, the thickness of the photoresist layer 40 may be 2.3 μm. It should be noted that, the adhesion performance of the surface of the second inorganic oxide layer 30 is stronger, after the surface of the formed second inorganic oxide layer 30 is rinsed and spin-dried with deionized water, the photoresist can be directly coated on the surface of the second inorganic oxide layer 30 to obtain a photoresist-homogenizing composite sheet with good adhesion, which lays a foundation for the subsequent preparation of a photoresist column mask pattern, and does not need the steps of baking coating or spin-coating adhesion promoter/modifier, etc., so that the preparation steps of the patterned substrate can be effectively reduced, and the defect of surface degumming of the patterned substrate can be reduced. Moreover, due to the adhesive property of the surface of the second inorganic oxide layer 30, the process of coating the photoresist is not limited by time, and an uncertain factor is added to the process of coating the photoresist and the corresponding step and cost of required materials are increased, compared to the case that the adhesion promoter/modifier in the steps of baking coating or spin coating the adhesion promoter/modifier is failed due to a long standing time.
S450, forming a pattern structure on the photoresist layer through exposure and development.
Specifically, referring to e) of fig. 6, since the surface of the photoresist layer 40 is formed to be smoother and the thickness is more uniform, the pattern structure of the photoresist column mask formed on the photoresist layer 40 by exposing and developing is more accurate, wherein the size of the photoresist column is more in line with the standard, the pattern of the photoresist column mask corresponds to the pattern finally formed on the patterned substrate based on the composite material film layer, and the pattern transfer technology such as photolithography or nanoimprinting can be used to prepare the photoresist column mask. Illustratively, taking a photolithography process as an example, the photoresist layer 40 is exposed through a photoresist column mask, and then the photoresist layer 40 may be patterned by a developing step, i.e., transferring the pattern of the photoresist column mask onto the photoresist layer 40 to form the photoresist column mask.
S460, transferring the pattern structure to the second inorganic oxide layer and the first inorganic oxide layer.
Specifically, referring to f) of fig. 6, according to the process of transferring the pattern by using the photoresist column mask, the second inorganic oxide layer 30 and the first inorganic oxide layer 20 may be respectively etched by using a dry etching process or a wet etching process to complete patterning, and the formed pattern structure includes a part of the material of the first inorganic oxide layer 20 and a part of the material of the second inorganic oxide layer 30.
And S470, removing the second inorganic oxide layer through an over-etching process to obtain the patterned substrate based on the composite material film layer with the pattern structure, wherein the pattern structure is prepared from the first inorganic oxide layer.
Specifically, referring to g) of fig. 6, the first inorganic oxide layer 20 may be optionally deposited to a thickness ranging from 1.0um to 2.4um, and the second inorganic oxide layer 30 may be deposited to a thickness ranging from 50nm to 180nm. The deposition thickness of the first inorganic oxide layer 20 is far greater than that of the second inorganic oxide layer 30, and the second inorganic oxide layer 30 can be removed through an over-etching process, so that only part of the material of the first inorganic oxide layer 20 is included in the finally formed pattern structure, and the finally obtained patterned substrate based on the composite material film layer with the formed pattern structure comprises the flat sapphire substrate 10 and the pattern structure prepared from the part of the material of the first inorganic oxide layer 20. It should be noted that, the finally obtained patterned substrate based on the composite material film layer does not include the second inorganic oxide layer 30, and the deposition and removal processes of the second inorganic oxide layer 30 do not affect the optical properties, the electrical properties, and the like of the finally obtained patterned substrate based on the composite material film layer, and the first inorganic oxide layer 20 has the property of low refractive index, for example, the finally obtained patterned substrate based on the composite material film layer still has the property of low refractive index.
According to the technical scheme, the photoresist is coated on the surface of the second inorganic oxide layer, and the patterned substrate with the pattern structure based on the composite material film layer is finally obtained, so that the transfer of the pattern structure is realized, the property of the patterned substrate is not affected, the preparation steps of baking coating or spin coating of the tackifier/modifier and the like of the patterned substrate are effectively reduced, the defect of surface degumming of the patterned substrate is reduced, the time limitation of the photoresist coating process is avoided, and meanwhile, the occurrence of uncertain factors in the preparation process, the corresponding steps and the cost of required materials are also reduced.
Fig. 7 is a schematic diagram of a patterned substrate based on a composite film layer according to an embodiment of the present invention, where, as shown in fig. 7, the patterned substrate based on a composite film layer is prepared by using a method for preparing a patterned substrate based on a composite film layer according to any one of the embodiments of the present invention.
Based on the same inventive concept, the embodiment of the invention also provides an LED epitaxial wafer. Fig. 8 is a schematic structural diagram of an LED epitaxial wafer according to an embodiment of the present invention, and as shown in fig. 8, the LED epitaxial wafer includes a patterned substrate 1 based on a composite film layer according to any one of the foregoing embodiments, and further includes an epitaxial layer 2 formed on the patterned substrate 1 based on the composite film layer.
For forming epitaxial layers on patterned substrates of different materials, different LED epitaxial wafer growth techniques are required, and for the patterned substrate based on the composite material film layer provided by the embodiment of the invention, the epitaxial layer 2 in the LED epitaxial wafer can be GaN, alGaN epitaxial layers and the like. The patterned substrate 1 based on the composite material film layer provided by the embodiment of the LED epitaxial wafer has the same or similar beneficial effects as the patterned substrate 1 based on the composite material film layer, and will not be described herein.
Note that the above is only a preferred embodiment of the present invention and the technical principle applied. It will be understood by those skilled in the art that the present invention is not limited to the particular embodiments described herein, and that various obvious changes, rearrangements, combinations, and substitutions can be made by those skilled in the art without departing from the scope of the invention. Therefore, while the invention has been described in connection with the above embodiments, the invention is not limited to the embodiments, but may be embodied in many other equivalent forms without departing from the spirit or scope of the invention, which is set forth in the following claims.

Claims (10)

1. The preparation method of the patterned substrate based on the composite material film layer is characterized by comprising the following steps of:
providing a flat sapphire substrate;
forming a first inorganic oxide layer on the flat piece sapphire substrate through a first plasma enhanced chemical vapor deposition process;
and forming a second inorganic oxide layer on the first inorganic oxide layer through a second plasma enhanced chemical vapor deposition process, wherein the oxygen content of the second inorganic oxide layer is smaller than that of the first inorganic oxide layer.
2. The method of claim 1, wherein forming a first inorganic oxide layer on the flat piece of sapphire substrate by a first plasma enhanced chemical vapor deposition process comprises:
performing chemical vapor deposition by adopting inorganic gas and oxide gas according to a first flow ratio to obtain the first inorganic oxide layer, wherein the inorganic gas is gas containing inorganic chemical components of the first inorganic oxide layer, and the oxide gas is gas containing oxygen element chemical components;
forming a second inorganic oxide layer on the first inorganic oxide by a second plasma enhanced chemical vapor deposition process, comprising:
and performing chemical vapor deposition by adopting the inorganic gas and the oxide gas in a second flow ratio to obtain the second inorganic oxide layer, wherein the first flow ratio and the second flow ratio are proportional relations between the flow of the inorganic gas and the flow of the oxide gas, and the first flow ratio is smaller than the second flow ratio.
3. The method of claim 2, wherein the first inorganic oxide layer is obtained by chemical vapor deposition using an inorganic gas and an oxide gas at a first flow ratio, further comprising:
depositing the first inorganic oxide layer in nitrogen gas using the nitrogen gas as a carrier gas;
and performing chemical vapor deposition by adopting the inorganic gas and the oxide gas in a second flow ratio to obtain the second inorganic oxide layer, and further comprising:
the second inorganic oxide layer is deposited in the nitrogen gas using the nitrogen gas as a carrier gas.
4. The method of claim 3, wherein the second inorganic oxide layer is deposited in the nitrogen gas using the nitrogen gas as a carrier gas, further comprising:
there is a multiple relationship A between the gas amount of the nitrogen gas and the total gas amount of the inorganic gas and the oxide gas, wherein A < 1.5 < 3.
5. The method of manufacturing according to claim 2, wherein the first inorganic oxide layer comprises a first silicon dioxide layer, the second inorganic oxide layer comprises a second silicon dioxide layer, the inorganic gas comprises silane, and the oxide gas comprises laughing gas;
performing chemical vapor deposition by using an inorganic gas and an oxide gas at a first flow ratio to obtain the first inorganic oxide layer, including:
carrying out chemical vapor deposition by adopting the silane and the laughing gas to obtain the first silicon dioxide layer, wherein the flow ratio of the silane to the laughing gas is 1:40;
performing chemical vapor deposition with the inorganic gas and the oxide gas at a second flow ratio to obtain the second inorganic oxide layer, including:
and carrying out chemical vapor deposition by adopting the silane and the laughing gas to obtain the second silicon dioxide layer, wherein the flow ratio of the silane to the laughing gas is 9:10.
6. The method of claim 1, wherein the first inorganic oxide layer has a deposition thickness in the range of 1.0um to 2.4um and the second inorganic oxide layer has a deposition thickness in the range of 50nm to 180nm.
7. The method of manufacturing according to claim 1, further comprising: and coating photoresist on the second inorganic oxide layer through a photoresist homogenizing process to form a photoresist layer.
8. The method of claim 5, further comprising, after forming a photoresist layer by coating a photoresist on the second inorganic oxide layer by a photoresist uniformizing process:
forming a pattern structure on the photoresist layer through exposure and development;
transferring the graphic structure to the second inorganic oxide layer and the first inorganic oxide layer;
and removing the second inorganic oxide layer through an over-etching process to obtain a patterned substrate based on the composite material film layer, wherein the patterned substrate is formed with the pattern structure, and the pattern structure is prepared from the first inorganic oxide layer.
9. A patterned substrate based on a composite film layer, characterized in that the patterned substrate is prepared by the method for preparing a patterned substrate based on a composite film layer according to any one of claims 1-8.
10. An LED epitaxial wafer comprising the patterned substrate based on a composite film layer according to any one of claims 9.
CN202310175665.5A 2023-02-27 2023-02-27 Patterned substrate based on composite material film, preparation method and LED epitaxial wafer Pending CN116190507A (en)

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