Patterned substrate based on composite material film layer, preparation method and LED epitaxial wafer
By forming inorganic oxide layers with different oxygen contents on the sapphire substrate, the adhesion of the photoresist is improved, the problem of poor adhesion on the surface of the low-refractive-index film layer is solved, and an efficient photoresist process and low-cost patterned substrate preparation are achieved.
Patent Information
- Application Number
- CN202310175665.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-02-27
- Publication Date
- 2025-09-16
- Estimated Expiration
- 2043-02-27
AI Technical Summary
In the prior art, the surface adhesion of the low refractive index film layer is low, which requires surface modification and viscosity enhancement treatment in the coating process. The modification treatment is prone to failure, increasing uncertainty and cost.
By forming a first inorganic oxide layer and a second inorganic oxide layer on a sapphire substrate, controlling the oxygen content of the second layer to be lower than that of the first layer, improving the adhesion of the photoresist, reducing the number of surface modification and adhesion treatment steps, and using a plasma-enhanced chemical vapor deposition process to regulate the oxygen content and adhesion.
The photoresist film layer's uniform coating yield is improved, debonding defects are avoided, preparation efficiency is improved, and production costs are reduced.
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Figure CN116190507B_ABST
Abstract
Description
Technical Field
[0001] The embodiments of the present invention relate to the field of semiconductor manufacturing technology, and in particular to a patterned substrate based on a composite material film layer, a preparation method, and an LED epitaxial wafer. Background Art
[0002] The pursuit of higher light extraction efficiency is a key research focus in substrate materials. One of the key principles by which composite substrates can improve light extraction efficiency is the introduction of low-refractive-index heterogeneous materials. Low-refractive-index film layers can create a larger critical value for total reflection angle at the material interface during LED light extraction, facilitating full emission of light from within the LED device. Oxygen content is the primary factor affecting the refractive index of heterogeneous materials and also the adhesion between them and the photoresist.
[0003] A low refractive index requires a low oxygen content, and a low oxygen content means that the surface adhesion of the material is also low. Therefore, after obtaining the low refractive index film layer, people often need to perform surface modification and viscosity-enhancing treatment on the film layer in the coating process. This is also subject to time constraints. If the surface modification and viscosity-enhancing treatment is left for too long, it will become ineffective, increasing uncertainty and the cost of the corresponding steps. Summary of the Invention
[0004] The embodiments of the present invention provide a patterned substrate, a preparation method and an LED epitaxial wafer based on a composite material film layer, so as to improve the film layer's adhesive yield, reduce the steps of surface modification and adhesion enhancement treatment of the film layer, and avoid debonding defects of the patterned substrate.
[0005] In a first aspect, an embodiment of the present invention provides a method for preparing a patterned substrate based on a composite material film layer, comprising:
[0006] Providing a flat sapphire substrate;
[0007] forming a first inorganic oxide layer on the flat sapphire substrate by a first plasma enhanced chemical vapor deposition process;
[0008] A second inorganic oxide layer is formed 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 less than that of the first inorganic oxide layer.
[0009] Optionally, forming a first inorganic oxide layer on the flat sapphire substrate by a first plasma enhanced chemical vapor deposition process comprises:
[0010] Performing chemical vapor deposition using an inorganic gas and an oxide gas at a first flow ratio to form the first inorganic oxide layer, wherein the inorganic gas is a gas containing an inorganic chemical component of the first inorganic oxide layer, and the oxide gas is a gas containing a chemical component of the oxygen element;
[0011] Forming a second inorganic oxide layer on the first inorganic oxide by a second plasma enhanced chemical vapor deposition process, comprising:
[0012] Chemical vapor deposition is performed using the inorganic gas and the oxide gas at a second flow ratio to obtain the second inorganic oxide layer, wherein the first flow ratio and the second flow ratio are both proportional relationships between the flow rate of the inorganic gas and the flow rate of the oxide gas, and the first flow ratio is smaller than the second flow ratio.
[0013] Optionally, chemical vapor deposition is performed using an inorganic gas and an oxide gas at a first flow ratio to obtain the first inorganic oxide layer, further comprising:
[0014] Using nitrogen as a carrier gas, depositing the first inorganic oxide layer in the nitrogen;
[0015] The method further comprises: performing chemical vapor deposition using the inorganic gas and the oxide gas at a second flow ratio to obtain the second inorganic oxide layer;
[0016] The nitrogen gas is used as a carrier gas, and the second inorganic oxide layer is deposited in the nitrogen gas.
[0017] Optionally, the nitrogen gas is used as a carrier gas, and the second inorganic oxide layer is deposited in the nitrogen gas, further comprising:
[0018] 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 1.5<A<3.
[0019] Optionally, the first inorganic oxide layer includes a first silicon dioxide layer, the second inorganic oxide layer includes a second silicon dioxide layer, the inorganic gas includes silane, and the oxide gas includes nitrous oxide;
[0020] The first inorganic oxide layer is obtained by chemical vapor deposition using an inorganic gas and an oxide gas at a first flow ratio, comprising:
[0021] Performing chemical vapor deposition using 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;
[0022] Performing chemical vapor deposition using the inorganic gas and the oxide gas at a second flow ratio to obtain the second inorganic oxide layer comprises:
[0023] Chemical vapor deposition is performed using 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.
[0024] Optionally, the deposition thickness of the first inorganic oxide layer is in the range of 1.0 um to 2.4 um, and the deposition thickness of the second inorganic oxide layer is in the range of 50 nm to 180 nm.
[0025] Optionally, the method further includes: coating photoresist on the second inorganic oxide layer through a coating process to form a photoresist layer.
[0026] Optionally, after applying photoresist on the second inorganic oxide layer through a spin coat process to form a photoresist layer, the method further includes:
[0027] forming a pattern structure on the photoresist layer by exposure and development;
[0028] transferring the pattern structure to the second inorganic oxide layer and the first inorganic oxide layer;
[0029] The second inorganic oxide layer is removed by an over-etching process to obtain a patterned substrate based on a composite material film layer on which the pattern structure is formed, wherein the pattern structure is prepared by the first inorganic oxide layer.
[0030] In a second aspect, an embodiment of the present invention further provides a patterned substrate based on a composite material film layer, which is prepared using the method for preparing a patterned substrate based on a composite material film layer as described in any one of the first aspects.
[0031] In a third aspect, an embodiment of the present invention further provides an LED epitaxial wafer, comprising a patterned substrate based on a composite material film layer as described in any one of the second aspects.
[0032] Embodiments of the present invention provide a patterned substrate based on a composite film layer, a preparation method, and an LED epitaxial wafer. The preparation method for the patterned substrate based on a composite film layer includes: 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 less than that of the first inorganic oxide layer. Using the above method, the oxygen content of the second inorganic oxide layer is less than that of the first inorganic oxide layer, which helps improve the adhesion of the second inorganic oxide layer to the photoresist, thereby improving the photoresist film layer's coating yield, reducing the number of surface modification and viscosity-enhancing treatment steps for the film layer, reducing the time limit during the coating process, avoiding debonding defects in the patterned substrate, improving the preparation efficiency of the patterned substrate, and reducing the production cost of the patterned substrate. BRIEF DESCRIPTION OF THE DRAWINGS
[0033] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.
[0034] Figure 1 This is a schematic flow chart of a method for preparing a patterned substrate based on a composite material film layer provided by an embodiment of the present invention;
[0035] Figure 2 yes Figure 1 The structural flow chart of the method for preparing a patterned substrate based on a composite material film layer is shown;
[0036] Figure 3 This is a schematic flow chart of another method for preparing a patterned substrate based on a composite material film layer provided by an embodiment of the present invention;
[0037] Figure 4 This is a schematic flow chart of another method for preparing a patterned substrate based on a composite material film layer provided by an embodiment of the present invention;
[0038] Figure 5 This is a schematic flow chart of another method for preparing a patterned substrate based on a composite material film layer provided by an embodiment of the present invention;
[0039] Figure 6 yes Figure 5 The structural flow chart of the method for preparing a patterned substrate based on a composite material film layer is shown;
[0040] Figure 7A patterned substrate based on a composite material film layer provided by an embodiment of the present invention;
[0041] Figure 8 It is a structural schematic diagram of an LED epitaxial wafer provided by an embodiment of the present invention. DETAILED DESCRIPTION
[0042] The present invention will be further described in detail below with reference to the accompanying drawings and examples. It will be understood that the specific embodiments described herein are intended only to illustrate the present invention and are not intended to limit the present invention. It should also be noted that, for ease of description, the accompanying drawings only illustrate portions relevant to the present invention, not all structures.
[0043] The terms used in the embodiments of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. It should be noted that the directional words such as "upper", "lower", "left", and "right" described in the embodiments of the present invention are described based on the angles shown in the accompanying drawings and should not be understood as limiting the embodiments of the present invention. In addition, in the context, it is also necessary to understand that when it is mentioned that an element is formed "on" or "under" another element, it can not only be formed directly "on" or "under" another element, but can also be formed indirectly "on" or "under" another element through an intermediate element. The terms "first", "second", etc. are only used for descriptive purposes and do not indicate any order, quantity or importance, but are only used to distinguish different components. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.
[0044] The term "including" and its variations used in the present invention are open inclusions, that is, "including but not limited to." The term "based on" means "based at least in part on." The term "one embodiment" means "at least one embodiment."
[0045] It should be noted that the concepts such as "first" and "second" mentioned in the present invention are only used to distinguish the corresponding contents, and are not used to limit the order or mutual dependence.
[0046] It should be noted that the modifications of "one" and "multiple" mentioned in the present invention are illustrative rather than restrictive. Those skilled in the art should understand that unless otherwise clearly indicated in the context, it should be understood as "one or more".
[0047] Figure 1 1 is a flow chart of a method for preparing a patterned substrate based on a composite material film layer provided by an embodiment of the present invention. Figure 2 yes Figure 1 The structural flow chart of the method for preparing a patterned substrate based on a composite material film layer is shown in FIG. Figure 1 and Figure 2As shown, the method for preparing a patterned substrate based on a composite material film layer includes:
[0048] S110. Provide a flat sapphire substrate.
[0049] Specifically, refer to Figure 2 In Figure a), the flat sapphire substrate 10 is a smoothly polished, flat substrate with a flat surface. This means the flat sapphire substrate 10 has a high-quality C-plane, which facilitates the formation of epitaxial crystal nuclei and the growth of epitaxial layers. Furthermore, before the subsequent growth of epitaxial layers or heterogeneous layers, the flat sapphire substrate 10 needs to be pre-treated by cleaning and drying. For example, the flat sapphire substrate 10 can be wet-cleaned in a 90°C-150°C SPM solution (a mixture of sulfuric acid and hydrogen peroxide in a ratio of 6:1) for 20 minutes, then rinsed with deionized water. Finally, the flat sapphire substrate 10 is rotated for drying.
[0050] S120 , forming a first inorganic oxide layer on the flat sapphire substrate through a first plasma enhanced chemical vapor deposition process.
[0051] Specifically, refer to Figure 2 In Figure b), the first inorganic oxide layer 20 is a film layer made of an inorganic oxide material. The inorganic oxide material is actually relative to the flat sapphire substrate 10 and the epitaxial layer material such as gallium nitride, that is, a material different from the flat sapphire substrate 10 and the epitaxial material. Exemplarily, the inorganic oxide material can be silicon dioxide (SiO2), indium tin oxide (ITO), tin oxide (SnO2) and silver oxide (AgO), etc.
[0052] 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 less than the oxygen content of the first inorganic oxide layer.
[0053] Specifically, refer to Figure 2In Figure c), the second inorganic oxide layer 30 is a film layer made of an inorganic oxide material. The inorganic oxide material is actually relative to the flat sapphire substrate 10 and the epitaxial layer material such as gallium nitride, that is, a material different from the flat sapphire substrate 10 and the epitaxial material. The inorganic oxide material can be silicon dioxide (SiO2), indium tin oxide (ITO), tin oxide (SnO2) and silver oxide (AgO), etc. It should be noted that the inorganic oxide materials used in the first inorganic oxide layer 20 and the second inorganic oxide layer 30 can be the same or different, but the oxygen content of the second inorganic oxide layer 30 is less than that of the first inorganic oxide layer 20, which can effectively regulate the polarity of the surface of the entire film layer, so that the surface properties of the hydrophilic first inorganic oxide layer 20 are transformed into the surface properties of the hydrophobic second inorganic oxide layer 30, and the adhesion performance of the second inorganic oxide layer 30 is higher than that of the first inorganic oxide layer 20. The overall surface properties of the flat sapphire substrate 10, the first inorganic oxide layer 20 and the second inorganic oxide layer 30 finally formed are hydrophobic, and the overall adhesion performance is stronger, which facilitates the subsequent step of coating the photoresist layer.
[0054] The technical solution in an embodiment of the present invention first provides a flat sapphire substrate; then, a first inorganic oxide layer is formed on the flat sapphire substrate through a first plasma-enhanced chemical vapor deposition process; and finally, a second inorganic oxide layer is formed 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 less than that of the first inorganic oxide layer. Using this method, the oxygen content of the second inorganic oxide layer is less than that of the first inorganic oxide layer, which helps improve the adhesion of the second inorganic oxide layer to the photoresist, thereby improving the passivation yield of the photoresist film layer, reducing the number of surface modification and adhesion-enhancing treatment steps of the film layer, reducing the time limit during the passivation process, avoiding debonding defects in the patterned substrate, improving the preparation efficiency of the patterned substrate, and reducing the production cost of the patterned substrate.
[0055] Figure 3 This is a schematic flow diagram of another method for preparing a patterned substrate based on a composite material film layer, provided in an embodiment of the present invention. This embodiment is an optimization of the above embodiment. Optionally, a first inorganic oxide layer is formed on a flat sapphire substrate by a first plasma-enhanced chemical vapor deposition process, including:
[0056] Performing chemical vapor deposition with an inorganic gas and an oxide gas at a first flow ratio to form a first inorganic oxide layer, wherein the inorganic gas is a gas containing an inorganic chemical component of the first inorganic oxide layer, and the oxide gas is a gas containing a chemical component of oxygen;
[0057] Forming a second inorganic oxide layer on the first inorganic oxide by a second plasma enhanced chemical vapor deposition process, comprising:
[0058] Chemical vapor deposition is performed using inorganic gas and oxide gas at a second flow ratio to obtain a second inorganic oxide layer, wherein the first flow ratio and the second flow ratio are both proportional relationships between the flow rate of the inorganic gas and the flow rate of the oxide gas, and the first flow ratio is smaller than the second flow ratio.
[0059] For details not yet provided in this embodiment, please refer to the above embodiments. Figure 3 As shown, the method for preparing a patterned substrate based on a composite material film layer includes:
[0060] S210, providing a flat sapphire substrate.
[0061] S220, performing chemical vapor deposition using an inorganic gas and an oxide gas at a first flow ratio to obtain a first inorganic oxide layer, wherein the inorganic gas is a gas containing inorganic chemical components of the first inorganic oxide layer, and the oxide gas is a gas containing oxygen chemical components.
[0062] Specifically, continue to refer to Figure 2 As shown in FIG b), through a first plasma enhanced chemical vapor deposition process, inorganic gas and oxide gas can be used for chemical vapor deposition to form a first inorganic oxide layer 20 on a flat sapphire substrate 10, and by controlling a first flow ratio between the inorganic gas and the oxide gas, the oxygen content of the formed first inorganic oxide layer 20 can be changed.
[0063] Optionally, continue to refer to Figure 2 FIG b) shows a process of chemical vapor deposition of an inorganic gas and an oxide gas at a first flow ratio to obtain a first inorganic oxide layer 20, and further includes: using nitrogen as a carrier gas to deposit the first inorganic oxide layer 20 in the nitrogen. Specifically, nitrogen can be used as a carrier gas, or high-purity nitrogen can be used as a carrier gas. High-purity nitrogen has high purity, extremely low water and oxygen content, and high reliability. It is a colorless and odorless inert gas at room temperature and pressure. Depositing the first inorganic oxide layer 20 in nitrogen can make the surface of the film of the first inorganic oxide layer 20 obtained by chemical vapor deposition of the inorganic gas and the oxide gas more uniform, and nitrogen can also change the adhesion of the first inorganic oxide layer 20 to a certain extent. Optionally, the deposition thickness of the first inorganic oxide layer 20 can range from 1.0um to 2.4um.
[0064] S230. Perform chemical vapor deposition using an inorganic gas and an oxide gas at a second flow ratio to obtain a second inorganic oxide layer, wherein the first flow ratio and the second flow ratio are both proportional relationships between the flow rate of the inorganic gas and the flow rate of the oxide gas, and the first flow ratio is smaller than the second flow ratio.
[0065] Specifically, continue to refer to Figure 2 As shown in FIG. c), a second plasma-enhanced chemical vapor deposition process can be performed using an inorganic gas and an oxide gas for chemical vapor deposition to form a second inorganic oxide layer 30 on the first inorganic oxide 20. Furthermore, by controlling a second flow ratio between the inorganic gas and the oxide gas, the oxygen content of the formed second inorganic oxide layer 30 can be varied. It should be noted that if the first flow ratio is less than the second flow ratio, the proportion of the oxide gas during the deposition process decreases from large to small, thereby enabling the oxygen content of the deposited second inorganic oxide layer 30 to be less than that of the first inorganic oxide layer 20.
[0066] Optionally, continue to refer to Figure 2Figure c) shows that an inorganic gas and an oxide gas are chemically vapor deposited at a second flow ratio to obtain a second inorganic oxide layer 30, further comprising: using nitrogen as a carrier gas to deposit the second inorganic oxide layer 30 in the nitrogen. Furthermore, using nitrogen as a carrier gas to deposit the second inorganic oxide layer 30 in the nitrogen also comprises: there is a multiple relationship A between the gas amount of nitrogen and the total gas amount of the inorganic gas and the oxide gas, wherein 1.5<A<3. Specifically, nitrogen can be used as a carrier gas, or high-purity nitrogen can be used as a carrier gas. High-purity nitrogen has high purity, extremely low water and oxygen content, high reliability, and is a colorless and odorless inert gas at room temperature and pressure. Depositing the second inorganic oxide layer 30 in nitrogen can make the film surface of the second inorganic oxide layer 30 obtained by chemical vapor deposition of the inorganic gas and the oxide gas more uniform, and nitrogen can also change the adhesion of the second inorganic oxide layer 30 to a certain extent. In addition, the adhesion of the film surface is affected by both the oxygen content of the film and the properties of the nitrogen. During the deposition of the second inorganic oxide layer 30, to ensure that the oxygen content is within a relatively low range (the oxygen content of the second inorganic oxide layer 30 is less than that of the first inorganic oxide layer 20) and the adhesion performance of the film surface of the second inorganic oxide layer 30 is within a relatively high range (the adhesion of the second inorganic oxide layer 30 is greater than that of the first inorganic oxide layer 20), the amount of nitrogen should be greater than the total amount of the inorganic gas and the oxide gas. There is a multiple relationship A between the amount of nitrogen and the total amount of the inorganic gas and the oxide gas, where 1.5 < A < 3. For example, the amount of nitrogen can be twice the total amount of the inorganic gas and the oxide gas. Optionally, the deposition thickness of the second inorganic oxide layer 30 can range from 50 nm to 180 nm, and the deposition thickness of the second inorganic oxide layer 30 is less than the deposition thickness of the first inorganic oxide layer 20.
[0067] The technical solution in the embodiment of the present invention can effectively regulate the oxygen content in the deposited first inorganic oxide layer and the second inorganic oxide layer by changing the flow ratio of the inorganic gas and the oxide gas during the chemical vapor deposition process, thereby achieving the purpose of regulating the surface adhesion of the film layer of the first inorganic oxide layer and the second inorganic oxide layer, improving the adhesion of the overall film layer, avoiding the abnormal debonding phenomenon of the overall film layer, and improving the yield of uniform bonding.
[0068] In a specific embodiment, Figure 4This is a schematic flow diagram of another method for preparing a patterned substrate based on a composite material film layer provided in an embodiment of the present invention. This embodiment is optimized based on the above embodiment. Optionally, the first inorganic oxide layer includes a first silicon dioxide layer, the second inorganic oxide layer includes a second silicon dioxide layer, the inorganic gas includes silane, and the oxide gas includes nitrous oxide;
[0069] 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, comprising:
[0070] Chemical vapor deposition is performed using silane and nitrous oxide to obtain a first silicon dioxide layer, wherein the flow ratio of silane to nitrous oxide is 1:40;
[0071] 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, comprising:
[0072] Chemical vapor deposition is performed using silane and nitrous oxide to obtain a second silicon dioxide layer, wherein the flow ratio of silane to nitrous oxide is 9:10.
[0073] For details not yet provided in this embodiment, please refer to the above embodiments. Figure 4 As shown, the method for preparing a patterned substrate based on a composite material film layer includes:
[0074] S310, providing a flat sapphire substrate.
[0075] S320, using silane and nitrous oxide to perform chemical vapor deposition to obtain a first silicon dioxide layer, wherein the flow ratio of silane to nitrous oxide is 1:40.
[0076] Specifically, continue to refer to Figure 2 b) Figure, wherein the first inorganic oxide layer 20 can be a first silicon dioxide layer 21, the inorganic gas can be silane (SiH4), and the oxide gas can be laughing gas (N2O). Through a first plasma enhanced chemical vapor deposition process, silane and laughing gas can be used for chemical vapor deposition, using nitrogen as a carrier gas to form the first silicon dioxide layer 21 on the flat sapphire substrate 10. Exemplarily, the flow ratio of silane to laughing gas can be 1:40, which is a first flow ratio. This first flow ratio can effectively regulate the oxygen content of the first silicon dioxide layer 21. In addition, the process of depositing the first silicon dioxide layer 21 specifically includes: placing the flat sapphire substrate 10 on an aluminum carrier in a plasma-enhanced chemical vapor deposition chamber, setting the temperature of the aluminum carrier to 180-280°C, pumping the pressure of the chamber to 160-80 Pa, and depositing the first silicon dioxide layer 21 in an atmosphere of nitrogen, silane and nitrous oxide. Exemplarily, the deposition thickness of the first silicon dioxide layer 21 can be 2.1 um.
[0077] S330, using silane and nitrous oxide to perform chemical vapor deposition to obtain a second silicon dioxide layer, wherein the flow ratio of silane to nitrous oxide is 9:10.
[0078] Specifically, continue to refer to Figure 2 In Figure c), the second inorganic oxide layer 30 may be a second silicon dioxide layer 31, the inorganic gas may be silane, and the oxide gas may be nitrous oxide. Through a second plasma-enhanced chemical vapor deposition process, chemical vapor deposition may be performed using silane and nitrous oxide, with nitrogen as a carrier gas, to form the second silicon dioxide layer 31 on the first silicon dioxide layer 21. Exemplarily, the flow ratio of silane to nitrous oxide may be 9:10, which is a second flow ratio. This second flow ratio can effectively regulate the oxygen content of the second silicon dioxide layer 31. The second flow ratio is greater than the first flow ratio, and the oxygen content of the second silicon dioxide layer 31 is less than the oxygen content of the first silicon dioxide layer 21. In addition, during the process of depositing the second silicon dioxide layer 31, the process specifically includes: turning off the radio frequency energy after the deposition of the first silicon dioxide layer 21 is completed, and adjusting to increase the flow ratio of silane and laughing gas. After 15 seconds of stable deposition of the second silicon dioxide layer 31, the radio frequency energy is turned back on, and the second silicon dioxide layer 31 is deposited in an atmosphere of nitrogen, silane and laughing gas, and the amount of nitrogen gas is 2 times the total amount of silane and laughing gas. Exemplarily, the deposition thickness of the second silicon dioxide layer 31 can be 60nm.
[0079] The technical solution in the embodiment of the present invention provides a specific method for separately depositing a first silicon dioxide layer and a second silicon dioxide layer, which can effectively control the oxygen content of the first silicon dioxide layer to be greater than the oxygen content of the second silicon dioxide layer, thereby improving the adhesion performance of the overall film surface of the finally formed flat sapphire substrate, the first silicon dioxide layer and the second silicon dioxide layer, improving the uniform coating yield of the photoresist film layer, avoiding the debonding defects of the patterned substrate, improving the preparation efficiency of the patterned substrate, and reducing the production cost of the patterned substrate.
[0080] Figure 5 This is a schematic flow chart of another method for preparing a patterned substrate based on a composite material film layer provided by an embodiment of the present invention. Figure 6 yes Figure 5 The structural flow chart of the method for preparing a patterned substrate based on a composite material film layer is shown. This embodiment is optimized based on the above embodiment. Optionally, it further includes: applying a photoresist on the second inorganic oxide layer through a sizing process to form a photoresist layer. Furthermore, after applying a photoresist on the second inorganic oxide layer through a sizing process to form a photoresist layer, it further includes:
[0081] forming a pattern structure on the photoresist layer by exposure and development;
[0082] transferring the pattern structure to the second inorganic oxide layer and the first inorganic oxide layer;
[0083] The second inorganic oxide layer is removed through an over-etching process to obtain a patterned substrate based on a composite material film layer with a patterned structure, wherein the patterned structure is prepared by the first inorganic oxide layer.
[0084] For details not yet provided in this embodiment, please refer to the above embodiments. Figure 6 and Figure 7 As shown, the method for preparing a patterned substrate based on a composite material film layer includes:
[0085] S410, providing a flat sapphire substrate.
[0086] S420 , forming a first inorganic oxide layer on the flat sapphire substrate through a first plasma enhanced chemical vapor deposition process.
[0087] 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 less than the oxygen content of the first inorganic oxide layer.
[0088] S440 , coating a photoresist on the second inorganic oxide layer through a coating process to form a photoresist layer.
[0089] Specifically, refer to Figure 6d), the first inorganic oxide layer 20 and the second inorganic oxide layer 30 are respectively deposited in a nitrogen atmosphere, which can make the surfaces of the first inorganic oxide layer 20 and the second inorganic oxide layer 30 more uniform and flat. Through the uniform coating process, photoresist is coated on the surface of the flat second inorganic oxide layer 30, and the formed photoresist layer 40 will also be flatter and the thickness will be more uniform. For example, when preparing the photoresist layer 40, the photoresist can be selected as a positive photoresist or a negative photoresist. The photoresist layer 40 can be prepared by a spin coating or spray coating process, and its thickness can be set in the range of 0.3μm-5μm. For example, the thickness of the photoresist layer 40 can be 2.3μm. It should be noted that the surface adhesion of the second inorganic oxide layer 30 is stronger. After the surface of the formed second inorganic oxide layer 30 is rinsed with deionized water and spin-dried, a photoresist can be directly applied to the surface of the second inorganic oxide layer 30 to obtain a well-adhesive photoresist composite sheet, which lays the foundation for the subsequent production of the photoresist glue column mask pattern without the need for steps such as baking or spin-coating a tackifier / modifier. This can effectively reduce the preparation steps of the patterned substrate and reduce the defect of surface debonding of the patterned substrate. Moreover, due to the surface adhesion of the second inorganic oxide layer 30, the process of applying the photoresist is not subject to time constraints. Compared with the tackifier / modifier in the steps of baking or spin-coating a tackifier / modifier, the tackifier / modifier will lose its effectiveness due to long storage time, which adds uncertainty to the process of applying the photoresist and increases the cost of the corresponding steps and required materials.
[0090] S450 , forming a pattern structure on the photoresist layer through exposure and development.
[0091] Specifically, refer to Figure 6 As shown in FIG e), since the surface of the formed photoresist layer 40 is smoother and the thickness is more uniform, the graphic structure of the photoresist pillar mask prepared on the photoresist layer 40 by exposure and development is also more accurate, the size of the pillars is more in line with the standard, and the pattern of the photoresist pillar mask corresponds to the pattern on the final patterned substrate based on the composite film layer. In addition, when preparing the photoresist pillar mask, it can be achieved through pattern transfer technology such as photolithography or nanoimprinting. For example, taking the photolithography process as an example, exposure is performed on the photoresist layer 40 through the photoresist pillar mask, and then the photoresist layer 40 can be patterned by the development step, that is, the pattern of the photoresist pillar mask is transferred to the photoresist layer 40 to form a photoresist pillar mask.
[0092] S460 , transferring the pattern structure to the second inorganic oxide layer and the first inorganic oxide layer.
[0093] Specifically, refer to Figure 6f) of the figure, according to the process of pattern transfer using the photoresist column mask, a dry or wet etching process can be used to etch the second inorganic oxide layer 30 and the first inorganic oxide layer 20 respectively to complete the patterning. At this time, the pattern structure formed includes both part of the material of the first inorganic oxide layer 20 and part of the material of the second inorganic oxide layer 30.
[0094] S470, removing the second inorganic oxide layer through an over-etching process to obtain a patterned substrate based on a composite material film layer having a patterned structure, wherein the patterned structure is prepared by the first inorganic oxide layer.
[0095] Specifically, refer to Figure 6 g), optionally, the deposition thickness of the first inorganic oxide layer 20 ranges from 1.0 μm to 2.4 μm, and the deposition thickness of the second inorganic oxide layer 30 ranges from 50 nm to 180 nm. The deposition thickness of the first inorganic oxide layer 20 is much greater than the deposition thickness of the second inorganic oxide layer 30. The second inorganic oxide layer 30 can be removed by an over-etching process, so that the final patterned structure only includes a portion of the material of the first inorganic oxide layer 20. The final composite film-based patterned substrate with a patterned structure includes a flat sapphire substrate 10 and a patterned structure prepared from a portion of the material of the first inorganic oxide layer 20. It should be noted that the final composite film-based patterned substrate does not include the second inorganic oxide layer 30, and the deposition and removal process of the second inorganic oxide layer 30 will not affect the optical and electrical properties of the final composite film-based patterned substrate. For example, if the first inorganic oxide layer 20 has a low refractive index, the final composite film-based patterned substrate still has a low refractive index.
[0096] The technical solution in the embodiment of the present invention is to coat photoresist on the surface of the second inorganic oxide layer, and finally obtain a patterned substrate based on a composite material film layer with a patterned structure, which not only realizes the transfer of the patterned structure but also does not affect the properties of the patterned substrate, effectively reduces the preparation steps of baking or spin coating of the patterned substrate with a thickener / modifier, etc., reduces the surface debonding defect of the patterned substrate, avoids the time limitation of the photoresist coating process, and also reduces the occurrence of uncertain factors in the preparation process and the cost of the corresponding steps and required materials.
[0097] Figure 7 The embodiment of the present invention provides a patterned substrate based on a composite material film layer, such as Figure 7 As shown, the patterned substrate based on the composite material film layer is prepared by using the method for preparing the patterned substrate based on the composite material film layer provided by any one of the embodiments of the present invention.
[0098] Based on the same inventive concept, an embodiment of the present invention further provides an LED epitaxial wafer. Figure 8 Schematic diagram of the structure of an LED epitaxial wafer provided by an embodiment of the present invention, such as Figure 8 As shown, the LED epitaxial wafer includes a patterned substrate 1 based on a composite material film layer as provided in any of the above embodiments, and also includes an epitaxial layer 2 formed on the patterned substrate 1 based on a composite material film layer.
[0099] Forming epitaxial layers on patterned substrates of different materials requires different LED epitaxial wafer growth technologies. However, for the patterned substrate based on a composite film layer provided in the embodiments of the present invention, the epitaxial layer 2 in the LED epitaxial wafer can be a GaN, AlGaN epitaxial layer, or the like. Because this LED epitaxial wafer utilizes the patterned substrate 1 based on a composite film layer provided in the aforementioned embodiments, it exhibits the same or similar benefits as the patterned substrate 1 based on a composite film layer, and further description thereof will not be given here.
[0100] Note that the above are only preferred embodiments of the present invention and the technical principles employed. Those skilled in the art will appreciate that the present invention is not limited to the specific embodiments described herein, and that various obvious changes, readjustments, combinations, and substitutions are possible for those skilled in the art without departing from the scope of the present invention. Therefore, although the present invention has been described in detail through the above embodiments, the present invention is not limited to the above embodiments and may include many other equivalent embodiments without departing from the scope of the present invention. The scope of the present invention is determined by the scope of the appended claims.
Claims
1. A method for preparing a patterned substrate based on a composite material film layer, characterized in that: include: Providing a flat sapphire substrate; forming a first inorganic oxide layer on the flat sapphire substrate by a first plasma enhanced chemical vapor deposition process; forming a second inorganic oxide layer on the first inorganic oxide layer by a second plasma enhanced chemical vapor deposition process, wherein the oxygen content of the second inorganic oxide layer is less than the oxygen content of the first inorganic oxide layer; coating a photoresist on the second inorganic oxide layer through a spin coating process to form a photoresist layer; forming a pattern structure on the photoresist layer by exposure and development; transferring the pattern structure to the second inorganic oxide layer and the first inorganic oxide layer; The second inorganic oxide layer is removed by an over-etching process to obtain a patterned substrate based on a composite material film layer on which the pattern structure is formed, wherein the pattern structure is prepared by the first inorganic oxide layer.
2. The preparation method according to claim 1, characterized in that Forming a first inorganic oxide layer on the flat sapphire substrate by a first plasma enhanced chemical vapor deposition process, comprising: Performing chemical vapor deposition using an inorganic gas and an oxide gas at a first flow ratio to form the first inorganic oxide layer, wherein the inorganic gas is a gas containing an inorganic chemical component of the first inorganic oxide layer, and the oxide gas is a gas containing a chemical component of the oxygen element; Forming a second inorganic oxide layer on the first inorganic oxide by a second plasma enhanced chemical vapor deposition process, comprising: Chemical vapor deposition is performed using the inorganic gas and the oxide gas at a second flow ratio to obtain the second inorganic oxide layer, wherein the first flow ratio and the second flow ratio are both proportional relationships between the flow rate of the inorganic gas and the flow rate of the oxide gas, and the first flow ratio is smaller than the second flow ratio.
3. The preparation method according to claim 2, characterized in that The method further comprises: performing chemical vapor deposition using an inorganic gas and an oxide gas at a first flow ratio to obtain the first inorganic oxide layer; Using nitrogen as a carrier gas, depositing the first inorganic oxide layer in the nitrogen; The method further comprises: performing chemical vapor deposition using the inorganic gas and the oxide gas at a second flow ratio to obtain the second inorganic oxide layer; The nitrogen gas is used as a carrier gas, and the second inorganic oxide layer is deposited in the nitrogen gas.
4. The preparation method according to claim 3, characterized in that Using the nitrogen gas as a carrier gas and depositing the second inorganic oxide layer in the nitrogen gas further comprises: 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 1.5<A<3.
5. The preparation method according to claim 2, characterized in that The first inorganic oxide layer includes a first silicon dioxide layer, the second inorganic oxide layer includes a second silicon dioxide layer, the inorganic gas includes silane, and the oxide gas includes laughing gas; The first inorganic oxide layer is obtained by chemical vapor deposition using an inorganic gas and an oxide gas at a first flow ratio, comprising: Performing chemical vapor deposition using 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 using the inorganic gas and the oxide gas at a second flow ratio to obtain the second inorganic oxide layer comprises: Chemical vapor deposition is performed using 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 preparation method according to claim 1, characterized in that The deposition thickness of the first inorganic oxide layer is in the range of 1.0 μm to 2.4 μm, and the deposition thickness of the second inorganic oxide layer is in the range of 50 nm to 180 nm.
7. A patterned substrate based on a composite material film layer, characterized in that: The patterned substrate is prepared by the method for preparing a composite material film layer according to any one of claims 1 to 6.
8. An LED epitaxial wafer, characterized in that: It comprises a patterned substrate based on a composite material film layer as claimed in claim 7.
Citation Information
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