Method for preparing aluminum-doped zinc oxide thin film

By preparing alumina thin films on a substrate and then subjecting them to boiling and drying to form micro-nano structures, and then preparing aluminum-doped zinc oxide thin films on them, the problems of high preparation cost and high resistance of aluminum-doped zinc oxide thin films are solved, achieving high transmittance and low resistance, which is suitable for large-scale production.

CN117867468BActive Publication Date: 2026-07-24GUANGCHI SEMICON TECH (SHANGHAI) CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
GUANGCHI SEMICON TECH (SHANGHAI) CO LTD
Filing Date
2023-12-13
Publication Date
2026-07-24

AI Technical Summary

Technical Problem

The existing technology for preparing aluminum-doped zinc oxide thin films is costly, the preparation process causes serious environmental pollution, and the resulting thin films have excessively high resistance, which cannot meet the requirements for use.

Method used

Alumina thin films were prepared on a substrate and subjected to boiling and drying treatment to form micro-nano structures. Aluminum-doped zinc oxide thin films were then prepared on the substrate. Atomic layer deposition technology was used to control the doping ratio and plasma treatment to optimize the transmittance and resistivity of the thin films.

Benefits of technology

It reduces production costs, simplifies the preparation process, and produces aluminum-doped zinc oxide films with higher transmittance and lower resistance. It is also environmentally friendly and suitable for large-scale promotion.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application belongs to the technical field of transparent conductive films, and discloses a preparation method of an aluminum-doped zinc oxide film. The preparation method of the aluminum-doped zinc oxide film comprises the following steps: providing a substrate; preparing an aluminum oxide film on the substrate; performing water boiling and drying treatment on the aluminum oxide film to obtain a micro-nano structure, wherein the micro-nano structure is grass-like aluminum oxide; and preparing the aluminum-doped zinc oxide film on the micro-nano structure. According to the preparation method of the aluminum-doped zinc oxide film, the aluminum oxide film is first prepared on the substrate, and then the water boiling and drying treatment is performed on the aluminum oxide film to obtain the micro-nano structure, i.e. the grass-like aluminum oxide. The grass-like aluminum oxide is loose, porous, disordered and has a high specific surface area. The aluminum-doped zinc oxide film prepared on the grass-like aluminum oxide has high transmittance and low sheet resistance. The preparation method is simple in operation, economical and environmentally friendly, has low requirements on the environment, low production cost and high equipment compatibility, and is suitable for large-scale promotion.
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Description

Technical Field

[0001] This invention relates to the field of transparent conductive film technology, and in particular to a method for preparing an aluminum-doped zinc oxide thin film. Background Technology

[0002] Transparent conductive film (TCF) is a thin-film material that combines light transmittance and conductivity, and it has a wide range of applications in energy storage, displays, and other fields. Common TCFs include indium tin oxide (ITO) and aluminum zinc oxide (AZO). With the development of device integration, conventional TCF fabrication methods, such as magnetron sputtering and evaporation, are difficult to grow high-quality TCF films on substrates with complex morphologies. However, films prepared by atomic layer deposition (ALD) have the characteristics of high controllability and commonality. Therefore, ALD is considered a promising solution for TCF fabrication.

[0003] Similar to other deposition techniques, ITO prepared by ALD has high transmittance and conductivity, and the technology is more mature. However, its preparation process involves the rare element indium (In), making its preparation cost high and posing a significant environmental pollution problem. Therefore, AZO, as a cheaper and more environmentally friendly TCF material, has gradually attracted the attention of researchers. However, AZO prepared by ALD also faces the fundamental problem of excessively high resistance, making it difficult to meet the conditions for device use.

[0004] Therefore, there is an urgent need for a method for preparing aluminum-doped zinc oxide thin films to solve the above-mentioned technical problems. Summary of the Invention

[0005] The purpose of this invention is to provide a method for preparing aluminum-doped zinc oxide thin films, which aims to solve the problems of high preparation cost, serious environmental pollution during the preparation process, and excessively high resistance of the prepared aluminum-doped zinc oxide thin films that cannot meet the usage conditions in the prior art. This invention simplifies the preparation process of aluminum-doped zinc oxide thin films, reduces production costs, and has low environmental requirements, resulting in aluminum-doped zinc oxide thin films with lower sheet resistance.

[0006] To achieve this objective, the present invention adopts the following technical solution:

[0007] A method for preparing an aluminum-doped zinc oxide thin film, comprising:

[0008] Provide a base;

[0009] An alumina thin film is prepared on the substrate;

[0010] The alumina film is subjected to boiling and drying treatment to obtain a micro-nano structure, wherein the micro-nano structure is grass-like alumina;

[0011] Aluminum-doped zinc oxide thin films were prepared on the micro / nano structure.

[0012] Optionally, the thickness of the alumina film is 5nm-50nm.

[0013] Optionally, when the alumina film is subjected to boiling and drying treatment, the boiling temperature is set at 65℃-90℃, the boiling time is 1min-30min, the drying temperature is 85℃-120℃, and the drying time is 10min-20min.

[0014] Optionally, the alumina film is prepared by atomic layer deposition.

[0015] Optionally, when preparing an aluminum-doped zinc oxide thin film on the micro / nano structure, the following steps are included:

[0016] Aluminum precursors are pre-deposited on the micro / nano structure;

[0017] The aluminum-doped zinc oxide thin film was grown using atomic layer deposition.

[0018] Optionally, the aluminum precursor is trimethylaluminum, and when depositing the aluminum-doped zinc oxide film, the zinc source is diethylzinc and the oxygen source is water.

[0019] Optionally, the trimethylaluminum and the diethylzinc may be deposited in multiple cycles.

[0020] Optionally, the cycling ratio of the trimethylaluminum and the diethylzinc is 16:1 or 29:1.

[0021] Optionally, at the end of a single deposition cycle, hydrogen gas needs to be introduced into the chamber for plasma treatment, the plasma treatment time is 300s, and the plasma power is 900w.

[0022] Optionally, the thickness of the aluminum-doped zinc oxide film is 150 nm.

[0023] The beneficial effects of this invention are as follows: The method for preparing aluminum-doped zinc oxide thin films provided by this invention involves first preparing an aluminum oxide thin film on a substrate, and then subjecting the aluminum oxide thin film to a boiling and drying process to obtain a micro-nano structure, namely grass-like alumina. Grass-like alumina is loose, porous, and disordered, and has a high specific surface area. The aluminum-doped zinc oxide thin film prepared on grass-like alumina has high transmittance and low sheet resistance. Moreover, this preparation method is simple to operate, economical and environmentally friendly, has low environmental requirements, low production costs, and high equipment compatibility, making it suitable for large-scale promotion. Attached Figure Description

[0024] Figure 1 This is a schematic flowchart of the preparation method of aluminum-doped zinc oxide thin film provided in the embodiments of the present invention;

[0025] Figure 2 This is a line graph showing the changes in sheet resistance and average transmittance of an aluminum-doped zinc oxide thin film prepared on a D263T glass substrate under one embodiment of the present invention.

[0026] Figure 3 This is a line graph showing the changes in sheet resistance and average transmittance of an aluminum-doped zinc oxide thin film prepared on a D263T glass substrate under another embodiment of the present invention.

[0027] In the picture:

[0028] 100, substrate; 200, alumina film; 300, micro / nano structure; 400, aluminum-doped zinc oxide film. Detailed Implementation

[0029] The present invention will now be described in further detail with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and not intended to limit it. Furthermore, it should be noted that, for ease of description, the accompanying drawings show only the parts relevant to the present invention, and not all of the structures.

[0030] In the description of this invention, unless otherwise explicitly specified and limited, the terms "connected," "linked," and "fixed" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0031] In this invention, unless otherwise explicitly specified and limited, "above" or "below" the second feature can include direct contact between the first and second features, or contact between the first and second features through another feature between them. Furthermore, "above," "over," and "on top" of the second feature includes the first feature directly above or diagonally above the second feature, or simply indicates that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature includes the first feature directly below or diagonally below the second feature, or simply indicates that the first feature is at a lower horizontal level than the second feature.

[0032] In the description of this embodiment, the terms "upper," "lower," "right," etc., refer to the orientation or positional relationship shown in the accompanying drawings. They are used only for ease of description and simplification of operation, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the present invention. In addition, the terms "first" and "second" are used only for distinction in description and have no special meaning.

[0033] This embodiment provides a method for preparing aluminum-doped zinc oxide thin films, aiming to solve the problems of high preparation cost, serious environmental pollution during the preparation process, and excessively high resistance of the prepared aluminum-doped zinc oxide thin films that cannot meet the usage conditions in the prior art. The method simplifies the preparation process of aluminum-doped zinc oxide thin films, reduces production costs, and has low environmental requirements, resulting in aluminum-doped zinc oxide thin films with lower sheet resistance.

[0034] like Figure 1 As shown, the preparation method of this aluminum-doped zinc oxide thin film includes:

[0035] S1. Provide a substrate 100;

[0036] S2. Prepare an alumina thin film 200 on a substrate 100;

[0037] S3. The alumina film 200 is subjected to boiling and drying treatment to obtain micro-nano structure 300, which is grass-like alumina.

[0038] S4. Prepare aluminum-doped zinc oxide thin film 400 on micro / nano structure 300.

[0039] The method for preparing aluminum-doped zinc oxide thin films provided in this embodiment involves first preparing an aluminum oxide thin film 200 on a substrate 100, and then subjecting the aluminum oxide thin film 200 to a boiling and drying process to obtain a micro-nano structure 300, namely grass-like alumina. Grass-like alumina is loose, porous, and disordered, and has a high specific surface area. The aluminum-doped zinc oxide thin film 400 prepared on grass-like alumina has high transmittance and low sheet resistance. Moreover, this preparation method is simple to operate, economical and environmentally friendly, has low environmental requirements, low production costs, and high equipment compatibility, making it suitable for large-scale promotion.

[0040] Optionally, the thickness of the alumina film 200 is 5 nm to 50 nm. This setting ensures the formation of a micro / nano structure 300 of sufficient thickness. In this embodiment, the alumina film 200 is prepared by atomic layer deposition. Atomic layer deposition allows for precise control of the thickness of the alumina film 200 and ensures that the formed alumina film 200 is sufficiently uniform.

[0041] Optionally, when boiling and drying the alumina film 200, the boiling temperature is set at 65℃-90℃ for 1 min-30 min, and the drying temperature is set at 85℃-120℃ for 10 min-20 min. After boiling, the alumina film 200 will undergo... The self-assembly reaction, followed by drying to remove moisture, ensures the formation of loose, porous, and disordered grass-like alumina by setting the above parameters.

[0042] The fabrication of aluminum-doped zinc oxide thin films 400 on micro / nano structures 300 includes:

[0043] S41. Pre-deposit aluminum precursor on micro / nano structure 300;

[0044] By pre-depositing an aluminum precursor, the doping efficiency of the bottom layer of the aluminum-doped zinc oxide thin film 400 can be improved.

[0045] S42. Aluminum-doped zinc oxide thin films 400 are grown by atomic layer deposition.

[0046] For example, the aluminum precursor is trimethylaluminum, and when depositing the aluminum-doped zinc oxide film 400, the zinc source is diethylzinc, and the oxygen source is water. Preferably, in this embodiment, trimethylaluminum and diethylzinc require multiple deposition cycles, with a cycle ratio of 16:1 or 29:1. Optionally, at the end of each deposition cycle, hydrogen gas is introduced into the chamber for plasma treatment. The plasma treatment time is 300 seconds, and the plasma power is 900 W. By setting the above parameters, the resulting aluminum-doped zinc oxide film 400 has high transmittance and low sheet resistance. Preferably, the thickness of the aluminum-doped zinc oxide film 400 is 150 nm.

[0047] Taking a D263T glass substrate as an example, the specific preparation of the aluminum-doped zinc oxide thin film 400 involves first depositing initial alumina thin films 200 with thicknesses of 5 nm, 10 nm, 20 nm, 35 nm, and 50 nm on the surface of the D263T glass substrate via atomic layer deposition. The initial alumina thin films 200 are then immersed in pure water at 65°C for 30 min and dried at 85°C for 20 min to obtain a D263T glass substrate with a surface covered by a grass-like alumina micro / nano structure 300. Next, the sample is placed in an ALD chamber for zinc oxide doping deposition. The deposition process is as follows: first, a cycle of trimethylaluminum is introduced, setting the zinc oxide to alumina doping ratio of 29:1, and deposition is repeated until the thickness of the aluminum-doped zinc oxide thin film 400 reaches 150 nm. Figure 2 As shown, Figure 2The graph shows the changes in sheet resistance and average transmittance of the aluminum-doped zinc oxide thin film 400 prepared on a D263T glass substrate through the above process. As can be seen from the graph, when the initial thickness of the aluminum oxide thin film 200 is 5 nm, the aluminum-doped zinc oxide thin film 400 has the highest average transmittance and the lowest sheet resistance.

[0048] Alternatively, first, an initial alumina film 200 with a thickness of 10 nm is deposited on the surface of a D263T glass substrate by atomic layer deposition. Then, the initial alumina film 200 is immersed in pure water at 65°C for 1 min, 2 min, 3 min, 4 min, 5 min, 6 min, 10 min, 20 min, 40 min, and 60 min, followed by drying at 85°C for 20 min to obtain a D263T glass substrate with a surface covered by a grass-like alumina micro / nano structure 300. Next, the sample is placed in an ALD chamber for the deposition of doped zinc oxide. The deposition process is as follows: first, a cycle of trimethylaluminum is introduced, and the doping ratio of zinc oxide to alumina is set to 16:1. Deposition is repeated until the thickness of the aluminum-doped zinc oxide reaches 150 nm. Figure 3 As shown, Figure 3 The graph shows the changes in sheet resistance and average transmittance of the aluminum-doped zinc oxide thin film 400 prepared on the D263T glass substrate through the above process. When the initial aluminum oxide thin film 200 is immersed in pure water for 60 minutes, the aluminum-doped zinc oxide thin film 400 has a higher average transmittance and the lowest sheet resistance.

[0049] Obviously, the above embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the implementation of the present invention. Those skilled in the art will be able to make various obvious changes, readjustments, and substitutions without departing from the scope of protection of the present invention. It is neither necessary nor possible to exhaustively describe all embodiments here. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the scope of protection of the claims of the present invention.

Claims

1. A method for preparing aluminum-doped zinc oxide thin films, characterized in that, include: Provide a substrate (100); An alumina thin film (200) is prepared on the substrate (100); The alumina film (200) was subjected to boiling and drying treatment to obtain a micro / nano structure (300); An aluminum-doped zinc oxide thin film (400) is prepared on the micro / nano structure (300); The preparation of the aluminum-doped zinc oxide thin film (400) on the micro / nano structure (300) includes: An aluminum precursor is pre-deposited on the micro / nano structure (300); The aluminum-doped zinc oxide thin film (400) was grown by atomic layer deposition. The aluminum precursor is trimethylaluminum, and when depositing the aluminum-doped zinc oxide thin film (400), the zinc source is diethylzinc and the oxygen source is water; The trimethylaluminum and the diethylzinc require multiple cyclic depositions; The recycling ratio of trimethylaluminum to diethylzinc is 16:1 or 29:1; When the alumina film (200) is subjected to boiling and drying treatment, the boiling temperature is set at 65℃-90℃ and the boiling time is 1min-30min. The drying temperature is 85℃-120℃ and the drying time is 10min-20min.

2. The method for preparing aluminum-doped zinc oxide thin films according to claim 1, characterized in that, The thickness of the alumina film (200) is 5nm-50nm.

3. The method for preparing aluminum-doped zinc oxide thin films according to claim 1, characterized in that, The alumina film (200) was prepared by atomic layer deposition.

4. The method for preparing aluminum-doped zinc oxide thin films according to claim 1, characterized in that, At the end of a single deposition cycle, hydrogen gas needs to be introduced into the chamber for plasma treatment. The plasma treatment time is 300 seconds and the plasma power is 900W.

5. The method for preparing aluminum-doped zinc oxide thin films according to claim 1, characterized in that, The thickness of the aluminum-doped zinc oxide thin film (400) is 150 nm.