CN114318264A - Method for preparing ITO film based on magnetron sputtering and etching treatment - Google Patents

Method for preparing ITO film based on magnetron sputtering and etching treatment Download PDF

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CN114318264A
CN114318264A CN202111635703.8A CN202111635703A CN114318264A CN 114318264 A CN114318264 A CN 114318264A CN 202111635703 A CN202111635703 A CN 202111635703A CN 114318264 A CN114318264 A CN 114318264A
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ito film
magnetron sputtering
ito
preparing
substrate
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陈桂林
章学堤
黄庆
许德
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Fujian Fulan Optics Co ltd
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Fujian Fulan Optics Co ltd
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Abstract

The invention provides a method for preparing an ITO film based on magnetron sputtering and etching treatment, which comprises the following steps: step S1, rotating the substrate, and cleaning the surface of the substrate through clean water; step S2, uniformly spin-coating polystyrene microspheres on the surface of the substrate; step S3, performing oxygen plasma etching operation on the polystyrene microsphere to improve the size of the polystyrene microsphere; s4, sputtering an ITO target on the surface of the substrate under a vacuum condition to form an ITO film, and depositing for a period of time; and step S5, placing the ITO film in a toluene solution for ultrasonic treatment, so as to etch the polystyrene microspheres, and finally obtaining the ITO film, thereby realizing the preparation of the ITO film.

Description

Method for preparing ITO film based on magnetron sputtering and etching treatment
Technical Field
The invention relates to the technical field of transparent conductive films, in particular to a method for preparing an ITO film based on magnetron sputtering and etching treatment.
Background
The transparent conductive film is a film which is transparent in a visible light range and has a conductive property, and has an important role in the fields of thin film solar cells, organic light emitting diodes, intelligent household appliances, automotive electronics and the like. Indium Tin Oxide (Indium Tin Oxide) film is a heavily doped, highly degenerate n-type semiconductor, abbreviated as ITO film. In 1968, after a film with excellent light transmission performance and conductivity is firstly prepared by Philip company, the material becomes the mainstream of the transparent conductive material. The indium tin oxide film has a series of unique properties, such as high visible light transmittance; the conductivity and the processing performance are good; the film layer has high hardness and is wear-resistant and chemical-corrosion-resistant. Therefore, the ITO thin film is still the most widely studied and applied transparent conductive thin film at present, and particularly, the required amount for use as a transparent electrode is rapidly increasing. With the rapid development of electronic technology, electronic devices and equipment are gradually moving toward portable, light and flexible deformation. As a base film of the flexible transparent conductive film, high light transmittance and conductivity are required, and good flexibility and mechanical strength are also required, but the ITO film prepared by the traditional process does not have the characteristics.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a high-quality ITO film with a porous structure by etching polystyrene microspheres in an ITO film grown by magnetron sputtering.
The invention is realized by adopting the following method: a method for preparing an ITO film based on magnetron sputtering and etching treatment comprises the following steps:
step S1, rotating the substrate, and cleaning the surface of the substrate through clean water;
step S2, uniformly spin-coating polystyrene microspheres on the surface of the substrate;
step S3, performing oxygen plasma etching operation on the polystyrene microsphere to improve the size of the polystyrene microsphere;
s4, sputtering an ITO target on the surface of the substrate under a vacuum condition to form an ITO film, and depositing for a period of time;
and step S5, placing the ITO film in a toluene solution for ultrasonic treatment, so as to etch the polystyrene microspheres, and finally obtaining the ITO film, thereby realizing the preparation of the ITO film.
Further, the substrate in step S1 is one of a molybdenum-plated film, a conductive glass, soda-lime glass, quartz glass, and a metal foil.
Further, the polystyrene purity of the polystyrene microsphere in the step S2 is 96-99.99%.
Further, the polystyrene microspheres in the step S2 are dissolved in deionized water, and the mass fraction is 2-20 ω t%.
Further, the etching power of the oxygen plasma etching in the step S3 is 30-150 w, and the etching time is 1-20 min.
Further, the ITO purity of the ITO target in the step S4 is 96-99.99%, and the deposition time is 5-60 min.
Further, the vacuum condition in the step S4 is 0.01-1 pa environment, and the sputtering power is 100-300 w.
Furthermore, the thickness of the ITO film is 10-500 nm.
Further, the ultrasonic power of the ultrasonic treatment in the step S5 is 50-200 w, and the ultrasonic time is 1-20 min.
The invention has the beneficial effects that: the invention provides a high-quality ITO film with high transmittance and strong tensile stress resistance prepared by magnetron sputtering, and the ITO film prepared by other processes does not have the characteristic of flexibility and stretchability; by spin-coating a layer of PS beads on a substrate, then magnetron sputtering an ITO precursor film in vacuum, and performing a preparation method of ultrasonically etching the PS beads in a toluene solution, the synthesized ITO film has strong tensile stress capability, good conductivity, simple manufacturing process, safety and nontoxicity, and can realize large-area production;
the magnetron sputtering preparation of the film has four advantages:
firstly, preparing an ITO precursor film by a magnetron sputtering method, wherein the thickness of the film is realized by controlling the reaction temperature and time;
secondly, the ITO precursor film is prepared by a magnetron sputtering method, the preparation process is finished in vacuum, the sputtering environment is stable, the phase is single, and the preparation of the high-quality film is facilitated;
thirdly, the ITO precursor film is prepared by the magnetron sputtering method, so that the difficulty of the operation process can be reduced, and the method is suitable for industrial large-scale preparation;
fourthly, the ITO precursor film is prepared by a magnetron sputtering method, toxic solvents and the like are not involved in the reaction, and the environmental pollution caused by the preparation process is reduced;
the etching process has two major advantages:
firstly, the size of the final ITO film porous structure can be controlled by adjusting the size of the PS pellets;
secondly, the PS globule ultrasonic etching process using toluene is simple and suitable for industrial large-scale preparation.
Drawings
FIG. 1 is a schematic flow chart of the method of the present invention.
FIG. 2 is a surface SEM photograph of PS beads prepared in example 1 of the present invention.
FIG. 3 is an SEM image of the surface of a flexible transparent conductive ITO thin film prepared in example 1 of the present invention.
FIG. 4 is a transmission spectrum of the flexible transparent conductive ITO thin film prepared in example 1 of the present invention.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
Referring to fig. 1, the present invention provides a method for preparing an ITO thin film based on magnetron sputtering and etching processes, the method comprising the following steps:
step S1, rotating the substrate, and cleaning the surface of the substrate through clean water;
step S2, uniformly spin-coating polystyrene microspheres on the surface of the substrate;
step S3, performing oxygen plasma etching operation on the polystyrene microsphere to improve the size of the polystyrene microsphere;
s4, sputtering an ITO target on the surface of the substrate under a vacuum condition to form an ITO film, and depositing for a period of time;
and step S5, placing the ITO film in a toluene solution for ultrasonic treatment, so as to etch the polystyrene microspheres, and finally obtaining the ITO film, thereby realizing the preparation of the ITO film.
The invention is further illustrated by the following specific examples:
example 1 (please refer to FIG. 2)
1. Firstly, cleaning a glass substrate: sequentially immersing the glass substrate into a detergent, deionized water, ethanol and acetone solution, cleaning in a plasma cleaning machine, and drying by nitrogen;
2. placing the cleaned glass substrate on a spin coater, and spin-coating PS pellets with the mass fraction of 10 omega t% on the glass substrate at 2500r/min for 15 s;
3. placing the substrate coated with the layer of PS pellets in plasma etching equipment, and etching for 2min at a power of 60 w;
4. placing the processed substrate in a magnetron sputtering working chamber, and vacuumizing the background of a sputtering system to be less than 5.0pa by using a magnetron sputtering coating system;
5. bombarding the target material by sputtering gas Ar of a magnetron sputtering coating machine,
the sputtering gas is argon with the purity of 99.9 percent;
the target material is an ITO target with the purity of 99.8 percent;
the working air pressure in the magnetron sputtering working chamber is 0-0.2 pa;
6. the setting parameters are as follows: power: 200W; oxygen flow rate: 60 sccm; argon flow: 60 sccm; deposition time: the thickness of the obtained ITO film is 80nm after 10 min;
7. placing the ITO precursor film obtained in the step 6 in a toluene solution, performing ultrasonic treatment for 2min in an ultrasonic machine at a power of 60w, and etching the PS pellets to finally obtain a flexible stretchable transparent conductive ITO film;
the transmission spectrum test of the flexible stretchable transparent conductive ITO film prepared in this example is performed, as shown in fig. 4, which is a transmission spectrum of the flexible stretchable transparent conductive ITO film prepared in this example, and as can be seen from fig. 4, the film has excellent transmittance.
Example 2
1. Firstly, cleaning a glass substrate: sequentially immersing the glass substrate into a detergent, deionized water, ethanol and acetone solution, cleaning in a plasma cleaning machine, and drying by nitrogen;
2. placing the cleaned glass substrate on a spin coater, and spin-coating PS pellets with the mass fraction of 10 omega t% on the glass substrate at 2500r/min for 15 s;
3. placing the substrate coated with the layer of PS pellets in plasma etching equipment, and etching for 1min at a power of 60 w;
4. placing the processed substrate in a magnetron sputtering working chamber, and vacuumizing the background of a sputtering system to be less than 5.0pa by using a magnetron sputtering coating system;
5. bombarding the target material by sputtering gas Ar of a magnetron sputtering coating machine,
the sputtering gas is argon with the purity of 99.9 percent;
the target material is an ITO target with the purity of 99.8 percent;
the working air pressure in the magnetron sputtering working chamber is 0-0.2 pa;
6. the setting parameters are as follows: power: 200W; oxygen flow rate: 60 sccm; argon flow: 60 sccm; deposition time: 20min, the thickness of the obtained ITO film is 160 nm;
7. placing the ITO precursor film obtained in the step 6 in a toluene solution, performing ultrasonic treatment for 2min in an ultrasonic machine at a power of 60w, and etching the PS pellets to finally obtain a flexible stretchable transparent conductive ITO film;
example 3
1. Firstly, cleaning a glass substrate: sequentially immersing the glass substrate into a detergent, deionized water, ethanol and acetone solution, cleaning in a plasma cleaning machine, and drying by nitrogen;
2. placing the cleaned glass substrate on a spin coater, and spin-coating PS pellets with the mass fraction of 10 omega t% on the glass substrate at 2500r/min for 15 s;
3. placing the substrate coated with the layer of PS pellets in plasma etching equipment, and etching for 3min at a power of 60 w;
4. placing the processed substrate in a magnetron sputtering working chamber, and vacuumizing the background of a sputtering system to be less than 5.0pa by using a magnetron sputtering coating system;
5. bombarding the target material by sputtering gas Ar of a magnetron sputtering coating machine,
the sputtering gas is argon with the purity of 99.9 percent;
the target material is an ITO target with the purity of 99.8 percent;
the working air pressure in the magnetron sputtering working chamber is 0-0.2 pa;
6. the setting parameters are as follows: power: 200W; oxygen flow rate: 60 sccm; argon flow: 60 sccm; deposition time: 20min, the thickness of the obtained ITO film is 160 nm;
7. placing the ITO precursor film obtained in the step 6 in a toluene solution, performing ultrasonic treatment for 2min in an ultrasonic machine at a power of 60w, and etching the PS pellets to finally obtain a flexible stretchable transparent conductive ITO film;
in the three examples, the magnetron sputtering apparatus involved was prepared: the purity of the target material is 99.8%; the PS pellets are purchased from Mackexin, the toluene solution is purchased from Chinese medicine, and the molybdenum-plated glass and the soda-lime glass related to the substrate are purchased from new material science and technology (Ningbo) Inc. of Shengyang and Luoyang Longyao glass Inc. respectively.
In the above embodiment example 1, SEM image of the ITO thin film prepared is shown in FIG. 3. It is noted that the test results of examples 2 and 3 are similar to example 1.
The PS pellets involved in the invention are purchased from Mackexin, and the toluene solution is purchased from Chinese medicines. The molybdenum-plated glass and the soda-lime glass related to the substrate are respectively purchased from new sun-generating material science and technology (Ningbo) and Luoyang Longyao glass, and the PS pellets are polystyrene microspheres.
In a word, the magnetron sputtering is used for introducing a magnetic field on the surface of an ITO target, the plasma density and the sputtering rate of a sputtered film are improved by utilizing the constraint of the magnetic field on charged particles, the ITO film is directly deposited, and the subsequent phase forming process is avoided; and placing the obtained ITO precursor film in a toluene solution to perform ultrasonic etching on the PS pellets by utilizing the characteristic that the PS pellets are dissolved in the toluene.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.

Claims (9)

1. A method for preparing an ITO film based on magnetron sputtering and etching treatment is characterized by comprising the following steps:
step S1, rotating the substrate, and cleaning the surface of the substrate through clean water;
step S2, uniformly spin-coating polystyrene microspheres on the surface of the substrate;
step S3, performing oxygen plasma etching operation on the polystyrene microsphere to improve the size of the polystyrene microsphere;
s4, sputtering an ITO target on the surface of the substrate under a vacuum condition to form an ITO film, and depositing for a period of time;
and step S5, placing the ITO film in a toluene solution for ultrasonic treatment, so as to etch the polystyrene microspheres, and finally obtaining the ITO film, thereby realizing the preparation of the ITO film.
2. The method for preparing the ITO film based on magnetron sputtering and etching treatment according to claim 1, wherein the method comprises the following steps: the substrate in the step S1 is one of a molybdenum-plated film, conductive glass, soda-lime glass, quartz glass, and metal foil.
3. The method for preparing the ITO film based on magnetron sputtering and etching treatment according to claim 1, wherein the method comprises the following steps: the polystyrene purity of the polystyrene microspheres in the step S2 is 96-99.99%.
4. The method for preparing the ITO film based on magnetron sputtering and etching treatment according to claim 1, wherein the method comprises the following steps: and (3) dissolving the polystyrene microspheres in the step S2 in deionized water, wherein the mass fraction is 2-20 omega t%.
5. The method for preparing the ITO film based on magnetron sputtering and etching treatment according to claim 1, wherein the method comprises the following steps: the etching power of the oxygen plasma etching in the step S3 is 30-150 w, and the etching time is 1-20 min.
6. The method for preparing the ITO film based on magnetron sputtering and etching treatment according to claim 1, wherein the method comprises the following steps: the ITO purity of the ITO target in the step S4 is 96-99.99%, and the deposition time is 5-60 min.
7. The method for preparing the ITO film based on magnetron sputtering and etching treatment according to claim 1, wherein the method comprises the following steps: the vacuum condition in the step S4 is 0.01-1 pa environment, and the sputtering power is 100-300 w.
8. The method for preparing the ITO film based on magnetron sputtering and etching treatment according to claim 1, wherein the method comprises the following steps: the thickness of the ITO film is 10-500 nm.
9. The method for preparing the ITO film based on magnetron sputtering and etching treatment according to claim 1, wherein the method comprises the following steps: the ultrasonic power of the ultrasonic treatment in the step S5 is 50-200 w, and the ultrasonic time is 1-20 min.
CN202111635703.8A 2021-12-29 2021-12-29 Method for preparing ITO film based on magnetron sputtering and etching treatment Pending CN114318264A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115613352A (en) * 2022-10-10 2023-01-17 余翔 Breathable down-proof fabric and preparation method thereof

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CN107910383A (en) * 2017-10-09 2018-04-13 华南师范大学 A kind of preparation method of metal net shaped conducting film
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050224779A1 (en) * 2003-12-11 2005-10-13 Wang Zhong L Large scale patterned growth of aligned one-dimensional nanostructures
CN101246911A (en) * 2008-03-10 2008-08-20 北京航空航天大学 Metal microgrid transparent electrode and method for producing the same
CN101435110A (en) * 2008-12-04 2009-05-20 哈尔滨工业大学 Preparation of germanium three-dimensional photonic crystal
JP2013102064A (en) * 2011-11-09 2013-05-23 Toray Ind Inc Thin-film solar cell substrate
US20180066131A1 (en) * 2016-09-05 2018-03-08 NanoSD Inc. Polymer nanoparticle thermal insulators
CN106835012A (en) * 2016-12-21 2017-06-13 蚌埠玻璃工业设计研究院 A kind of preparation method of matte aluminum-doped zinc oxide films
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