CN113871061A - Conductive film, and preparation method and application thereof - Google Patents

Conductive film, and preparation method and application thereof Download PDF

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Publication number
CN113871061A
CN113871061A CN202111217303.5A CN202111217303A CN113871061A CN 113871061 A CN113871061 A CN 113871061A CN 202111217303 A CN202111217303 A CN 202111217303A CN 113871061 A CN113871061 A CN 113871061A
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layer
silicon dioxide
dioxide layer
conductive film
thickness
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CN202111217303.5A
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Inventor
胡业新
于佩强
吕敬波
刘世琴
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Jiangsu Rijiu Optoelectronics Joint Stock Co ltd
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Jiangsu Rijiu Optoelectronics Joint Stock Co ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/14Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables

Abstract

The invention discloses a conductive film and a preparation method and application thereof. The conductive film comprises a substrate layer, a first silicon dioxide layer, a first indium tin oxide layer, a second silicon dioxide layer and a second indium tin oxide layer which are sequentially stacked; wherein the first silicon dioxide layer and the second silicon dioxide layer have different thicknesses. The conductive film provided by the invention has the base material layer, the first silicon dioxide layer, the first indium tin oxide layer, the second silicon dioxide layer and the second indium tin oxide layer which are sequentially stacked, and the thicknesses of the first silicon dioxide layer and the second silicon dioxide layer are different, so that the conductive film has very low reflectivity and can effectively reduce chromatic aberration.

Description

Conductive film, and preparation method and application thereof
Technical Field
The invention relates to the technical field of conducting films, in particular to a low-reflection ITO conducting film and a preparation method and application thereof.
Background
Indium Tin Oxide (ITO) is an In oxide doped with Sn, and crystalline ITO has a low resistivity and a high transmittance, and is widely used for preparing transparent conductive films applied to the fields of flat panel displays, touch screens, solar cells, and the like. However, the existing SiO2Layer and ITO layer composite conductive film reflectiveIs relatively high, resulting in high color difference of the conductive film even if SiO is increased2The layer thickness also does not improve enough the color difference.
Therefore, in view of the above technical problems, it is necessary to provide a new conductive film.
Disclosure of Invention
The invention aims to provide a conductive film which has a very low reflectance and can effectively reduce chromatic aberration of the conductive film.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
in a first aspect, the present invention provides a conductive film, which includes a substrate layer, a first silicon dioxide layer, a first indium tin oxide layer, a second silicon dioxide layer, and a second indium tin oxide layer, which are sequentially stacked; wherein the first silicon dioxide layer and the second silicon dioxide layer have different thicknesses.
In one or more embodiments of the present invention, the thickness of the first silicon dioxide layer is less than the thickness of the second silicon dioxide layer.
In one or more embodiments of the present invention, the first silicon dioxide layer has a thickness of 10 to 15nm, and the second silicon dioxide layer has a thickness of 5 to 12 nm.
In one or more embodiments of the present invention, the first ito layer has a thickness of 5 to 25nm, and the second ito layer has a thickness of 5 to 28 nm.
In one or more embodiments of the invention, the first and second layers of indium tin oxide have crystalline therein.
In one or more embodiments of the present invention, the substrate layer is a transparent high molecular polymer film.
In one or more embodiments of the present invention, the transparent high molecular polymer is selected from one or more of PET, COP, PI, PC, PMMA, PP and PE.
In one or more embodiments of the present invention, the thickness of the substrate layer is 5.7 to 188 μm.
In a second aspect, the present invention provides a use of the conductive film as described above in a display or a touch screen.
In a third aspect, the present invention provides a method for manufacturing a conductive film, including:
forming a first silicon dioxide layer on the substrate layer;
forming a first ITO layer on the first silicon dioxide layer;
forming a second silicon dioxide layer on the first indium tin oxide layer;
forming a second indium tin oxide layer on the second silicon dioxide layer to obtain a laminated body;
carrying out heat treatment on the laminated body at the temperature of 110-150 ℃ for 30-50 min to obtain a conductive film;
wherein the first silicon dioxide layer and the second silicon dioxide layer have different thicknesses.
Compared with the prior art, the conductive film provided by the invention has the base material layer, the first silicon dioxide layer, the first indium tin oxide layer, the second silicon dioxide layer and the second indium tin oxide layer which are sequentially stacked, and the thicknesses of the first silicon dioxide layer and the second silicon dioxide layer are different, so that the conductive film has very low reflectivity and can effectively reduce chromatic aberration.
Drawings
FIG. 1 is a schematic structural diagram of a conductive film according to an embodiment of the invention;
FIG. 2 is a graph showing the reflectance test of the conductive film obtained in example 1 of the present invention;
FIG. 3 is a graph showing the reflectance test of the conductive film obtained in example 2 of the present invention;
FIG. 4 is a graph showing the reflectance test of the conductive film obtained in example 3 of the present invention;
FIG. 5 is a graph showing the reflectance test of the conductive film obtained in example 4 of the present invention;
FIG. 6 is a graph showing a reflectance test of a conductive film obtained in comparative example 1 of the present invention;
FIG. 7 is a graph showing a reflectance test of a conductive film obtained in comparative example 2 of the present invention;
FIG. 8 is a graph showing the reflectance test of the conductive film obtained in example 3 of the present invention.
Description of the main reference numerals:
1-a substrate layer, 2-a first silicon dioxide layer, 3-a first indium tin oxide layer, 4-a second silicon dioxide layer, and 5-a second indium tin oxide layer.
Detailed Description
The following detailed description of the present invention is provided in conjunction with the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
As shown in fig. 1, the conductive film according to an embodiment of the present invention can be applied to the fields of displays, touch panels, and the like. The conductive film comprises a substrate layer 1, a first silicon dioxide layer 2, a first indium tin oxide layer 3, a second silicon dioxide layer 4 and a second indium tin oxide layer 5 which are sequentially stacked; wherein the first silicon dioxide layer 2 and the second silicon dioxide layer 4 have different thicknesses.
In an exemplary embodiment, the thickness of the first silicon dioxide layer 2 is less than the thickness of the second silicon dioxide layer 4. Wherein, the thickness of the first silicon dioxide layer 2 is 10-15 nm, and the thickness of the second silicon dioxide layer 4 is 5-12 nm. For example, the thickness of the first silicon dioxide layer 2 may be 10nm, 10.5nm, 11.22nm, 12nm, 15nm, or any other dimension between 10nm and 15 nm; the thickness of the second silicon dioxide layer 4 can be 5nm, 6.6nm, 8nm, 10nm, 12nm and other arbitrary sizes between 5nm and 12 nm.
In an exemplary embodiment, the thickness of the first ITO layer 3 is 5-25 nm, and the thickness of the second ITO layer 5 is 5-28 nm. The first ito layer 3 and the second ito layer 5 have crystals formed by crystallizing the first ito layer 3 and the second ito layer 5 after heat treatment.
In an exemplary embodiment, the substrate layer 1 is preferably a transparent high molecular polymer film. The thickness of the base material layer 1 is preferably 5.7 to 188 μm. The transparent high molecular polymer of the present invention is not particularly limited, and for example, the transparent high molecular polymer may be one or more selected from PET (polyethylene terephthalate), COP (cycloolefin polymer), PI (polyimide), PC (polycarbonate), PMMA (polymethyl methacrylate), PP (polypropylene), and PE (polyethylene).
The invention also provides a preparation method of the conductive film, which comprises the following steps:
s1: forming a first silicon dioxide layer 2 on the substrate layer 1;
s2: forming a first ito layer 3 on the first sio layer 2;
s3: forming a second silicon dioxide layer 4 on the first ito layer 3;
s4: forming a second indium tin oxide layer 5 on the second silicon dioxide layer 4 to obtain a laminated body;
s5: and carrying out heat treatment on the laminated body at the temperature of 110-150 ℃ for 30-50 min to obtain the conductive film.
Wherein the first silicon dioxide layer 2 and the second silicon dioxide layer 4 have different thicknesses.
The surface of the base material layer 1 may be subjected to etching treatment such as sputtering, corona discharge, flame, ultraviolet irradiation, electron beam irradiation, chemical conversion, or oxidation, or undercoating treatment in advance, so as to improve the adhesion between the base material layer 1 and the layer structure formed on the surface thereof. Before forming another layer structure on the base material layer 1, the surface of the base material layer 1 may be subjected to dust removal and cleaning treatment by solvent cleaning, ultrasonic cleaning, or the like as needed.
In the present invention, the method of forming the first silicon dioxide layer 2 and the second silicon dioxide layer 4 in the conductive film is not particularly limited, and a conventionally known method can be used. For example, magnetron sputtering, ion beam sputtering, chemical vapor deposition, thermal oxidation, gel-sol method, or the like can be used.
In the present invention, the method of forming the first ito layer 3 and the second ito layer 5 in the conductive film is not particularly limited, and a conventionally known method can be used. For example, a vacuum deposition method, a sputtering method, an ion plating method, or the like may be used. In addition, an appropriate method may be adopted according to the desired film thickness.
When a plastic film is used as the base layer 1 and the first indium tin oxide layer 3 and the second indium tin oxide layer 5 are formed by a sputtering method, it is impossible to perform sputtering film formation at a high temperature in consideration of the heat resistance of the base layer 1. Therefore, the first ito layer 3 and the second ito layer 5 immediately after film formation are mostly amorphous films (sometimes partially crystallized). These amorphous transparent conductive films have a lower transmittance than crystalline films, and may have a problem of a large resistance change after a humidification heating test.
Therefore, after the first ito layer 3 and the second ito layer 5 are formed to be amorphous, they may be converted into a crystalline film by performing heat treatment in an atmosphere in which oxygen is present. Generally, the first ITO layer 3 and the second ITO layer 5, which are amorphous, can be converted into crystalline films by heat treatment at a temperature of 110-150 ℃ for about 30-50 min. By crystallizing the first ito layer 3 and the second ito layer 5, the transparency can be improved, the resistance can be reduced, and the resistance change after the humidification heating test is small, and the humidification heating reliability can be improved.
The invention is further illustrated by the following specific examples and comparative examples:
example 1
In a chamber of a vacuum magnetron sputtering device, a first silicon dioxide layer 2 with the thickness of 12nm is formed on one surface of a PET substrate layer 1 with the thickness of 50 μm in a sputtering mode, a first indium tin oxide layer 3 with the thickness of 11nm is formed on the first silicon dioxide layer 2 in a sputtering mode, a second silicon dioxide layer 4 with the thickness of 8nm is formed on the first indium tin oxide layer 3 in a sputtering mode, and a second indium tin oxide layer 5 with the thickness of 11nm is formed on the second silicon dioxide layer 4 in a sputtering mode to obtain a laminated body.
Wherein the reaction vacuum degree in the chamber of the vacuum magnetron sputtering equipment is 0.5Pa, the ratio of argon to oxygen is 100:1, and the first sputtering is carried outSiO in the case of silicon dioxide layer 22The sputtering power of the target material is 12.5kW, and SiO is generated when the second silicon dioxide layer 4 is sputtered2The sputtering power of the target material is 8.5kW, and the sputtering power of the ITO target material is 5.1kW when the first ITO layer 3 and the second ITO layer 5 are sputtered.
And taking out the laminated body from a chamber of vacuum magnetron sputtering equipment, and carrying out heat treatment for 40min at the temperature of 130 ℃ to obtain the conductive film. The reflectance test chart of the conductive film obtained in this example is shown in FIG. 2 (in the figure, the abscissa is the wavelength (nm) and the ordinate is the reflectance (%)).
Example 2
In a chamber of a vacuum magnetron sputtering device, a first silicon dioxide layer 2 with the thickness of 10nm is formed on one surface of a PET substrate layer 1 with the thickness of 5.7 mu m in a sputtering mode, a first indium tin oxide layer 3 with the thickness of 11nm is formed on the first silicon dioxide layer 2 in a sputtering mode, a second silicon dioxide layer 4 with the thickness of 5nm is formed on the first indium tin oxide layer 3 in a sputtering mode, and a second indium tin oxide layer 5 with the thickness of 11nm is formed on the second silicon dioxide layer 4 in a sputtering mode to obtain a laminated body.
Wherein the reaction vacuum degree in the chamber of the vacuum magnetron sputtering equipment is 0.5Pa, the ratio of argon to oxygen is 100:1, and SiO is generated when the first silicon dioxide layer 2 is sputtered2The sputtering power of the target material is 10.5kW, and SiO is generated when the second silicon dioxide layer 4 is sputtered2The sputtering power of the target material is 5.3kW, and the sputtering power of the ITO target material is 5.1kW when the first ITO layer 3 and the second ITO layer 5 are sputtered.
And taking out the laminated body from a chamber of vacuum magnetron sputtering equipment, and carrying out heat treatment for 40min at the temperature of 130 ℃ to obtain the conductive film. The reflectance test chart of the conductive film obtained in this example is shown in FIG. 3 (in the figure, the abscissa is the wavelength (nm) and the ordinate is the reflectance (%)).
Example 3
In a chamber of a vacuum magnetron sputtering device, a first silicon dioxide layer 2 with the thickness of 15nm is formed on one surface of a PET substrate layer 1 with the thickness of 188 mu m in a sputtering mode, a first indium tin oxide layer 3 with the thickness of 11nm is formed on the first silicon dioxide layer 2 in a sputtering mode, a second silicon dioxide layer 4 with the thickness of 12nm is formed on the first indium tin oxide layer 3 in a sputtering mode, and a second indium tin oxide layer 5 with the thickness of 11nm is formed on the second silicon dioxide layer 4 in a sputtering mode to obtain a laminated body.
Wherein the reaction vacuum degree in the chamber of the vacuum magnetron sputtering equipment is 0.5Pa, the ratio of argon to oxygen is 100:1, and SiO is generated when the first silicon dioxide layer 2 is sputtered2The sputtering power of the target material is 16kW, and SiO is formed when the second silicon dioxide layer 4 is sputtered2The sputtering power of the target was 12.5kW, and the sputtering power of the ITO target was 5.1kW when the first ITO layer 3 and the second ITO layer 5 were sputtered.
And taking out the laminated body from a chamber of vacuum magnetron sputtering equipment, and carrying out heat treatment for 40min at the temperature of 130 ℃ to obtain the conductive film. The reflectance test chart of the conductive film obtained in this example is shown in FIG. 4 (in the figure, the abscissa is the wavelength (nm) and the ordinate is the reflectance (%)).
Example 4
In a chamber of a vacuum magnetron sputtering device, a first silicon dioxide layer 2 with the thickness of 12nm is formed on one surface of a PET substrate layer 1 with the thickness of 50 μm in a sputtering mode, a first indium tin oxide layer 3 with the thickness of 5nm is formed on the first silicon dioxide layer 2 in a sputtering mode, a second silicon dioxide layer 4 with the thickness of 8nm is formed on the first indium tin oxide layer 3 in a sputtering mode, and a second indium tin oxide layer 5 with the thickness of 5nm is formed on the second silicon dioxide layer 4 in a sputtering mode to obtain a laminated body.
Wherein the reaction vacuum degree in the chamber of the vacuum magnetron sputtering equipment is 0.5Pa, the ratio of argon to oxygen is 100:1, and SiO is generated when the first silicon dioxide layer 2 is sputtered2The sputtering power of the target material is 12.5kW, and SiO is generated when the second silicon dioxide layer 4 is sputtered2The sputtering power of the target material is 8.5kW, and the sputtering power of the ITO target material is 2.3kW when the first ITO layer 3 and the second ITO layer 5 are sputtered.
And taking out the laminated body from a chamber of vacuum magnetron sputtering equipment, and carrying out heat treatment for 40min at the temperature of 130 ℃ to obtain the conductive film. The reflectance test chart of the conductive film obtained in this example is shown in FIG. 5 (in the figure, the abscissa is the wavelength (nm) and the ordinate is the reflectance (%)).
Example 5
In this example, the ratio of argon gas to oxygen gas in the chamber of the vacuum magnetron sputtering apparatus was adjusted to 100:0.8 as compared with example 1, and the other conditions were the same as in example 1.
Example 6
Compared with example 1, the ratio of argon to oxygen in the chamber of the vacuum magnetron sputtering apparatus in this example was adjusted to 100:1.2, and the other conditions were the same as example 1.
Example 7
In this example, the thickness of the second silicon oxide layer 4 was adjusted to 13nm as compared with example 1, and the other conditions were the same as example 1.
Comparative example 1
In a chamber of a vacuum magnetron sputtering device, a first silicon dioxide layer 2 with the thickness of 12nm is formed on one surface of a PET substrate layer 1 with the thickness of 50 μm in a sputtering mode, a first indium tin oxide layer 3 with the thickness of 11nm is formed on the first silicon dioxide layer 2 in a sputtering mode, and a second silicon dioxide layer 4 with the thickness of 8nm is formed on the first indium tin oxide layer 3 in a sputtering mode, so that a laminated body is obtained.
Wherein the reaction vacuum degree in the chamber of the vacuum magnetron sputtering equipment is 0.5Pa, the ratio of argon to oxygen is 100:1, and SiO is generated when the first silicon dioxide layer 2 is sputtered2The sputtering power of the target material is 12.5kW, and SiO is generated when the second silicon dioxide layer 4 is sputtered2The sputtering power of the target was 8.5kW, and the sputtering power of the ITO target was 5.1kW when the first ITO layer 3 was sputtered.
And taking out the laminated body from a chamber of vacuum magnetron sputtering equipment, and carrying out heat treatment for 40min at the temperature of 130 ℃ to obtain the conductive film. The reflectance test chart of the conductive film obtained in this example is shown in FIG. 6 (in the figure, the abscissa is the wavelength (nm) and the ordinate is the reflectance (%)).
Comparative example 2
In a chamber of a vacuum magnetron sputtering device, a first silicon dioxide layer 2 with the thickness of 12nm is formed on one surface of a PET substrate layer 1 with the thickness of 50 μm in a sputtering mode, a first indium tin oxide layer 3 with the thickness of 11nm is formed on the first silicon dioxide layer 2 in a sputtering mode, and a second silicon dioxide layer 4 with the thickness of 19nm is formed on the first indium tin oxide layer 3 in a sputtering mode, so that a laminated body is obtained.
Wherein the reaction vacuum degree in the chamber of the vacuum magnetron sputtering equipment is 0.5Pa, the ratio of argon to oxygen is 100:1, and SiO is generated when the first silicon dioxide layer 2 is sputtered2The sputtering power of the target material is 12.5kW, and SiO is generated when the second silicon dioxide layer 4 is sputtered2The sputtering power of the target was 8.5kW, and the sputtering power of the ITO target was 5.1kW when the first ITO layer 3 was sputtered.
And taking out the laminated body from a chamber of vacuum magnetron sputtering equipment, and carrying out heat treatment for 40min at the temperature of 130 ℃ to obtain the conductive film. The reflectance test chart of the conductive film obtained in this example is shown in FIG. 7 (in the figure, the abscissa is the wavelength (nm) and the ordinate is the reflectance (%)).
Comparative example 3
In a chamber of a vacuum magnetron sputtering device, a first silicon dioxide layer 2 with the thickness of 12nm is formed on one surface of a PET substrate layer 1 with the thickness of 50 microns in a sputtering mode, a first indium tin oxide layer 3 with the thickness of 11nm is formed on the first silicon dioxide layer 2 in a sputtering mode, a metal silicon layer with the thickness of 8nm is formed on the first indium tin oxide layer 3 in a sputtering mode, and a second indium tin oxide layer 5 with the thickness of 11nm is formed on the metal silicon layer in a sputtering mode to obtain a laminated body.
Wherein the reaction vacuum degree in the chamber of the vacuum magnetron sputtering equipment is 0.5Pa, the ratio of argon to oxygen is 100:1, and SiO is generated when the first silicon dioxide layer 2 is sputtered2The sputtering power of the target material is 12.5kW, and SiO is generated when the metal silicon layer is sputtered2The sputtering power of the target material is 8.5kW, and the sputtering power of the ITO target material is 5.1kW when the first ITO layer 3 and the second ITO layer 5 are sputtered.
And taking out the laminated body from a chamber of vacuum magnetron sputtering equipment, and carrying out heat treatment for 40min at the temperature of 130 ℃ to obtain the conductive film. The reflectance test chart of the conductive film obtained in this example is shown in FIG. 8 (in the figure, the abscissa is the wavelength (nm) and the ordinate is the reflectance (%)).
Performance testing
The sheet resistance and crystallinity of the conductive films obtained in examples 1, 5, 6 and 7 were tested, and the test results are shown in the following table:
square resistance (omega) Crystallinity of the compound
Example 1 118Ω Good crystallization property
Example 5 124Ω Good crystallization property
Example 6 115Ω Good crystallization property
Example 7 102Ω Good crystallization property
Referring to fig. 2 to 8, it can be seen that the conductive film manufactured by the technical scheme of the present invention can effectively reduce the emissivity by combining the examples and the comparative examples.
In summary, the conductive film provided by the invention has very low reflectivity and can effectively reduce chromatic aberration.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.

Claims (10)

1. The conducting film is characterized by comprising a substrate layer, a first silicon dioxide layer, a first indium tin oxide layer, a second silicon dioxide layer and a second indium tin oxide layer which are sequentially stacked;
wherein the first silicon dioxide layer and the second silicon dioxide layer have different thicknesses.
2. The conductive film of claim 1, wherein a thickness of the first silicon dioxide layer is less than a thickness of the second silicon dioxide layer.
3. The conductive film according to claim 2, wherein the first silicon dioxide layer has a thickness of 10 to 15nm, and the second silicon dioxide layer has a thickness of 5 to 12 nm.
4. The conductive film according to claim 1, wherein the first ITO layer has a thickness of 5 to 25nm, and the second ITO layer has a thickness of 5 to 28 nm.
5. The conductive film of claim 4, wherein the first indium tin oxide layer and the second indium tin oxide layer have crystalline therein.
6. The conductive film according to claim 1, wherein the substrate layer is a transparent high molecular polymer film.
7. The conductive film according to claim 6, wherein the transparent high molecular polymer is selected from one or more of PET, COP, PI, PC, PMMA, PP, and PE.
8. The conductive film according to claim 6, wherein the substrate layer has a thickness of 5.7 to 188 μm.
9. Use of the conductive film according to any one of claims 1 to 8 in a display or touch screen.
10. A method for producing a conductive film, comprising:
forming a first silicon dioxide layer on the substrate layer;
forming a first ITO layer on the first silicon dioxide layer;
forming a second silicon dioxide layer on the first indium tin oxide layer;
forming a second indium tin oxide layer on the second silicon dioxide layer to obtain a laminated body;
carrying out heat treatment on the laminated body at the temperature of 110-150 ℃ for 30-50 min to obtain a conductive film;
wherein the first silicon dioxide layer and the second silicon dioxide layer have different thicknesses.
CN202111217303.5A 2021-10-19 2021-10-19 Conductive film, and preparation method and application thereof Pending CN113871061A (en)

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CN202111217303.5A CN113871061A (en) 2021-10-19 2021-10-19 Conductive film, and preparation method and application thereof

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Application Number Priority Date Filing Date Title
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Publication Number Publication Date
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