CN117275830B - Preparation method of capacitive touch screen ITO film - Google Patents

Preparation method of capacitive touch screen ITO film Download PDF

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Publication number
CN117275830B
CN117275830B CN202311132140.XA CN202311132140A CN117275830B CN 117275830 B CN117275830 B CN 117275830B CN 202311132140 A CN202311132140 A CN 202311132140A CN 117275830 B CN117275830 B CN 117275830B
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methylimidazole
carbon nano
touch screen
capacitive touch
ito film
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CN117275830A (en
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龙文
易国安
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Lengshuijiang Jingke Electronic Technology Co ltd
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Lengshuijiang Jingke Electronic Technology Co ltd
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    • 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
    • GPHYSICS
    • G06COMPUTING; CALCULATING OR COUNTING
    • G06FELECTRIC DIGITAL DATA PROCESSING
    • G06F3/00Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
    • G06F3/01Input arrangements or combined input and output arrangements for interaction between user and computer
    • G06F3/03Arrangements for converting the position or the displacement of a member into a coded form
    • G06F3/041Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
    • G06F3/044Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means by capacitive means
    • 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
    • GPHYSICS
    • G06COMPUTING; CALCULATING OR COUNTING
    • G06FELECTRIC DIGITAL DATA PROCESSING
    • G06F2203/00Indexing scheme relating to G06F3/00 - G06F3/048
    • G06F2203/041Indexing scheme relating to G06F3/041 - G06F3/045
    • G06F2203/04103Manufacturing, i.e. details related to manufacturing processes specially suited for touch sensitive devices

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  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • Theoretical Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Human Computer Interaction (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing Of Electric Cables (AREA)
  • Non-Insulated Conductors (AREA)

Abstract

The invention relates to the technical field of ITO film preparation, in particular to a preparation method of a capacitive touch screen ITO film, which comprises the steps of firstly preparing a carbon nano tube film, then immersing the carbon nano tube film in ITO sol, taking out, drying and heat treating.

Description

Preparation method of capacitive touch screen ITO film
Technical Field
The invention relates to the technical field of ITO film preparation, in particular to a preparation method of a capacitive touch screen ITO film.
Background
ITO thin films have been widely used as a transparent conductive thin film having excellent properties in various fields of electronics, electricity, information and optics, such as electrodes of flat panel displays, anti-fog heating films for window glass, energy-saving infrared reflection films, electrodes of solar cells, selective projection films for solar heat, and optical wave selectors, protective coatings, gas sensors, etc., but ITO thin films have been limited in application due to their poor flexibility.
Disclosure of Invention
The invention aims to: aiming at the technical problems, the invention provides a preparation method of an ITO film of a capacitive touch screen.
The technical scheme adopted is as follows:
a preparation method of a capacitive touch screen ITO film comprises the following steps: firstly preparing a carbon nano tube film, then soaking the carbon nano tube film in ITO sol, taking out, and then drying and heat treating.
Further, the preparation method of the capacitive touch screen ITO film comprises the following specific steps:
s1: preparing ITO sol by taking indium salt, tin salt, ethanolamine, 4-dimethylaminopyridine and a solvent as raw materials;
s2: mixing carbon nano tubes, a dispersing agent and water, performing ultrasonic dispersion, centrifuging, taking supernatant, adding an ionic liquid and a conductive polymer to obtain carbon nano tube dispersion liquid, spraying the carbon nano tube dispersion liquid on a substrate by using a spraying method, wherein the temperature of the substrate is 105-120 ℃, and removing a formed carbon nano tube film from the substrate;
s3: immersing and pulling the carbon nano tube film in ITO sol for several times, taking out and drying, and then performing heat treatment at 400-420 ℃ for 30-60min;
s1 and S2 are not sequential.
Further, in S1, the indium salt is indium chloride or indium nitrate, and the tin salt is tin tetrachloride.
Further, the solvent in S1 includes acetylacetone and acetic anhydride.
Further, the carbon nanotubes in S2 are epoxidized carbon nanotubes.
Further, the preparation method of the epoxidized carbon nanotube comprises the following steps:
adding carboxylated carbon nanotubes into an organic solvent, uniformly dispersing by ultrasonic, adding KH-560, heating to reflux for 5-10h, filtering, washing and drying.
Further, the dispersing agent comprises sodium dodecyl benzene sulfonate and sodium carboxymethyl cellulose, and the weight ratio of the sodium dodecyl benzene sulfonate to the sodium carboxymethyl cellulose is 1-5:1-5.
Further, the ionic liquid is any one or a combination of a plurality of chloridized 1-butyl-3-methylimidazole, brominated 1-butyl-3-methylimidazole, 1-butyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methylimidazole mesylate, chloridized 1-hexyl-3-methylimidazole, brominated 1-hexyl-3-methylimidazole, 1-hexyl-3-methylimidazole tetrafluoroborate and 1-hexyl-3-methylimidazole mesylate.
Further, the conductive polymer is poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid.
Further, the heating rate during the heat treatment is 1-15 ℃/min.
The invention has the beneficial effects that:
the invention provides a preparation method of a capacitive touch screen ITO film, which takes a carbon nano tube film as a core layer, enables ITO sol to form a film on the carbon nano tube film, is favorable for improving the flexibility of the formed ITO film, has little influence on the light transmittance of the ITO film due to good optical transparency of the carbon nano tube, reduces the surface resistance of the carbon nano tube due to the addition of ionic liquid and conductive polymer, can generate chemical reaction with ethanolamine and acetic anhydride mutually when carrying out heat treatment by introducing epoxy groups to the carbon nano tube, enables the carbon nano tube film to be combined with the ITO sol more tightly, is favorable for forming the film of the ITO sol, reduces the aggregation tendency of indium tin oxide, avoids the reduction of photoelectric property, and has higher light transmittance, lower resistivity and good flexibility.
Drawings
Fig. 1 is a schematic structural diagram of the ITO film prepared in example 1, in which reference numeral 1 represents a carbon nanotube film, which is located at the center of the ITO film, and is coated with ITO nano-grains to form a "sandwich" structure.
Detailed Description
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention. The technology not mentioned in the present invention refers to the prior art, and unless otherwise indicated, the following examples and comparative examples are parallel tests, employing the same processing steps and parameters.
Example 1:
a preparation method of a capacitive touch screen ITO film comprises the following steps:
s1: adding 300.8g of indium nitrate into 5.8L of acetylacetone, carrying out ultrasonic oscillation for 30min to uniformly mix, stirring and heating until a bright light path is observed in a vertical illumination direction when the solution is irradiated by laser, stopping stirring and heating to obtain indium sol, adding 26g of tin tetrachloride into 51mL of acetic anhydride to uniformly mix to obtain tin solution, adding 5g of triethanolamine and 0.1g of 4-dimethylaminopyridine into 20mL of acetylacetone to uniformly mix to obtain a mixed solution, slowly dripping the tin solution and the mixed solution into the indium sol, and stirring for 0.5h after dripping to obtain ITO sol;
s2: adding 10g of carboxylated carbon nano tube into 250mL of ethyl acetate, carrying out ultrasonic dispersion for 30min, adding 50g of KH-560, heating to reflux reaction for 8h, filtering, washing by ethyl acetate to remove unreacted KH-560, drying at 50 ℃ and drying for 8h to obtain the epoxidized carbon nano tube, mixing 2g of the epoxidized carbon nano tube, 10g of sodium dodecyl benzene sulfonate, 10g of sodium carboxymethyl cellulose and 200mL of water, carrying out ultrasonic dispersion for 60min, centrifuging, taking supernatant, adding 5g of 1-butyl-3-methylimidazole chloride and 25mL of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid, stirring uniformly to obtain a carbon nano tube dispersion, spraying the carbon nano tube dispersion on a glass substrate with the temperature of 110+/-5 ℃, keeping the distance between the gun mouth of a spray gun and the glass substrate at 15+/-1 cm, and taking down the formed carbon nano tube film 1 from the glass substrate after the spraying is finished and waiting for 2min, wherein the thickness is 0.5 mu m;
s3: immersing and pulling the carbon nano tube film in ITO sol for 5 times after tensioning the carbon nano tube film by a clamp, wherein the pulling speed is 5mm/s, suspending and standing for 5min during each pulling, enabling the ITO sol to be attached to the surfaces of two sides of the carbon nano tube film, taking out and drying at 50 ℃ for 8h, then performing heat treatment at 400 ℃ for 40min, wherein the heating speed during heat treatment is 5 ℃/min, and naturally recovering the room temperature after the heat treatment is finished to obtain the ITO film with the total thickness of 0.75 mu m.
Example 2:
substantially the same as in example 1, except that the heat treatment temperature was 410 ℃.
Example 3:
substantially the same as in example 1, except that the heat treatment temperature was 420 ℃.
Comparative example 1:
substantially the same as in example 1, except that 4-dimethylaminopyridine was not added.
Comparative example 2:
substantially the same as in example 1, except that the carbon nanotubes of the same specification as those of the commercial product were used instead of the carbon nanotubes of the epoxidation.
Comparative example 3:
substantially the same as in example 1, except that 1-butyl-3-methylimidazole chloride was not added.
Comparative example 4:
substantially the same as in example 1, except that acetic anhydride was replaced with ethanol.
Comparative example 5:
the procedure was substantially the same as in example 1, except that the ITO sol was coated on a glass substrate having a temperature of 110.+ -. 5 ℃ by spin coating, the thickness of the ITO film was controlled by controlling the number of spin coating, and after drying at 50 ℃ for 8 hours after the spin coating was completed, heat treatment was further performed at 400 ℃ for 40 minutes at a heating rate of 5 ℃ per minute, and after the heat treatment was completed, the ITO film having a thickness of 0.75 μm was naturally recovered to room temperature.
Performance test:
the ITO thin films of examples 1 to 3 and comparative examples 1 to 4 of the present invention were used as test pieces for performance test;
resistivity: the square resistance of the sample measured by the double-electric-measurement four-probe tester is selected, and the calculation formula is as follows: r is R s ρ/t, where ρ is the resistivity of the sample and t is the thickness of the sample;
transmittance: measuring the light transmittance of the sample by using a UV-3600plus type ultraviolet visible near infrared spectrophotometer of Shimadzu corporation, wherein the wavelength is 400-900nm;
when the sample is bent, the larger the generated strain is, the larger the stress generated between corresponding film microelements is, when the strain quantity is increased to a certain value, the structure of the sample is seriously damaged and can not be recovered, the resistance value of the sample is obviously suddenly changed, the resistance value is called critical strain, the inventor performs critical strain test of the sample on a series of standard cylinders with different radiuses, and the maximum bending radius when the critical strain is generated is recorded and is used as an evaluation index of sample flexibility;
the test results are shown in table 1 below:
table 1:
as shown in Table 1, the ITO film provided by the invention has higher transmittance, lower resistivity and good flexibility.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (6)

1. The preparation method of the ITO film of the capacitive touch screen is characterized by comprising the following steps of:
s1: preparing ITO sol by taking indium salt, tin salt, ethanolamine, 4-dimethylaminopyridine and a solvent as raw materials;
the solvent in S1 comprises acetylacetone and acetic anhydride;
s2: mixing carbon nano tubes, a dispersing agent and water, performing ultrasonic dispersion, centrifuging, taking supernatant, adding an ionic liquid and a conductive polymer to obtain carbon nano tube dispersion liquid, spraying the carbon nano tube dispersion liquid on a substrate by using a spraying method, wherein the temperature of the substrate is 105-120 ℃, and removing a formed carbon nano tube film from the substrate;
s2, the carbon nanotubes are epoxidized carbon nanotubes;
the preparation method of the epoxy carbon nano tube comprises the following steps:
adding carboxylated carbon nanotubes into an organic solvent, uniformly dispersing by ultrasonic, adding KH-560, heating to reflux reaction for 5-10h, filtering, washing and drying;
s3: immersing and pulling the carbon nano tube film in ITO sol for several times, taking out and drying, and then performing heat treatment at 400-420 ℃ for 30-60min;
s1 and S2 are not sequential.
2. The method for preparing an ITO film for capacitive touch screen according to claim 1, wherein the indium salt in S1 is indium chloride or indium nitrate, and the tin salt is tin tetrachloride.
3. The method for preparing the capacitive touch screen ITO film according to claim 1, wherein the dispersing agent comprises sodium dodecyl benzene sulfonate and sodium carboxymethyl cellulose, and the weight ratio of the sodium dodecyl benzene sulfonate to the sodium carboxymethyl cellulose is 1-5:1-5.
4. The method for preparing a capacitive touch screen ITO film according to claim 1, wherein the ionic liquid is any one or more of chlorinated 1-butyl-3-methylimidazole, brominated 1-butyl-3-methylimidazole, 1-butyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methylimidazole mesylate, chlorinated 1-hexyl-3-methylimidazole, brominated 1-hexyl-3-methylimidazole, 1-hexyl-3-methylimidazole tetrafluoroborate and 1-hexyl-3-methylimidazole mesylate.
5. The method for manufacturing a capacitive touch screen ITO film according to claim 1, wherein the conductive polymer is poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid.
6. The method for manufacturing an ITO film for capacitive touch screen according to claim 1, wherein a heating rate at the time of heat treatment is 1-15 ℃/min.
CN202311132140.XA 2023-09-04 2023-09-04 Preparation method of capacitive touch screen ITO film Active CN117275830B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010033775A (en) * 2008-07-25 2010-02-12 Touch Panel Kenkyusho:Kk Transparent conductive composite film and sheet
KR20130081374A (en) * 2012-01-09 2013-07-17 충남대학교산학협력단 Tio2/ito/single-wall carbon nanotube composites and preparation method thereof
CN103325859A (en) * 2013-06-26 2013-09-25 深圳市亚太兴实业有限公司 Preparation method of ITO thin film
CN104318983A (en) * 2014-10-31 2015-01-28 徐东 Preparation method of ITO thin film
CN107093495A (en) * 2017-03-22 2017-08-25 合肥仁德电子科技有限公司 A kind of preparation method of ito thin film for touch-screen

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100045610A1 (en) * 2008-08-20 2010-02-25 Snu R&Db Foundation Transparent conductive films
US20120148835A1 (en) * 2010-12-08 2012-06-14 Bayer Materialscience Ag Hybrid conductive composite

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010033775A (en) * 2008-07-25 2010-02-12 Touch Panel Kenkyusho:Kk Transparent conductive composite film and sheet
KR20130081374A (en) * 2012-01-09 2013-07-17 충남대학교산학협력단 Tio2/ito/single-wall carbon nanotube composites and preparation method thereof
CN103325859A (en) * 2013-06-26 2013-09-25 深圳市亚太兴实业有限公司 Preparation method of ITO thin film
CN104318983A (en) * 2014-10-31 2015-01-28 徐东 Preparation method of ITO thin film
CN107093495A (en) * 2017-03-22 2017-08-25 合肥仁德电子科技有限公司 A kind of preparation method of ito thin film for touch-screen

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