CN115132404A - Method for manufacturing transparent flexible film electrode - Google Patents
Method for manufacturing transparent flexible film electrode Download PDFInfo
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- CN115132404A CN115132404A CN202210900687.9A CN202210900687A CN115132404A CN 115132404 A CN115132404 A CN 115132404A CN 202210900687 A CN202210900687 A CN 202210900687A CN 115132404 A CN115132404 A CN 115132404A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
Abstract
The invention relates to the technical field of electronic components, in particular to a manufacturing method of a transparent flexible film electrode, which comprises the following steps: (1) pretreating the surface of the substrate; (2) coating polyimide slurry on the surface of the pretreated substrate and curing to obtain a polyimide layer; (3) forming a conductive groove on the polyimide layer according to the electrode pattern design; (4) spraying heat-conducting ink in the electric conduction groove and curing to obtain a heat-conducting protective layer; (5) filling the nano-silver conductive ink into the conductive groove sprayed with the heat-conducting ink, and drying and curing; (6) removing the redundant nano silver conductive ink outside the conductive groove to obtain an electrode pattern; (7) and coating ultraviolet curing liquid on the surface of the polyimide coating with the obtained electrode pattern and curing to obtain the transparent packaging layer. The electrode prepared by the invention has the response speed of 2-5s, the bending resistance times of more than 30 ten thousand, the temperature of 35-50 ℃ after heating for 72h, good high-temperature performance and greatly prolonged service life.
Description
Technical Field
The invention relates to the technical field of electronic components, in particular to a manufacturing method of a transparent flexible thin film electrode.
Background
With the continuous pursuit of human beings on visual enjoyment and improvement of living texture, transparent flexible display and wearable foldable electronic products are applied more in the aspect of meeting the requirements under personalized, diversified and complex conditions. The flexible electrode is a thin film material with high light transmittance, high conductivity and bending performance, and is a core element for forming optoelectronic devices such as solar cells, light emitting diodes, liquid crystal displays, touch screens and the like.
The most widely used transparent electrode material at present is a metal oxide semiconductor, such as Indium Tin Oxide (ITO), and despite of high conductivity and high transmittance, the ITO thin film has limited yield and high price due to the rare indium content; meanwhile, the inherent brittleness, complex instruments and high temperature required in preparation greatly limit the application of the silver nanowire conductive nano material in the field of flexible transparent electrodes, and the silver nanowire conductive nano material is widely researched as a transparent electrode material due to a series of advantages of good conductivity, light transmission, flexibility, solution treatment processing mode and the like.
The preparation of the flexible transparent electrode of current nanometer silver adopts the mode preparation conducting layer of whole face coating nanometer silver conductive ink usually, then laser etching goes out conductive channel, and in the time of laser etching conductive channel, the nanometer silver line can be broken the ablation by laser to form the conducting wire, observe under the microscope, the line edge of laser etching is more crude, and this kind of roughness can cause there is following harmful effects to the electrode: firstly, after the touch control film set is made, etching marks exist, and the appearance is influenced; secondly, in the running process of the device, current continuously flows through the transparent electrode, the generated Joule heat can cause the local temperature of the silver nanowire to rise, especially for the device with poor heat conductivity of the base material, the Joule heat generated by the silver nanowire is difficult to diffuse outwards through the base material, and further causes the accumulation of local heat, and the damage effect of the Joule heat effect on the structure and the electric conductivity of the silver nanowire is more serious than that of uniform external heating; thirdly, once the packaging is poor or in a high-humidity environment, silver migration occurs on the broken nano silver particles, so that the conductive circuit is short-circuited, and the device fails. Therefore, forming a thin film electrode having excellent uniformity, light transmittance, conductivity, and smoothness is a technical problem that those skilled in the art are demanding to solve.
Disclosure of Invention
In order to solve the problems, the invention provides a method for manufacturing a transparent flexible thin film electrode, and the transparent flexible thin film electrode which is quick in response and long in service life is manufactured.
A method for manufacturing a transparent flexible film electrode comprises the following steps:
(1) pretreating the surface of the substrate;
(2) coating polyimide slurry on the surface of the pretreated substrate and curing to obtain a polyimide layer;
(3) opening a conductive groove on the polyimide layer according to the electrode pattern design;
(4) spraying heat-conducting ink in the electric conduction groove and curing to obtain a heat-conducting protective layer;
(5) filling the nano-silver conductive ink into the conductive groove sprayed with the heat-conducting ink, and drying and curing;
(6) removing the redundant nano silver conductive ink outside the conductive groove to obtain an electrode pattern;
(7) and coating ultraviolet curing liquid on the surface of the polyimide coating with the obtained electrode pattern and curing to obtain the transparent packaging layer.
Further, the dyne value of the surface of the substrate after pretreatment in the step (1) is controlled to be 40-60mN/m, and the thickness of the polyimide layer in the step (2) is controlled to be 5-15 um. Preferably, the dyne value of the surface of the substrate after pretreatment in the step (1) is controlled to be 45-55mN/m, and the thickness of the polyimide layer in the step (2) is 8-12 um.
Further, the conductive groove in the step (3) is a V-shaped conductive groove, and the V-shaped conductive groove is obtained by laser grooving. The groove is usually a single-side groove, including but not limited to a V-shape, a U-shape, a W-shape, an X-shape, etc., and the conductive groove is defined to have a V-shape in cross section in the present application, so that two walls at the groove bottom of the V-shaped conductive groove are used for compacting the nano silver conductive ink, and the compacting density is increased, thereby increasing the contact area between nano silver in the ink, further increasing the conductive paths of the silver nanowires, and reducing the wire resistance.
Furthermore, the groove angle of the V-shaped conductive groove is 10-80 degrees, and the groove depth is 0.05-0.15 um. Preferably, the slotting angle of the V-shaped conductive groove is 30-60 degrees, and the slotting depth is 0.05-0.08 um.
Further, the thickness of the heat-conducting protective layer in the step (4) is 3-10 nm. Preferably, the thickness of the heat-conducting protective layer in the step (4) is 5-8 nm.
Further, the heat conductive ink consists of the following components:
50-65% of matrix resin;
0.5 to 1.0 percent of dispersant;
10-25% of organic solvent;
10-25% of heat-conducting filler;
0.5 to 1.0 percent of coupling agent; and the number of the first and second groups,
0.5 to 1.0 percent of modified additive.
Preferably, the thermally conductive ink consists of the following components:
55% of matrix resin;
0.8 percent of dispersant;
20% of an organic solvent;
20% of heat-conducting filler;
1% of a coupling agent; and (c) a second step of,
0.5 to 1.0 percent of modified additive.
Specifically, the matrix resin is selected from polyimide resins; the dispersing agent is an organic dispersing agent and is selected from one or more of triethyl hexyl phosphoric acid, sodium dodecyl sulfate, methyl amyl alcohol, cellulose derivatives, polyacrylamide, Guel gum and fatty acid polyglycol ester; the organic solvent is at least one selected from polyethylene glycol, polyvinyl alcohol, ethanol, isopropanol, n-butanol, propylene glycol methyl ether, butanone and gamma-butyrolactone.
Further, the heat conducting filler is selected from one of graphene, silicon carbide, boron nitride, silicon nitride, aluminum oxide and zinc oxide; the coupling agent is selected from one of silane coupling agent, titanate coupling agent, aluminate coupling agent, bimetallic coupling agent, phosphate coupling agent and borate coupling agent.
Further, the modification additive is selected from at least one of octadecyl amine, octadecyl amine oxide, polydopamine, 1-pyrenebutyric acid and chlorosulfonic acid.
The heat conduction ink takes the heat conduction filler as a functional material, plays a heat conduction role, prevents the internal temperature of the electrode from being too high to influence the conductivity, and the coupling agent is mainly used for enhancing the adhesiveness of a heat conduction protective layer, the polyimide of the electric conduction groove and the electric conduction pattern. .
The heat conduction protective layer sets up in electrically conductive slot bottom, can reduce heat conduction printing ink quantity on the one hand, prevents that electrode thickness from increasing, and on the other hand can not cause the contact resistance increase yet to influence the response speed and the sensitivity of touch-control. After the heat conduction layer is increased, heat is fully transferred inside the electrode, the temperature of the conductive circuit is increased along with the prolonging of the service life, the strengthening of the lattice vibration of the conductive metal (silver nanowires) interferes the movement of free electrons, the heat conductivity coefficient is reduced, and the heat generated inside is fully led out through the arrangement of the heat conduction protection layer, so that the nano silver wires are protected from being broken due to high temperature, and the high temperature performance of the electrode is ensured.
Further, in the step (6), the excess nano silver conductive ink outside the conductive groove is removed, and the specific steps are as follows: and coating a release agent outside the cured nano-silver conductive ink to obtain a release layer, controlling the stripping force of the release layer to be 10-30 g, and then stripping the release layer to remove the redundant nano-silver conductive ink to obtain an electrode pattern.
Further, the thickness of the transparent encapsulation layer in the step (7) is 100-200 nm. Preferably, the thickness of the transparent encapsulation layer in step (7) is 150 nm.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method for manufacturing the transparent flexible film electrode comprises the steps of pre-coating a film on the surface of a transparent optical film substrate, manufacturing a conductive groove, a heat-conducting protective layer, a conductive circuit and a packaging layer, and filling nano-silver conductive ink into the conductive groove to obtain an electrode pattern by presetting the conductive groove on polyimide, so that the conductive layer is prevented from being etched, the conductive material of the nano-silver wire is prevented from being broken and ablated, the broken nano-silver wire is prevented from transmitting silver migration under bad external conditions, and the service life of a device is prolonged. The electrode prepared by the invention has the response speed of 2-5s, the bending resistance times of more than 30 ten thousand, the temperature of 35-50 ℃ after heating for 72h, good high-temperature performance and greatly prolonged service life.
(2) The manufacturing method of the transparent flexible film electrode provided by the invention prepares the conductive groove in advance, and can adjust the filling amount of the conductive material by controlling the grooving depth and the grooving angle of the groove, thereby achieving the purpose of controlling the resistance of the electrode wire; through setting up electrically conductive slot and being V type groove, can utilize the V type lateral wall to carry out the compaction to the electrically conductive printing ink in the electrically conductive slot to increase the area of contact of nanometer silver line, increase electrically conductive route, and then reduce the electrode line and hinder.
(3) According to the manufacturing method of the transparent flexible film electrode, the heat conduction protective layer is prepared by coating the heat conduction ink in the electric conduction groove in advance, then the electric conduction ink is filled, the heat conduction performance of the electrode is improved by utilizing the heat conduction protective layer, and the phenomenon that the electrode performance is influenced due to overhigh local temperature caused by joule heat generated inside the electrode when a device runs is prevented.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Carrying out corona pretreatment on the substrate to control the surface dyne value of the substrate to be 45-55 mN/m;
(2) coating polyimide slurry on the surface of the pretreated substrate and curing to obtain a polyimide layer, wherein the solid content of the polyimide slurry is 20%, and the coating film-forming technological parameters are as follows: the pumping flow is 15ml/s, the speed of a coating machine is 10m/min, the coating head gap is 50um, and the thickness of the polyimide layer is controlled to be 10 um;
(3) according to the design of an electrode pattern, a conductive groove is formed in a polyimide layer by using laser, the laser wavelength is 278 plus 355nm, the output power is 10W, the pulse width is 5-500 ns and is adjustable, the repetition frequency is 20-100KHz, a scanning galvanometer and an XY moving platform are used for scanning and processing the conductive film, the grooving angle is controlled to be 45 degrees, and the grooving depth is 0.11 um;
(4) and spraying heat-conducting ink in the electric conduction groove and curing to obtain a heat-conducting protective layer, wherein the thickness of the heat-conducting protective layer is 7nm, and the heat-conducting ink comprises the following components: 55 parts of polyimide resin, 25 parts of (gamma-butyrolactone: propylene glycol monomethyl ether) mixed solvent with the mass ratio of 1:1, 1 part of triethyl hexyl phosphoric acid dispersant, 20 parts of boron nitride conductive filler, 1 part of titanate coupling agent and 1 part of octadecyl amine oxide modified additive.
(5) Filling the nano-silver conductive ink into the conductive groove sprayed with the heat-conducting ink, drying and curing, wherein the content of Ag in the nano-silver conductive ink is 0.5%, the viscosity is 10cps, and the drying temperature is 100 ℃;
(6) removing redundant nano silver conductive ink outside the V-shaped conductive groove to obtain an electrode pattern, and peeling by coating a release agent, wherein the peeling force is controlled to be 20-25 g;
(7) coating ultraviolet curing liquid on the surface of the polyimide coating with the obtained electrode pattern and curing to obtain a transparent packaging layer, wherein the solid content of the ultraviolet curing liquid is 10%, and the coating film-forming technological parameters are as follows: the pumping flow is 10ml/s, the speed of a coating machine is 15m/min, the coating head gap is 100um, and the thickness of the transparent packaging layer is controlled to be 150 nm.
Example 2
(1) Carrying out corona pretreatment on the substrate to control the surface dyne value of the substrate to be 40-45 mN/m;
(2) coating polyimide slurry on the surface of the pretreated substrate and curing to obtain a polyimide layer, wherein the solid content of the polyimide slurry is 20%, and the coating film-forming technological parameters are as follows: the pumping flow is 15ml/s, the speed of a coating machine is 10m/min, the coating head gap is 50um, and the thickness of the polyimide layer is controlled to be 5 um;
(3) according to the design of an electrode pattern, a conductive groove is formed in a polyimide layer by using laser, the laser wavelength is 278 plus 355nm, the output power is 10W, the pulse width is 5-500 ns and is adjustable, the repetition frequency is 20-100KHz, a scanning galvanometer and an XY moving platform are used for scanning and processing the conductive film, the grooving angle is controlled to be 30 degrees, and the grooving depth is 0.05 um;
(4) and spraying heat-conducting ink in the electric conduction groove and curing to obtain a heat-conducting protective layer, wherein the thickness of the heat-conducting protective layer is 3nm, and the heat-conducting ink comprises the following components: 50 parts of polyimide resin, 23 parts of (ethylene glycol: isopropanol) mixed solvent with the mass ratio of 1:1, 0.5 part of sodium dodecyl sulfate dispersing agent, 25 parts of graphene conductive filler, 0.5 part of silane coupling agent and 1 part of polydopamine modified additive.
(5) Filling the nano-silver conductive ink into the conductive groove sprayed with the heat-conducting ink, drying and curing, wherein the content of Ag in the nano-silver conductive ink is 0.5%, the viscosity is 10cps, and the drying temperature is 80 ℃;
(6) removing redundant nano silver conductive ink outside the V-shaped conductive groove to obtain an electrode pattern, and peeling by coating a release agent, wherein the peeling force is controlled to be 10-20 g;
(7) coating ultraviolet curing liquid on the surface of the polyimide coating with the obtained electrode pattern and curing to obtain a transparent packaging layer, wherein the solid content of the ultraviolet curing liquid is 10%, and the coating film-forming technological parameters are as follows: the pumping flow is 10ml/s, the speed of a coating machine is 15m/min, the coating head gap is 100um, and the thickness of the transparent packaging layer is controlled to be 100 nm.
Example 3
(1) Carrying out corona pretreatment on the substrate to control the surface dyne value of the substrate to be 55-60 mN/m;
(2) coating polyimide slurry on the surface of the pretreated substrate and curing to obtain a polyimide layer, wherein the solid content of the polyimide slurry is 20%, and the coating film-forming technological parameters are as follows: the pumping flow is 15ml/s, the speed of a coating machine is 10m/min, the coating head gap is 50um, and the thickness of the polyimide layer is controlled to be 12 um;
(3) according to the design of an electrode pattern, a conductive groove is formed in a polyimide layer by using laser, the laser wavelength is 278 plus 355nm, the output power is 10W, the pulse width is 5-500 ns and is adjustable, the repetition frequency is 20-100KHz, a scanning galvanometer and an XY moving platform are used for scanning and processing the conductive film, the grooving angle is controlled to be 60 degrees, and the grooving depth is 0.15 um;
(4) and spraying heat-conducting ink in the electric conduction groove and curing to obtain a heat-conducting protective layer, wherein the thickness of the heat-conducting protective layer is 10nm, and the heat-conducting ink comprises the following components: 65 parts of polyimide resin, 20 parts of (polyvinyl alcohol: butanone) mixed solvent with the mass ratio of 1:1, 0.7 part of fatty acid polyglycol ester dispersant, 12 parts of zinc oxide conductive filler, 0.8 part of phosphate coupling agent and 1.5 parts of chlorosulfonic acid modified additive.
(5) Filling the nano-silver conductive ink into the conductive groove sprayed with the heat-conducting ink, drying and curing, wherein the content of Ag in the nano-silver conductive ink is 0.5%, the viscosity of the nano-silver conductive ink is 10cps, and the drying temperature is 80 ℃;
(6) removing redundant nano silver conductive ink outside the V-shaped conductive groove to obtain an electrode pattern, and peeling by coating a release agent, wherein the peeling force is controlled to be 25-30 g;
(7) coating ultraviolet curing liquid on the surface of the polyimide coating with the obtained electrode pattern and curing to obtain a transparent packaging layer, wherein the solid content of the ultraviolet curing liquid is 10%, and the coating film-forming technological parameters are as follows: the pumping flow is 10ml/s, the speed of a coating machine is 15m/min, the coating head gap is 100um, and the thickness of the transparent packaging layer is controlled to be 200 nm.
Example 4
This example includes most of the operation steps of example 1, except that the conductive trench has a 0 ° open angle, i.e., the open bottom is a flat surface. The preparation method comprises the following steps:
(1) carrying out corona pretreatment on the substrate to control the surface dyne value of the substrate to be 45-55 mN/m;
(2) coating polyimide slurry on the surface of the pretreated substrate and curing to obtain a polyimide layer, wherein the solid content of the polyimide slurry is 20%, and the coating film-forming technological parameters are as follows: the pumping flow is 15ml/s, the speed of a coating machine is 10m/min, the coating head gap is 50um, and the thickness of the polyimide layer is controlled to be 10 um;
(3) forming a conductive groove on the polyimide layer according to the electrode pattern design, coating photosensitive photoresist, exposing and developing to obtain the conductive groove, wherein the groove opening angle is 0 degree, and the groove opening depth is 0.11 um;
(4) and spraying heat-conducting ink in the electric conduction groove and curing to obtain a heat-conducting protective layer, wherein the thickness of the heat-conducting protective layer is 7nm, and the heat-conducting ink comprises the following components: 55 parts of polyimide resin, 25 parts of (gamma-butyrolactone: propylene glycol monomethyl ether) mixed solvent with the mass ratio of 1:1, 1 part of triethyl hexyl phosphoric acid dispersant, 20 parts of boron nitride conductive filler, 1 part of titanate coupling agent and 1 part of octadecyl amine oxide modified additive.
(5) Filling the nano-silver conductive ink into the conductive groove sprayed with the heat-conducting ink, drying and curing, wherein the content of Ag in the nano-silver conductive ink is 0.5%, the viscosity of the nano-silver conductive ink is 10cps, and the drying temperature is 100 ℃;
(6) removing redundant nano silver conductive ink outside the V-shaped conductive groove to obtain an electrode pattern, and peeling by coating a release agent, wherein the peeling force is controlled to be 20-25 g;
(7) coating ultraviolet curing liquid on the surface of the polyimide coating with the obtained electrode pattern and curing to obtain a transparent packaging layer, wherein the solid content of the ultraviolet curing liquid is 10%, and the coating film-forming technological parameters are as follows: the pumping flow is 10ml/s, the speed of a coating machine is 15m/min, the coating head gap is 100um, and the thickness of the transparent packaging layer is controlled to be 150 nm.
Example 5
This example includes most of the steps of example 1, except that the conductive trench is notched at an angle of 80 °. The preparation method comprises the following steps:
(1) carrying out corona pretreatment on the substrate to control the surface dyne value of the substrate to be 45-55 mN/m;
(2) coating polyimide slurry on the surface of the pretreated substrate and curing to obtain a polyimide layer, wherein the solid content of the polyimide slurry is 20%, and the coating film-forming technological parameters are as follows: the pumping flow is 15ml/s, the speed of a coating machine is 10m/min, the coating head gap is 50um, and the thickness of the polyimide layer is controlled to be 10 um;
(3) according to the design of an electrode pattern, a conductive groove is formed in a polyimide layer by using laser, the laser wavelength is 278 and 355nm, the output power is 10W, the pulse width is 5-500 ns and is adjustable, the repetition frequency is 20-100KHz, the conductive film is scanned and processed by a scanning galvanometer and an XY moving platform, the grooving angle is controlled to be 80 degrees, and the grooving depth is 0.11 um;
(4) and spraying heat-conducting ink in the electric conduction groove and curing to obtain a heat-conducting protective layer, wherein the thickness of the heat-conducting protective layer is 7nm, and the heat-conducting ink comprises the following components: 55 parts of polyimide resin, 25 parts of (gamma-butyrolactone: propylene glycol monomethyl ether) mixed solvent with the mass ratio of 1:1, 1 part of triethyl hexyl phosphoric acid dispersant, 20 parts of boron nitride conductive filler, 1 part of titanate coupling agent and 1 part of octadecyl amine oxide modified additive.
(5) Filling the nano-silver conductive ink into the conductive groove sprayed with the heat-conducting ink, drying and curing, wherein the content of Ag in the nano-silver conductive ink is 0.5%, the viscosity of the nano-silver conductive ink is 10cps, and the drying temperature is 100 ℃;
(6) removing redundant nano silver conductive ink outside the V-shaped conductive groove to obtain an electrode pattern, and peeling by coating a release agent, wherein the peeling force is controlled to be 20-25 g;
(7) coating ultraviolet curing liquid on the surface of the polyimide coating with the obtained electrode pattern and curing to obtain a transparent packaging layer, wherein the solid content of the ultraviolet curing liquid is 10%, and the coating film-forming technological parameters are as follows: the pumping flow is 10ml/s, the speed of a coating machine is 15m/min, the coating head gap is 100um, and the thickness of the transparent packaging layer is controlled to be 150 nm.
Example 6
This embodiment includes most of the operation steps of embodiment 1, except that the depth of the conductive trench is 0.02 um. The preparation method comprises the following steps:
(1) carrying out corona pretreatment on the substrate to control the surface dyne value of the substrate to be 45-55 mN/m;
(2) coating polyimide slurry on the surface of the pretreated substrate and curing to obtain a polyimide layer, wherein the solid content of the polyimide slurry is 20%, and the coating film-forming technological parameters are as follows: the pumping flow is 15ml/s, the speed of a coating machine is 10m/min, the coating head gap is 50um, and the thickness of the polyimide layer is controlled to be 10 um;
(3) according to the design of an electrode pattern, a conductive groove is formed in a polyimide layer by using laser, the laser wavelength is 278 plus 355nm, the output power is 10W, the pulse width is 5-500 ns and is adjustable, the repetition frequency is 20-100KHz, a scanning galvanometer and an XY moving platform are used for scanning and processing the conductive film, the grooving angle is controlled to be 45 degrees, and the grooving depth is 0.02 um;
(4) and spraying heat-conducting ink in the electric conduction groove and curing to obtain a heat-conducting protective layer, wherein the thickness of the heat-conducting protective layer is 7nm, and the heat-conducting ink comprises the following components: 55 parts of polyimide resin, 25 parts of (gamma-butyrolactone: propylene glycol monomethyl ether) mixed solvent with the mass ratio of 1:1, 1 part of triethyl hexyl phosphoric acid dispersant, 20 parts of boron nitride conductive filler, 1 part of titanate coupling agent and 1 part of octadecyl amine oxide modified additive.
(5) Filling the nano-silver conductive ink into the conductive groove sprayed with the heat-conducting ink, drying and curing, wherein the content of Ag in the nano-silver conductive ink is 0.5%, the viscosity is 10cps, and the drying temperature is 100 ℃;
(6) removing redundant nano silver conductive ink outside the V-shaped conductive groove to obtain an electrode pattern, and peeling by coating a release agent, wherein the peeling force is controlled to be 20-25 g;
(7) coating ultraviolet curing liquid on the surface of the polyimide coating with the obtained electrode pattern and curing to obtain a transparent packaging layer, wherein the solid content of the ultraviolet curing liquid is 10%, and the coating film-forming technological parameters are as follows: the pumping flow is 10ml/s, the speed of a coating machine is 15m/min, the coating head gap is 100um, and the thickness of the transparent packaging layer is controlled to be 150 nm.
Example 7
This embodiment includes most of the operation steps of embodiment 1, except that the depth of the conductive trench is 0.25 um. The preparation method comprises the following steps:
(1) carrying out corona pretreatment on the substrate to control the surface dyne value of the substrate to be 45-55 mN/m;
(2) coating polyimide slurry on the surface of the pretreated substrate and curing to obtain a polyimide layer, wherein the solid content of the polyimide slurry is 20%, and the coating film-forming technological parameters are as follows: the pumping flow is 15ml/s, the speed of a coating machine is 10m/min, the coating head gap is 50um, and the thickness of the polyimide layer is controlled to be 10 um;
(3) according to the design of an electrode pattern, a conductive groove is formed in a polyimide layer by using laser, the laser wavelength is 278 plus 355nm, the output power is 10W, the pulse width is 5-500 ns and is adjustable, the repetition frequency is 20-100KHz, a scanning galvanometer and an XY moving platform are used for scanning and processing the conductive film, the grooving angle is controlled to be 45 degrees, and the grooving depth is 0.25 um;
(4) and spraying heat-conducting ink in the electric conduction groove and curing to obtain a heat-conducting protective layer, wherein the thickness of the heat-conducting protective layer is 7nm, and the heat-conducting ink comprises the following components: 55 parts of polyimide resin, 25 parts of (gamma-butyrolactone: propylene glycol monomethyl ether) mixed solvent with the mass ratio of 1:1, 1 part of triethyl hexyl phosphoric acid dispersant, 20 parts of boron nitride conductive filler, 1 part of titanate coupling agent and 1 part of octadecyl amine oxide modified additive.
(5) Filling the nano-silver conductive ink into the conductive groove sprayed with the heat-conducting ink, drying and curing, wherein the content of Ag in the nano-silver conductive ink is 0.5%, the viscosity is 10cps, and the drying temperature is 100 ℃;
(6) removing redundant nano silver conductive ink outside the V-shaped conductive groove to obtain an electrode pattern, and peeling by coating a release agent, wherein the peeling force is controlled to be 20-25 g;
(7) coating ultraviolet curing liquid on the surface of the polyimide coating with the obtained electrode pattern and curing to obtain a transparent packaging layer, wherein the solid content of the ultraviolet curing liquid is 10%, and the coating film-forming technological parameters are as follows: the pumping flow is 10ml/s, the speed of a coating machine is 15m/min, the coating head gap is 100um, and the thickness of the transparent packaging layer is controlled to be 150 nm.
Example 8
This example includes most of the steps of example 1, except that the thermal conductive protective layer is 25nm thick. The preparation method comprises the following steps:
(1) carrying out corona pretreatment on the substrate to control the surface dyne value of the substrate to be 45-55 mN/m;
(2) coating polyimide slurry on the surface of the pretreated substrate and curing to obtain a polyimide layer, wherein the solid content of the polyimide slurry is 20%, and the coating film-forming technological parameters are as follows: the pumping flow is 15ml/s, the speed of a coating machine is 10m/min, the coating head gap is 50um, and the thickness of the polyimide layer is controlled to be 10 um;
(3) according to the design of an electrode pattern, a conductive groove is formed in a polyimide layer by using laser, the laser wavelength is 278 plus 355nm, the output power is 10W, the pulse width is 5-500 ns and is adjustable, the repetition frequency is 20-100KHz, a scanning galvanometer and an XY moving platform are used for scanning and processing the conductive film, the grooving angle is controlled to be 45 degrees, and the grooving depth is 0.11 um;
(4) and spraying heat-conducting ink in the electric conduction groove and curing to obtain a heat-conducting protective layer, wherein the thickness of the heat-conducting protective layer is 25nm, and the heat-conducting ink comprises the following components: 55 parts of polyimide resin, 25 parts of (gamma-butyrolactone: propylene glycol monomethyl ether) mixed solvent with the mass ratio of 1:1, 1 part of triethyl hexyl phosphoric acid dispersant, 20 parts of boron nitride conductive filler, 1 part of titanate coupling agent and 1 part of octadecyl amine oxide modified additive.
(5) Filling the nano-silver conductive ink into the conductive groove sprayed with the heat-conducting ink, drying and curing, wherein the content of Ag in the nano-silver conductive ink is 0.5%, the viscosity is 10cps, and the drying temperature is 100 ℃;
(6) removing redundant nano silver conductive ink outside the V-shaped conductive groove to obtain an electrode pattern, and peeling by coating a release agent, wherein the peeling force is controlled to be 20-25 g;
(7) coating ultraviolet curing liquid on the surface of the polyimide coating with the obtained electrode pattern and curing to obtain a transparent packaging layer, wherein the solid content of the ultraviolet curing liquid is 10%, and the coating film-forming technological parameters are as follows: the pumping flow is 10ml/s, the speed of a coating machine is 15m/min, the coating head gap is 100um, and the thickness of the transparent packaging layer is controlled to be 150 nm.
Example 9
This example includes most of the operations of example 1, except that no modifying additives are added to the thermally conductive ink of the thermally conductive protective layer. The preparation method comprises the following steps:
(1) carrying out corona pretreatment on the substrate to control the surface dyne value of the substrate to be 45-55 mN/m;
(2) coating polyimide slurry on the surface of the pretreated substrate and curing to obtain a polyimide layer, wherein the solid content of the polyimide slurry is 20%, and the coating film-forming technological parameters are as follows: the pumping flow is 15ml/s, the speed of a coating machine is 10m/min, the coating head gap is 50um, and the thickness of the polyimide layer is controlled to be 10 um;
(3) according to the design of an electrode pattern, a conductive groove is formed in a polyimide layer by using laser, the laser wavelength is 278 plus 355nm, the output power is 10W, the pulse width is 5-500 ns and is adjustable, the repetition frequency is 20-100KHz, a scanning galvanometer and an XY moving platform are used for scanning and processing the conductive film, the grooving angle is controlled to be 45 degrees, and the grooving depth is 0.11 um;
(4) and spraying heat-conducting ink in the electric conduction groove and curing to obtain a heat-conducting protective layer, wherein the thickness of the heat-conducting protective layer is 7nm, and the heat-conducting ink comprises the following components: 55 parts of polyimide resin, 25 parts of (gamma-butyrolactone: propylene glycol monomethyl ether) mixed solvent with the mass ratio of 1:1, 1 part of triethyl hexyl phosphoric acid dispersant, 20 parts of boron nitride conductive filler and 1 part of titanate coupling agent.
(5) Filling the nano-silver conductive ink into the conductive groove sprayed with the heat-conducting ink, drying and curing, wherein the content of Ag in the nano-silver conductive ink is 0.5%, the viscosity of the nano-silver conductive ink is 10cps, and the drying temperature is 100 ℃;
(6) removing redundant nano silver conductive ink outside the V-shaped conductive groove to obtain an electrode pattern, and peeling by coating a release agent, wherein the peeling force is controlled to be 20-25 g;
(7) coating ultraviolet curing liquid on the surface of the polyimide coating with the obtained electrode pattern and curing to obtain a transparent packaging layer, wherein the solid content of the ultraviolet curing liquid is 10%, and the coating film-forming technological parameters are as follows: the pumping flow is 10ml/s, the speed of a coating machine is 15m/min, the coating head gap is 100um, and the thickness of the transparent packaging layer is controlled to be 150 nm.
Comparative example 1
This comparative example includes most of the operation steps of example 1, except that the heat conductive protective layer is not provided. The preparation method comprises the following steps:
(1) carrying out corona pretreatment on the substrate to control the surface dyne value of the substrate to be 45-55 mN/m;
(2) coating polyimide slurry on the surface of the pretreated substrate and curing to obtain a polyimide layer, wherein the solid content of the polyimide slurry is 20%, and the coating film-forming technological parameters are as follows: the pumping flow is 15ml/s, the speed of a coating machine is 10m/min, the coating head gap is 50um, and the thickness of the polyimide layer is controlled to be 10 um;
(3) according to the design of an electrode pattern, a conductive groove is formed in a polyimide layer by using laser, the laser wavelength is 278 plus 355nm, the output power is 10W, the pulse width is 5-500 ns and is adjustable, the repetition frequency is 20-100KHz, a scanning galvanometer and an XY moving platform are used for scanning and processing the conductive film, the grooving angle is controlled to be 45 degrees, and the grooving depth is 0.11 um;
(4) filling the nano-silver conductive ink into the conductive groove, drying and curing, wherein the content of Ag in the nano-silver conductive ink is 0.5%, the viscosity is 10cps, and the drying temperature is 100 ℃;
(5) removing redundant nano silver conductive ink outside the V-shaped conductive groove to obtain an electrode pattern, and peeling by coating a release agent, wherein the peeling force is controlled to be 20-25 g;
(6) coating ultraviolet curing liquid on the surface of the polyimide coating with the obtained electrode pattern and curing to obtain a transparent packaging layer, wherein the solid content of the ultraviolet curing liquid is 10%, and the coating film-forming technological parameters are as follows: the pumping flow is 10ml/s, the speed of a coating machine is 15m/min, the coating head gap is 100um, and the thickness of the transparent packaging layer is controlled to be 150 nm.
Comparative example 2
This comparative example includes most of the operation steps of example 1 except that a thermally conductive protective layer is disposed between the electrically conductive pattern and the encapsulation layer. The preparation method comprises the following steps:
(1) carrying out corona pretreatment on the substrate to control the surface dyne value of the substrate to be 45-55 mN/m;
(2) coating polyimide slurry on the surface of the pretreated substrate and curing to obtain a polyimide layer, wherein the solid content of the polyimide slurry is 20%, and the coating film-forming technological parameters are as follows: the pumping flow is 15ml/s, the speed of a coating machine is 10m/min, the coating head gap is 50um, and the thickness of the polyimide layer is controlled to be 10 um;
(3) according to the design of an electrode pattern, a conductive groove is formed in a polyimide layer by using laser, the laser wavelength is 278-355nm, the output power is 10W, the pulse width is 5-500 ns adjustable, the repetition frequency is 20-100KHz, the conductive film is scanned and processed by a scanning galvanometer and an XY moving platform, the slotting angle is controlled to be 45 degrees, and the slotting depth is 0.11 um;
(4) filling the nano-silver conductive ink into the conductive groove sprayed with the heat-conducting ink, drying and curing, wherein the content of Ag in the nano-silver conductive ink is 0.5%, the viscosity is 10cps, and the drying temperature is 100 ℃;
(5) removing redundant nano silver conductive ink outside the V-shaped conductive groove to obtain an electrode pattern, and peeling by coating a release agent, wherein the peeling force is controlled to be 20-25 g;
(6) and spraying heat-conducting ink on the surface of the polyimide coating with the obtained electrode pattern and curing to obtain a heat-conducting protective layer, wherein the thickness of the heat-conducting protective layer is 7nm, and the heat-conducting ink comprises the following components: 55 parts of polyimide resin, 25 parts of (gamma-butyrolactone: propylene glycol monomethyl ether) mixed solvent with the mass ratio of 1:1, 1 part of triethyl hexyl phosphoric acid dispersant, 20 parts of boron nitride conductive filler, 1 part of titanate coupling agent and 1 part of octadecyl amine oxide modified additive.
(7) Coating ultraviolet curing liquid on the surface of the heat-conducting protective layer and curing to obtain a transparent packaging layer, wherein the solid content of the ultraviolet curing liquid is 10%, and the coating film-forming technological parameters are as follows: the pumping flow is 10ml/s, the speed of a coating machine is 15m/min, the coating head gap is 100um, and the thickness of the transparent packaging layer is controlled to be 150 nm.
Test example
The electrodes prepared in examples 1 to 10 and comparative example 1 were subjected to performance tests, the test items being as follows:
(1) and (3) etching mark testing: adopting human eye test, judging the standard: the distance between the human eye and the device is 50cm, whether the device pattern is distinguished is taken as a reference, and the etching line cannot be distinguished is taken as an excellent value.
A: 50um and 30um etched lines can be resolved.
B: a 50um etch line can be resolved but a 30um etch line cannot be resolved.
C: etching line capable of not distinguishing 50um and 30um
(2) And (3) xenon lamp weather resistance test: radiation intensity 0.8W/m 2 The temperature is 40 ℃, the humidity is 55 percent, and the time is 1000 h;
(3) bending test: the bending angle is 180 degrees, the bending R is 3mm, and the times are 30W.
(4) Thermal conductivity test: and taking the conductive film manufactured by the pre-patterned conductive groove as a testing device, wherein the DC direct current electrifying time is 24h, 48h and 72h respectively, and the handheld infrared thermometer is used for testing the surface temperature of the device at different time nodes.
The test results are shown in tables 1-3.
TABLE 1
TABLE 2
TABLE 3
The transparent flexible thin film electrode prepared in the embodiment 1-3 is disclosed by the invention, and the test results show that the cross section shape of the electrode can be controlled by pre-burying the conductive groove, the edge of the prepared electrode pattern is flat, the etching trace of the electrode is weak, the integral appearance is improved, the response speed of the prepared electrode is 2-5s, the bending resistance times are more than 30 ten thousand times, the temperature is 35-50 ℃ after heating for 72 hours, the heat conduction performance is good, and the service life is greatly prolonged.
Examples 1 and 4 to 7 are comparative experiments on conductive trenches, wherein examples 4 to 7 are studies on the grooving angles of conductive trenches, the grooving angles of conductive trenches affect the compaction density of nano-silver conductive ink in the trenches, and further affect the lapping condition of conductive lines, the grooving angles of examples 4 to 5 are 0 ° and 80 °, respectively, the etching marks are severe, and poor bending resistance is manifested as cracks and whitening marks; embodiments 6 to 7 relate to the research on the groove depth of the conductive groove, the groove depth of the conductive groove actually reflects the filling depth of the conductive pattern, the groove depths of embodiments 6 to 7 are 0.02um and 0.25um, respectively, the groove depth is too small, the filling amount of the conductive material is low, the touch response speed is slow, the response is insensitive, the groove depth is too large, the etching mark is severe, and the contact resistance is large.
Examples 1, 8-9 and comparative examples 1-2 are comparative experiments on a heat conductive protective layer, wherein the thickness of the heat conductive protective layer in example 8 is 25nm, the heat conductive protective layer is too thick, the contact resistance is increased, the bending property is reduced, and microcracks occur; example 9 no modifying additive was added to the thermally conductive ink of the thermally conductive protective layer, which resulted in a decrease in the thermal conductivity of the thermally conductive ink, affecting the thermal conductivity of the electrode; comparative example 1, no heat-conducting protective layer is arranged, the heat conductivity of the electrode is poor, and the temperature is 120 ℃ after heating for 72 hours; comparative example 2 sets up the heat conduction protective layer between electrically conductive pattern and packaging layer, on the one hand the heat conduction printing ink quantity increases, has increased electrode thickness simultaneously, and on the other hand contact resistance grow, influences the response speed and the sensitivity of touch-control.
In conclusion, the transparent flexible film electrode prepared by the method has the advantages of good heat conductivity, high response speed, good surface quality, long service life and good popularization and application values.
The present invention has been further described with reference to specific embodiments, but it should be understood that the detailed description should not be construed as limiting the spirit and scope of the present invention, and various modifications made to the above-described embodiments by those of ordinary skill in the art after reading this specification are within the scope of the present invention.
Claims (10)
1. A method for manufacturing a transparent flexible film electrode is characterized by comprising the following steps:
(1) pretreating the surface of the substrate;
(2) coating polyimide slurry on the surface of the pretreated substrate and curing to obtain a polyimide layer;
(3) forming a conductive groove on the polyimide layer according to the electrode pattern design;
(4) spraying heat-conducting ink in the electric conduction groove and curing to obtain a heat-conducting protective layer;
(5) filling the nano-silver conductive ink into the conductive groove sprayed with the heat-conducting ink, and drying and curing;
(6) removing the redundant nano silver conductive ink outside the conductive groove to obtain an electrode pattern;
(7) and coating ultraviolet curing liquid on the surface of the polyimide coating with the obtained electrode pattern and curing to obtain the transparent packaging layer.
2. The method for manufacturing the transparent flexible thin film electrode according to claim 1, wherein the dyne value of the surface of the substrate after pretreatment in step (1) is controlled to be 40-60mN/m, and the thickness of the polyimide layer in step (2) is 5-15 um.
3. The method according to claim 1, wherein the conductive trench in step (3) is a V-shaped conductive trench, and the V-shaped conductive trench is formed by laser grooving.
4. The method for manufacturing the transparent flexible thin film electrode according to claim 3, wherein the groove angle of the V-shaped conductive groove is 10-80 degrees, and the groove depth is 0.05-0.15 um.
5. The method for manufacturing the transparent flexible thin film electrode according to claim 1, wherein the thickness of the heat-conducting protective layer in the step (4) is 3-10 nm.
6. The method for manufacturing a transparent flexible thin film electrode according to claim 1, wherein the heat conductive ink is composed of the following components:
50-65% of matrix resin;
0.5 to 1.0 percent of dispersant;
10-25% of organic solvent;
10-25% of heat-conducting filler;
0.5 to 1.0 percent of coupling agent; and (c) a second step of,
0.5 to 1.0 percent of modified additive.
7. The method for manufacturing the transparent flexible thin-film electrode according to claim 6, wherein the heat conductive filler is selected from one of graphene, silicon carbide, boron nitride, silicon nitride, aluminum oxide and zinc oxide; the coupling agent is selected from one of silane coupling agent, titanate coupling agent, aluminate coupling agent, bimetallic coupling agent, phosphate coupling agent and borate coupling agent.
8. The method of claim 6, wherein the modifying additive is at least one selected from octadecylamine, octadecylamine oxide, polydopamine, 1-pyrenebutanoic acid, and chlorosulfonic acid.
9. The method for manufacturing the transparent flexible thin film electrode according to claim 1, wherein the step (6) of removing the excess nano silver conductive ink outside the conductive groove comprises the following specific steps: and coating a release agent outside the cured nano-silver conductive ink to obtain a release layer, controlling the stripping force of the release layer to be 10-30 g, and then stripping the release layer to remove the redundant nano-silver conductive ink to obtain an electrode pattern.
10. The method as claimed in claim 1, wherein the thickness of the transparent encapsulating layer in step (7) is 100-200 nm.
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| CN116445037A (en) * | 2023-06-16 | 2023-07-18 | 合肥晶合集成电路股份有限公司 | Metal nano ink and preparation method thereof, and preparation method of semiconductor structure |
| CN116445037B (en) * | 2023-06-16 | 2023-10-03 | 合肥晶合集成电路股份有限公司 | Metal nano ink and preparation method thereof, and preparation method of semiconductor structure |
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