CN113045935A - High-thermal-stability conductive ink applied to flexible circuit and preparation method thereof - Google Patents
High-thermal-stability conductive ink applied to flexible circuit and preparation method thereof Download PDFInfo
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- CN113045935A CN113045935A CN201911366712.4A CN201911366712A CN113045935A CN 113045935 A CN113045935 A CN 113045935A CN 201911366712 A CN201911366712 A CN 201911366712A CN 113045935 A CN113045935 A CN 113045935A
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- 238000002360 preparation method Methods 0.000 title abstract description 12
- 229920000144 PEDOT:PSS Polymers 0.000 claims abstract description 72
- 239000011230 binding agent Substances 0.000 claims abstract description 47
- 239000003960 organic solvent Substances 0.000 claims abstract description 41
- 239000002562 thickening agent Substances 0.000 claims abstract description 36
- 239000002071 nanotube Substances 0.000 claims abstract description 31
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 28
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 27
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 27
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 27
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 13
- -1 Polytetrafluoroethylene Polymers 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 39
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 16
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 14
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 12
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 12
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 12
- 150000002148 esters Chemical class 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 12
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 12
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 12
- 238000009210 therapy by ultrasound Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 239000002202 Polyethylene glycol Substances 0.000 claims description 10
- 229920001223 polyethylene glycol Polymers 0.000 claims description 10
- YFSUTJLHUFNCNZ-UHFFFAOYSA-M 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctane-1-sulfonate Chemical compound [O-]S(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YFSUTJLHUFNCNZ-UHFFFAOYSA-M 0.000 claims description 7
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000007650 screen-printing Methods 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 239000013530 defoamer Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000853 adhesive Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 230000002687 intercalation Effects 0.000 abstract description 3
- 238000009830 intercalation Methods 0.000 abstract description 3
- 229920001467 poly(styrenesulfonates) Polymers 0.000 abstract description 3
- 239000012760 heat stabilizer Substances 0.000 abstract description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract 2
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract 2
- 238000001723 curing Methods 0.000 description 16
- 239000000463 material Substances 0.000 description 15
- 239000000243 solution Substances 0.000 description 10
- 238000007639 printing Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000011231 conductive filler Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 238000013019 agitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229960002796 polystyrene sulfonate Drugs 0.000 description 1
- 239000011970 polystyrene sulfonate Substances 0.000 description 1
Classifications
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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
- C09D11/52—Electrically conductive inks
-
- 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
-
- 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
-
- 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
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C09D11/14—Printing inks based on carbohydrates
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
- H05K1/092—Dispersed materials, e.g. conductive pastes or inks
- H05K1/097—Inks comprising nanoparticles and specially adapted for being sintered at low temperature
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Dispersion Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a high-thermal-stability conductive ink applied to a flexible circuit and a preparation method thereof. The adhesive is characterized by being mainly prepared from poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate, tetraethoxysilane, kaolin nanotubes, an organic solvent, a binder, a defoaming agent, a thickening agent and deionized water; the weight portions of the raw materials are as follows: 40-60 parts of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate, 3-10 parts of tetraethoxysilane, 5-30 parts of kaolin nanotubes, 25-100 parts of organic solvent, 12-26 parts of binder, 2-8 parts of defoaming agent, 4-8 parts of thickening agent and 30-50 parts of deionized water. According to the invention, through selection of the binder and use of the heat stabilizer, the intercalation effect of PEDOT (Polytetrafluoroethylene)/PSS (Polytetrafluoroethylene) in the kaolin nanotube is utilized, and the micropores and the inner core of the nanotube are filled and the surface of the nanotube is covered, so that the thermal stability, the adhesiveness and the electric conductivity of the ink are effectively improved, and the ink has the advantages of low cost, excellent thermal stability and electric conductivity and wide application prospect.
Description
Technical Field
The invention belongs to the technical field of conductive ink materials, and particularly relates to high-thermal-stability conductive ink applied to a flexible circuit and a preparation method thereof.
Background
The in-mold electronic technology (IME) is a new technology that combines in-mold film coating and printed electronics together, and can upgrade in-mold decoration products into intelligent electronic functional products. The ink is a key material for restricting the development of printed electronic technology, is a hotspot and a difficult point of research at home and abroad at present, and also limits the popularization and application of the IME technology to a great extent. The printing requirement of a general flexible circuit is very high in thermal stability, and when the circuit is formed along with the diaphragm, the ink cannot be decomposed, discolored, broken and the like; in addition, the printed circuit is required to have good conductive performance, and can meet the design requirements of different conductive circuits. The traditional conductive ink is low in curing temperature, and the phenomena of flexible circuit fracture and resistance increase caused by stretching deformation can occur when the flexible circuit is formed along with the membrane. The research on the preparation process of the ink material is one of effective ways for improving the thermal stability, the electric conductivity and the adhesive force of the printed flexible circuit.
Disclosure of Invention
The invention aims to provide a high-thermal-stability conductive ink applied to a flexible circuit and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: a high-thermal stability conductive ink applied to a flexible circuit is characterized in that the conductive ink is mainly prepared from poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS), tetraethoxysilane, kaolin nanotubes, an organic solvent, a binder, a defoaming agent, a thickening agent and deionized water; the weight portions of the raw materials are as follows: 40-60 parts of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS), 3-10 parts of tetraethoxysilane, 5-30 parts of kaolin nanotubes, 25-100 parts of organic solvent, 12-26 parts of binder, 2-8 parts of defoaming agent, 4-8 parts of thickening agent and 30-50 parts of deionized water.
The poly (3, 4-ethylenedioxythiophene): polystyrene sulfonate (PEDOT: PSS) is a conductive filler, and the function of the conductive filler is to improve the conductivity of the ink. The tetraethoxysilane is a stabilizer, abbreviated as TEOS. The kaolin nanotubes are heat stabilizers, abbreviated as HNTs, which act to improve the thermal stability of the ink.
Preferably, the organic solvent is any one or a mixture of any two or more (including two) of isopropanol, dimethyl sulfoxide, N-dimethyl amide, tetrahydrofuran and perfluorooctane sulfonate in any proportion.
Preferably, when the organic solvent is isopropanol, dimethyl sulfoxide, N-dimethyl amide, tetrahydrofuran and perfluorooctane sulfonate, the mass ratio of the organic solvent to the organic solvent is 5:10:4:1: 5.
Preferably, the binder is polyvinyl alcohol ester and sodium carboxymethyl cellulose, and the mass ratio of the polyvinyl alcohol ester to the sodium carboxymethyl cellulose is 10:3, so that the adhesion of the ink is improved.
Preferably, the antifoaming agent is polyethylene glycol with a molecular weight of 1000, which serves to avoid air bubbles during ink agitation.
Preferably, the thickener is a PTF thickener.
The preparation method of the high-thermal-stability conductive ink applied to the flexible circuit is characterized by comprising the following steps of:
1) the weight portions of the raw materials are as follows: 40-60 parts of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS), 3-10 parts of tetraethoxysilane, 5-30 parts of kaolin nanotube, 25-100 parts of organic solvent, 12-26 parts of binder, 2-8 parts of defoaming agent, 4-8 parts of thickening agent and 30-50 parts of deionized water, wherein the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS), tetraethoxysilane, kaolin nanotube, organic solvent, binder, defoaming agent, thickening agent and deionized water are selected for standby;
2) dispersing poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) in an organic solvent, and magnetically stirring for 30-45min to obtain a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) dispersion liquid;
adding the binder into deionized water, heating and stirring at 30-50 ℃ for 2-2.5h to obtain binder liquid for later use;
3) adding kaolin nanotubes (HNTs) and a binder solution into a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) dispersion solution at room temperature, and magnetically stirring uniformly to obtain a mixed solution;
4) adding tetraethoxysilane, a defoaming agent and a thickening agent into the mixed solution, and carrying out ultrasonic treatment under the stirring condition to obtain the high-thermal-stability conductive ink applied to the flexible circuit;
preferably, in the step 3), the stirring speed is 800r/min, and the stirring time is 18-20 h.
Preferably, in the step 4), the ultrasonic treatment power is 1000W, and the ultrasonic time is 15-20 min.
The application comprises the following steps: printing high-thermal-stability conductive ink applied to a flexible circuit on a PET substrate by a screen printing method, and drying and curing to obtain a flexible printed circuit; the drying and curing temperature is 150-200 ℃, and the curing time is 4-10 min.
Compared with the prior art, the invention has the beneficial effects that: the invention provides the high-thermal-stability conductive ink applied to the flexible circuit and the preparation method thereof by reasonably designing a formula and selecting a binder, a stabilizer and an organic solvent, utilizing the intercalation effect (intercalation effect in HNTs) of PEDOT (PSS) in kaolin nanotubes, filling micropores and inner cores of the nanotubes and covering the surfaces of the nanotubes, and being suitable for forming a printed circuit following a membrane in an in-mold electronic technology, so that the prepared ink has excellent thermal stability, conductivity and adhesion performance, low cost and wide application prospect.
Detailed Description
The following detailed description is of specific embodiments of the invention, which are presented as part of the specification, and is intended to illustrate the principles, features, and advantages of the invention by way of example, and to enable one skilled in the art to more readily understand the invention.
The embodiment of the invention comprises the following steps:
example 1
A high-thermal stability conductive ink applied to a flexible circuit is prepared from poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS), tetraethoxysilane, kaolin nanotubes, an organic solvent, a binder, a defoaming agent, a thickening agent and deionized water; the weight portions of the raw materials are as follows: 40 parts of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS), 3 parts of tetraethoxysilane, 5 parts of kaolin nanotubes, 25 parts of organic solvent, 12 parts of binder, 2 parts of defoamer, 4 parts of thickener and 30 parts of deionized water.
When the organic solvent is isopropanol, dimethyl sulfoxide, N-dimethyl amide, tetrahydrofuran and perfluorooctane sulfonate, the mass ratio of the organic solvent to the organic solvent is 5:10:4:1: 5.
The binder is polyvinyl alcohol ester and sodium carboxymethylcellulose, and the mass ratio of the polyvinyl alcohol ester to the sodium carboxymethylcellulose is 10: 3. The defoaming agent is polyethylene glycol, and the molecular weight of the polyethylene glycol is 1000. The thickener is a PTF thickener.
The preparation method of the high-thermal-stability conductive ink applied to the flexible circuit comprises the following steps:
1) selecting the raw materials according to the proportion for later use;
2) dispersing poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) in an organic solvent, and magnetically stirring for 30min to obtain a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) dispersion liquid;
adding the binder into deionized water, heating and stirring for 2 hours at 35 ℃ to obtain binder liquid for later use;
3) adding kaolin nanotubes (HNTs) and a binder solution into a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) dispersion solution at room temperature, and magnetically stirring uniformly to obtain a mixed solution; the stirring speed is 800r/min, and the stirring time is 18 h;
4) adding tetraethoxysilane, a defoaming agent and a thickening agent into the mixed solution, and carrying out ultrasonic treatment under the stirring condition to obtain the high-thermal-stability conductive ink applied to the flexible circuit; the ultrasonic treatment power is 1000W, and the ultrasonic time is 15 min.
The application comprises the following steps: printing high-thermal-stability conductive ink applied to a flexible circuit on a PET substrate by a screen printing method, and drying and curing to obtain a flexible printed circuit; the drying and curing temperature is 150 ℃, and the curing time is 4 min.
After the conductive ink prepared by the invention is kept at the high temperature of 150 ℃ for 4min, the conductivity reaches 636S/cm, and the color difference value is small; the adhesive force grade is 2 grade; the prepared conductive ink is ground into powder, the thermal stability and the mass loss of the ink material are detected when the temperature is increased to 800 ℃ from room temperature at the speed of 10 ℃/min under the nitrogen atmosphere, and when the temperature reaches 800 ℃, the material still keeps 50% of the mass, which shows that the thermal stability of the composite material is increased compared with that of a pure poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) material, and the conductive ink prepared by the invention has stronger comprehensive performance.
Example 2
A high-thermal stability conductive ink applied to a flexible circuit is prepared from poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS), tetraethoxysilane, kaolin nanotubes, an organic solvent, a binder, a defoaming agent, a thickening agent and deionized water; the weight portions of the raw materials are as follows: 60 parts of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS), 10 parts of tetraethoxysilane, 30 parts of kaolin nanotubes, 100 parts of organic solvent, 26 parts of binder, 8 parts of defoaming agent, 8 parts of thickening agent and 50 parts of deionized water.
When the organic solvent is isopropanol, dimethyl sulfoxide, N-dimethyl amide, tetrahydrofuran and perfluorooctane sulfonate, the mass ratio of the organic solvent to the organic solvent is 5:10:4:1: 5. The binder is polyvinyl alcohol ester and sodium carboxymethylcellulose, the mass ratio of the polyvinyl alcohol ester to the sodium carboxymethylcellulose is 10:3, and the binder has the function of improving the ink adhesiveness. The defoaming agent is polyethylene glycol, the molecular weight of the polyethylene glycol is 1000, and the defoaming agent has the function of avoiding bubbles in the ink stirring process. The thickener is a PTF thickener.
The preparation method of the high-thermal-stability conductive ink applied to the flexible circuit comprises the following steps:
1) selecting the raw materials according to the proportion for later use;
2) dispersing poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) in an organic solvent, and magnetically stirring for 30min to obtain a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) dispersion liquid;
adding the binder into deionized water, heating and stirring for 2 hours at 35 ℃ to obtain binder liquid for later use;
3) adding kaolin nanotubes (HNTs) and a binder solution into a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) dispersion solution at room temperature, and magnetically stirring uniformly to obtain a mixed solution; the stirring speed is 800r/min, and the stirring time is 20 h;
4) adding tetraethoxysilane, a defoaming agent and a thickening agent into the mixed solution, and carrying out ultrasonic treatment under the stirring condition to obtain the high-thermal-stability conductive ink applied to the flexible circuit; the ultrasonic treatment power is 1000W, and the ultrasonic time is 20 min.
The application comprises the following steps: printing high-thermal-stability conductive ink applied to a flexible circuit on a PET substrate by a screen printing method, and drying and curing to obtain a flexible printed circuit; the drying and curing temperature is 200 ℃, and the curing time is 10 min.
After the conductive ink prepared by the invention is kept at the high temperature of 200 ℃ for 10min, the conductivity reaches 1700S/cm, and the color difference value is small; the adhesion grade is 1 grade; the prepared conductive ink is ground into powder, the thermal stability and the mass loss of the ink material are detected when the temperature is increased to 800 ℃ from room temperature at the speed of 10 ℃/min under the nitrogen atmosphere, and the material still keeps 80% of the mass when the temperature reaches 800 ℃, which shows that the thermal stability of the composite material is increased compared with that of a pure poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) material, and the conductive ink prepared by the invention has stronger comprehensive performance.
Example 3
A high-thermal stability conductive ink applied to a flexible circuit is prepared from poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS), tetraethoxysilane, kaolin nanotubes, an organic solvent, a binder, a defoaming agent, a thickening agent and deionized water; the weight portions of the raw materials are as follows: 50 parts of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS), 6 parts of tetraethoxysilane, 20 parts of kaolin nanotubes, 60 parts of organic solvent, 20 parts of binder, 6 parts of defoaming agent, 6 parts of thickening agent and 40 parts of deionized water.
When the organic solvent is isopropanol, dimethyl sulfoxide, N-dimethyl amide, tetrahydrofuran and perfluorooctane sulfonate, the mass ratio of the organic solvent to the organic solvent is 5:10:4:1: 5. The binder is polyvinyl alcohol ester and sodium carboxymethylcellulose, the mass ratio of the polyvinyl alcohol ester to the sodium carboxymethylcellulose is 10:3, and the binder has the function of improving the ink adhesiveness. The defoaming agent is polyethylene glycol, the molecular weight of the polyethylene glycol is 1000, and the defoaming agent has the function of avoiding bubbles in the ink stirring process. The thickener is a PTF thickener.
The preparation method of the high-thermal-stability conductive ink applied to the flexible circuit comprises the following steps:
1) selecting the raw materials according to the proportion for later use;
2) dispersing poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) in an organic solvent, and magnetically stirring for 30min to obtain a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) dispersion liquid;
adding the binder into deionized water, heating and stirring for 2 hours at 35 ℃ to obtain binder liquid for later use;
3) adding kaolin nanotubes (HNTs) and a binder solution into a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) dispersion solution at room temperature, and magnetically stirring uniformly to obtain a mixed solution; the stirring speed is 800r/min, and the stirring time is 19 h;
4) adding tetraethoxysilane, a defoaming agent and a thickening agent into the mixed solution, and carrying out ultrasonic treatment under the stirring condition to obtain the high-thermal-stability conductive ink applied to the flexible circuit; the ultrasonic treatment power is 1000W, and the ultrasonic time is 18 min.
The application comprises the following steps: printing high-thermal-stability conductive ink applied to a flexible circuit on a PET substrate by a screen printing method, and drying and curing to obtain a flexible printed circuit; the drying and curing temperature is 180 ℃, and the curing time is 6 min.
The conductivity of the conductive ink prepared by the invention reaches 1300S/cm after the conductive ink is kept at a high temperature of 180 ℃ for 6min, and the color difference value is small; the adhesion grade is 1 grade; the prepared conductive ink is ground into powder, the thermal stability and the mass loss of the ink material are detected when the temperature is increased to 800 ℃ from room temperature at the speed of 10 ℃/min under the nitrogen atmosphere, and when the temperature reaches 800 ℃, the material still keeps 65% of mass, which shows that the thermal stability of the composite material is increased compared with that of a pure poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) material, and the conductive ink prepared by the invention has stronger comprehensive performance.
Example 4
A high-thermal stability conductive ink applied to a flexible circuit is prepared from poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS), tetraethoxysilane, kaolin nanotubes, an organic solvent, a binder, a defoaming agent, a thickening agent and deionized water; the weight portions of the raw materials are as follows: 55 parts of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS), 7 parts of tetraethoxysilane, 25 parts of kaolin nanotubes, 70 parts of organic solvent, 21 parts of binder, 7 parts of defoamer, 5 parts of thickener and 45 parts of deionized water.
The organic solvent is isopropanol. The binder is polyvinyl alcohol ester and sodium carboxymethylcellulose, the mass ratio of the polyvinyl alcohol ester to the sodium carboxymethylcellulose is 10:3, and the binder has the function of improving the ink adhesiveness. The defoaming agent is polyethylene glycol, the molecular weight of the polyethylene glycol is 1000, and the defoaming agent has the function of avoiding bubbles in the ink stirring process. The thickener is a PTF thickener.
The preparation method of the high-thermal-stability conductive ink applied to the flexible circuit comprises the following steps:
1) selecting the raw materials according to the proportion for later use;
2) dispersing poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) in an organic solvent, and magnetically stirring for 45min to obtain a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) dispersion liquid;
adding the binder into deionized water, heating and stirring at 50 ℃ for 2.5 hours to obtain binder liquid for later use;
3) adding kaolin nanotubes (HNTs) and a binder solution into a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) dispersion solution at room temperature, and magnetically stirring uniformly to obtain a mixed solution; the stirring speed is 800r/min, and the stirring time is 20 h;
4) adding tetraethoxysilane, a defoaming agent and a thickening agent into the mixed solution, and carrying out ultrasonic treatment under the stirring condition to obtain the high-thermal-stability conductive ink applied to the flexible circuit; the ultrasonic treatment power is 1000W, and the ultrasonic time is 15 min.
The application comprises the following steps: printing high-thermal-stability conductive ink applied to a flexible circuit on a PET substrate by a screen printing method, and drying and curing to obtain a flexible printed circuit; the drying and curing temperature is 150 ℃, and the curing time is 10 min.
After the conductive ink prepared by the invention is kept at the high temperature of 150 ℃ for 10min, the conductivity reaches 758S/cm, and the color difference value is small; the adhesive force grade is 2 grade; the prepared conductive ink is ground into powder, the thermal stability and the mass loss of the ink material are detected when the temperature is increased to 800 ℃ from room temperature at the speed of 10 ℃/min under the nitrogen atmosphere, and when the temperature reaches 800 ℃, the material still keeps 50% of the mass, which shows that the thermal stability of the composite material is increased compared with that of a pure poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) material, and the conductive ink prepared by the invention has stronger comprehensive performance.
Table 1 shows the performance indexes of the examples.
Table 1:
the above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and it should be noted that, for those skilled in the art, all modifications and variations which do not depart from the spirit of the present invention should be construed as being included within the scope of the present invention.
Claims (10)
1. A high-thermal stability conductive ink applied to a flexible circuit is characterized in that the conductive ink is mainly prepared from poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate, tetraethoxysilane, kaolin nanotubes, an organic solvent, a binder, a defoaming agent, a thickening agent and deionized water; the weight portions of the raw materials are as follows: 40-60 parts of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate, 3-10 parts of tetraethoxysilane, 5-30 parts of kaolin nanotubes, 25-100 parts of organic solvent, 12-26 parts of binder, 2-8 parts of defoaming agent, 4-8 parts of thickening agent and 30-50 parts of deionized water.
2. The conductive ink with high thermal stability for flexible circuits as claimed in claim 1, wherein the organic solvent is one or a mixture of two or more selected from isopropanol, dimethyl sulfoxide, N-dimethyl amide, tetrahydrofuran and perfluorooctane sulfonate.
3. A high thermal stability conductive ink for flexible circuit as claimed in claim 1 or 2, wherein the organic solvent is isopropanol, dimethyl sulfoxide, N-dimethyl amide, tetrahydrofuran and perfluorooctane sulfonate at a mass ratio of 5:10:4:1: 5.
4. The conductive ink with high thermal stability for the flexible circuit as claimed in claim 1, wherein the binder is polyvinyl alcohol ester and sodium carboxymethyl cellulose, and the mass ratio of the polyvinyl alcohol ester to the sodium carboxymethyl cellulose is 10: 3.
5. A highly thermally stable conductive ink for flexible circuits according to claim 1 wherein said defoamer is polyethylene glycol having a molecular weight of 1000.
6. A thermally stable conductive ink for application to flexible circuits according to claim 1 wherein said thickener is a PTF thickener.
7. A method of making a highly thermally stable conductive ink for flexible circuits according to claim 1, comprising the steps of:
1) the weight portions of the raw materials are as follows: 40-60 parts of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate, 3-10 parts of tetraethoxysilane, 5-30 parts of kaolin nanotubes, 25-100 parts of organic solvent, 12-26 parts of binder, 2-8 parts of defoamer, 4-8 parts of thickener and 30-50 parts of deionized water, wherein the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate, tetraethoxysilane, kaolin nanotubes, organic solvent, binder, defoamer, thickener and deionized water are selected for standby;
2) dispersing poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate in an organic solvent, and magnetically stirring for 30-45min to obtain a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate dispersion liquid;
adding the binder into deionized water, heating and stirring at 30-50 ℃ for 2-2.5h to obtain binder liquid for later use;
3) adding the kaolin nanotube and the binder liquid into the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate dispersion liquid at room temperature, and uniformly stirring by magnetic force to obtain a mixed solution;
4) and adding tetraethoxysilane, a defoaming agent and a thickening agent into the mixed solution, and carrying out ultrasonic treatment under the stirring condition to obtain the high-thermal-stability conductive ink applied to the flexible circuit.
8. The method as claimed in claim 7, wherein in step 3), the stirring speed is 800r/min and the stirring time is 18-20 h.
9. The method as claimed in claim 7, wherein in step 4), the ultrasonic treatment power is 1000W, and the ultrasonic time is 15-20 min.
10. The application of the high thermal stability conductive ink for the flexible circuit as claimed in the claims 1 to 6, wherein the high thermal stability conductive ink for the flexible circuit is printed on the PET substrate by a screen printing method, dried and cured to obtain the flexible printed circuit; the drying and curing temperature is 150-200 ℃, and the curing time is 4-10 min.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103804995A (en) * | 2012-11-09 | 2014-05-21 | 财团法人工业技术研究院 | Conductive ink composition and transparent conductive film |
| CN103923335A (en) * | 2014-05-08 | 2014-07-16 | 郑州大学 | PEDOT : PSS/kaolin nanotube composite materials and manufacturing method thereof |
| CN105385242A (en) * | 2015-12-28 | 2016-03-09 | 王璐 | Stable conductive printing ink |
| CN107384025A (en) * | 2017-08-10 | 2017-11-24 | 珠海纳金科技有限公司 | One kind spraying electrically conducting transparent ink and its preparation method and application |
| CN108219593A (en) * | 2017-05-03 | 2018-06-29 | 上海幂方电子科技有限公司 | A kind of flexible capacitor electrode ink scratched and preparation method thereof |
-
2019
- 2019-12-26 CN CN201911366712.4A patent/CN113045935A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103804995A (en) * | 2012-11-09 | 2014-05-21 | 财团法人工业技术研究院 | Conductive ink composition and transparent conductive film |
| CN103923335A (en) * | 2014-05-08 | 2014-07-16 | 郑州大学 | PEDOT : PSS/kaolin nanotube composite materials and manufacturing method thereof |
| CN105385242A (en) * | 2015-12-28 | 2016-03-09 | 王璐 | Stable conductive printing ink |
| CN108219593A (en) * | 2017-05-03 | 2018-06-29 | 上海幂方电子科技有限公司 | A kind of flexible capacitor electrode ink scratched and preparation method thereof |
| CN107384025A (en) * | 2017-08-10 | 2017-11-24 | 珠海纳金科技有限公司 | One kind spraying electrically conducting transparent ink and its preparation method and application |
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