CN108129913A - Watersoluble plumbago alkene electrically conductive ink and preparation method thereof - Google Patents

Watersoluble plumbago alkene electrically conductive ink and preparation method thereof Download PDF

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Publication number
CN108129913A
CN108129913A CN201711449353.XA CN201711449353A CN108129913A CN 108129913 A CN108129913 A CN 108129913A CN 201711449353 A CN201711449353 A CN 201711449353A CN 108129913 A CN108129913 A CN 108129913A
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Prior art keywords
electrically conductive
conductive ink
watersoluble plumbago
plumbago alkene
agent
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Inventor
李冰
王东卫
丁显波
刘克
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Shenzhen Guochuang Jiawei Graphene Technology Co Ltd
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Shenzhen Guochuang Jiawei Graphene Technology Co Ltd
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Priority to CN201711449353.XA priority Critical patent/CN108129913A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/52Electrically conductive inks
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/03Printing inks characterised by features other than the chemical nature of the binder
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/03Printing inks characterised by features other than the chemical nature of the binder
    • C09D11/033Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/10Printing inks based on artificial resins
    • C09D11/106Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C09D11/107Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)

Abstract

The present invention provides a kind of watersoluble plumbago alkene electrically conductive ink, it includes being prepared by the raw material of following parts by weight, graphene dispersing solution 20 85, conductive black 2000 be 4 40 solvents 5 15, graphite powder 5 38, binder 20 45, antifoaming agent 0.1 2.9, levelling agent 0.05 0.5, adhesion promoter 1.0 15, PH conditioning agents 0.05 0.5.The slow drying speed of the watersoluble plumbago alkene electrically conductive ink of the present invention in screen printing process, the phenomenon that will not causing network blocking version because of the quick volatilization of solvent, can meet the requirement that industrialization is continuous, repeatedly prints.

Description

Watersoluble plumbago alkene electrically conductive ink and preparation method thereof
Technical field
The present invention relates to flexible printing electronic field more particularly to a kind of slow curing type watersoluble plumbago alkene electrically conductive ink and its Preparation method.
Background technology
With the development of material science and technology, flexible printing electronic technology is also being constantly progressive, unique flexible, extension Property and efficiently, low cost manufacturing technique, it is often more important that discharging of waste liquid brought based on Conventional printing process etc. can be eliminated Environmental issue is a kind of environmentally friendly manufacturing technology.Therefore, flexible printing electronic technology has wide application prospect in various fields, Such as flexible electronic displays, Organic Light Emitting Diode OLED, printed wiring board, blood sugar test paper, printing RFID, thin film solar Solar panel, electronics surface mount etc..
The Chemical market many places of China in 2017 are under the pattern of environmental protection concussion, especially most middle-size and small-size paintings in downstream Material enterprise faces the situation that limited production even stops production.The Environmental Protection Situation that Chinese Enterprises face is more acute, and harsh environmental regulation falls Enterprise is closed to green, harmonious, sustainable development.Therefore, for flexible printing electronics industry, watersoluble plumbago alkene electrically conductive ink Using deionized water as primary solvent, the volatile organic solvent contained is less, caused by environment harm it is less, meet very much Country is to the policy requirements of chemical industry at present.
And the rate of drying of current watersoluble plumbago alkene electrically conductive ink is very fast, it is quick with solvent in silk-screen printing The phenomenon that volatilization, solid part under remaining can cause network blocking version, halftone need to be through that could use for second after over cleaning, Wu Fada To the print production of rapid continuous, this brings certain difficulty to the industrial production of aqueous Graphene conductive ink.
Invention content
A kind of watersoluble plumbago alkene electrically conductive ink for being designed to provide slow curing type of the technical program embodiment and its preparation Method, prepared watersoluble plumbago alkene electrically conductive ink have slow drying speed, quick continuous printing can be achieved, and aqueous molten Agent is pollution-free.
The present invention provides a kind of watersoluble plumbago alkene electrically conductive ink, including being prepared by the raw material of following parts by weight,
Graphene dispersing solution 20-85;
2000 4-40 of conductive black;
Solvent 5-15;
Graphite powder 5-38;
Binder 20-45;
Antifoaming agent 0.1-2.9;
Levelling agent 0.05-0.5;
Adhesion promoter 1.0-15;
PH conditioning agents 0.05-0.5.
The binder is aqueous thermal-curable acrylic resin, aqueous alkide resin, aqueous polyester resin, water-base epoxy One or more in resin, waterborne polyurethane resin;The aqueous alkyl-modified organic silicon defoamer of the antifoaming agent, Organic silicone antifoaming agent, high-molecular-weight propylene acid ester homopolymer non-silicon defoaming agent, low molecular weight propylene acid ester homopolymer non-silicon disappear One or more in infusion;The levelling agent is polyether-modified dimethyl silicone polymer aqueous levelling agent, aqueous poly- One or more in urethane levelling agent;The adhesion promoter is silane coupling agent class adhesion promoter, titanium One or more in acid esters coupling agent class adhesion promoter, resinae adhesion promoter;The solvent is goes One or more in ionized water, absolute ethyl alcohol, ammonium hydroxide.
The PH conditioning agents are one or more.
The present invention also provides a kind of preparation methods of watersoluble plumbago alkene electrically conductive ink, include the following steps:By 20-85 parts Graphene dispersing solution be added in the agitator tank of dispersion machine, and open stirring dispersion machine, rotating speed is set as 1000-2000r/ Min obtains solution A;5-10 parts of solvent, 20-45 parts of binder are continuously added into agitator tank, persistently stirs 10-15 Minute, obtain solution B;Solution B from dispersion machine agitator tank is taken out, is added in grinder, the parameter of grinder is set as 1000-2000r/min, pressure are set as 3.0-5.0MPa, and 4-40 parts of conductive charcoals are added in the backward solution B of grinding 30 minutes It is black, 5-38 parts of graphite powders, 0.1-2.9 parts of antifoaming agent, 0.05-0.5 part of levelling agent, 1.0-15 parts of adhesive force promotion Agent is ground to fineness≤5 μm of electrically conductive ink, obtains slurry C;Ammonium hydroxide is added in slurry C and deionized water adjusts rotation and glues Degree to 2000-3000MPa s, pH value is 7.5-9 to get watersoluble plumbago alkene electrically conductive ink.
It advantages of the present invention and has the beneficial effect that:
1. the slow drying speed of the watersoluble plumbago alkene electrically conductive ink of the present invention, will not be because of solvent in screen printing process The phenomenon that quickly volatilizing and causing network blocking version can meet the requirement that industrialization is continuous, repeatedly prints.Specifically, the water of the present invention Property Graphene conductive ink is by adding corresponding auxiliary agent, to reduce the rate of drying of watersoluble plumbago alkene electrically conductive ink.Aqueous stone The auxiliary agent added in black alkene electrically conductive ink is pH value adjustment agent.PH value adjustment agent dosage plays in watersoluble plumbago alkene electrically conductive ink Adjust Graphene conductive ink pH value, in watersoluble plumbago alkene conductive ink systems, pH value general control 7.5-9.0 it Between, the printability of water-based ink is best at this time;
2. the sheet resistance value of the watersoluble plumbago alkene electrically conductive ink of the present invention is 10-20 Ω/, electric conductivity is most better than existing market Conductive carbon paste;
3. for the watersoluble plumbago alkene electrically conductive ink of the present invention using deionized water as solvent, environment-friendly type is good and is practically free of organic wave Stimulating food(VOC), harm is not generated to electrically conductive ink production, operation, user of service;
4. watersoluble plumbago alkene electrically conductive ink obtained by the present invention is ground to ink fineness≤5 μm, printing precision is high, can with Screen printing screens with 100-300 mesh different sizes.Electrically conductive ink can meet flexible printing electronic device to electrically conductive ink Printing precision requirement.
Specific embodiment
The technical solution in the technical program embodiment is clearly and completely described below, it is clear that described Embodiment is only the technical program part of the embodiment, instead of all the embodiments.Based on the implementation in the technical program Example, those of ordinary skill in the art's all other embodiments obtained without creative efforts, belongs to The scope of protection of the invention.
Watersoluble plumbago alkene electrically conductive ink described in the embodiment of the present invention, including being prepared by the raw material of following parts by weight;
Graphene dispersing solution 20-85;
2000 4-40 of conductive black;
Solvent 5-15;
Graphite powder 5-38;
Binder 20-45;
Antifoaming agent 0.1-2.9;
Levelling agent 0.05-0.5;
N- methylethanolamines 0.5-10.0;
Adhesion promoter 1.0-15.
Wherein, graphene dispersing solution is 5% graphene dispersing solution prepared using liquid phase stripping method.
Wherein watersoluble plumbago alkene electrically conductive ink is 100 parts of weight meters, and the weight composition of each component is shown in Table 1:
Table 1
Component Mass fraction
Graphene dispersing solution 20—85
Conductive black 2000 5—40
Solvent 5.0—15
Graphite powder 15—38
Binder 20—45
Antifoaming agent 0.1—2.9
Levelling agent 0.05—0.5
N- methylethanolamines 0.5—10.0
Adhesion promoter 1.0—15
Raw material is commercially available convenient source used by the embodiment of the present invention.
The raw materials used supplier of following embodiment is specific as follows:
(1)Expanded graphite source is Qingdao Jin Tao graphite Co., Ltd, and specification is 100 mesh, fixed carbon content >=95%;
(2)Conductive black source is upper sea cowry Qing Li career developments Co., Ltd, and model is Cabot conductive black 2000;
(3)Graphite powder is nano graphite powder, and source reaches graphite Co., Ltd, model XF056 for Qingdao Tian Yuan;
(4)Ammonium hydroxide be concentration 20%, source be Hua Xisheng Chemical Co., Ltd.s of Foshan City, model(CAS accession number)For:1336- 21-6[2];
(5)Binder is aqueous thermosetting acrylic resin, and source can be reached for Canada(Heshan)Co., Ltd, model AC4060;
(6)Antifoaming agent be aqueous alkyl-modified organic silicon defoamer, source be Dongguan City De Feng antifoaming agent Co., Ltd, model For:DF-184;
(7)The polyether-modified dimethyl silicone polymer aqueous levelling agent of model of levelling agent, it is limited from Shanghai celestial being nation chemistry Company, model:BYK-348;
(8)Adhesion promoter source be Dongguan City Yi Lian Chinese workers Science and Technology Ltd., model EL-9501;
(9)NMP Shanghai Yuan Ji Industrial Co., Ltd.s, model(No. CAS)For:872-50-4;
(10)Cellulose filtering film, source are plasticized Science and Technology Ltd., model 006 for sea salt New Orient.
The graphene dispersing solution is a concentration of 0.3% graphene that expanded graphite is prepared through liquid phase stripping method Aqueous dispersions, the mass fraction that graphene aqueous dispersions account for conductive ink systems are 40% -70%, watersoluble plumbago alkene slurry source In Guo Chuanjiawei graphenes Science and Technology Ltd. of Shenzhen, preparation method is:Take 200 mesh expanded graphite be added to it is organic molten In agent NMP, and surfactant is added in into NMP(Cetyl trimethylammonium bromide)Ultrasonication 60min(750W work( Rate), by 2 h of water bath sonicator, 5 min are centrifuged, then it is that graphene is pre- that supernatant is taken, which to centrifuge 30 min to remove supernatant fraction, Treatment fluid filters the nmp solvent in removal graphene solution using cellulose membrane and graphene film is made, clear with deionized water It washes film three times, then graphene film is placed in deionized water, the obtained graphene aqueous solution of ultrasound, watersoluble plumbago obtained The mass fraction of alkene dispersion liquid is 0.3%.Calculating for graphene concentration in graphene aqueous solution is according to UV, visible light luminosity Instrument measures the absorbance of gained graphene solution, and by langbobier law, calculating acquires its graphene-containing concentration.
The conductive black is one in Cabot conductive black 2000, Degussa conductive black XE2-B, acetylene carbon black Kind or more than one, wherein Cabot conductive black 2000 is as being best performance of the watersoluble plumbago to electrically conductive ink(Cabot BP2000 has the characteristics that ultra-high conductivity, easily dispersion).Conductive black can adjust the concentration of watersoluble plumbago alkene electrically conductive ink, And electrically conductive ink is assigned with certain covering power.
The graphite powder be conductive filler, be nano graphite powder, highly conductive graphite powder, one kind in superfine graphite powder or More than one.Preferably, 3500 mesh nano graphite powders are selected, superfine graphite powder is 3000 mesh graphite powders, and highly conductive graphite powder is The graphite powder of carbon content 99%.The grain size of graphite powder is about 5-10 microns, and wherein nano-graphite is allocated as being watersoluble plumbago to conduction The conductive filler best performance of ink(Nano-graphite gradation diameter is small, it is easier to disperse, and form uniform conductive network).Nanometer Graphite powder forms conductive network in the dried film of electrically conductive ink.
The binder is aqueous thermal-curable acrylic resin, aqueous alkide resin, aqueous polyester resin, water-base epoxy One or more in resin, waterborne polyurethane resin.Aqueous thermosetting acrylic resin has that glossiness is good, hardness It gets well, the weatherability that strong adhesive force, flexibility are good, recoatability is good, excellent, chemical resistance, salt fog resistance.It is therefore preferable that water Binder of the property thermosetting acrylic resin as watersoluble plumbago alkene electrically conductive ink.
The aqueous alkyl-modified organic silicon defoamer of the antifoaming agent, organic silicone antifoaming agent, high-molecular-weight propylene acid esters One or more in homopolymer non-silicon defoaming agent, low molecular weight propylene acid ester homopolymer non-silicon defoaming agent.Preferably, water Antifoaming agent of the alkyl-modified organic silicon defoamer of property as watersoluble plumbago alkene electrically conductive ink.Aqueous alkyl-modified organic silicon defoamer Defoaming, foam-inhibiting effect can be played simultaneously, i.e., not only should destroy foam rapidly, and can be prevented within considerable time Foam generates.
The solvent is deionized water, the one or more in absolute ethyl alcohol, ammonium hydroxide.Solvent act as adjusting The pH value of watersoluble plumbago alkene electrically conductive ink, and dissolving resin.Preferably, in the present embodiment, ammonium hydroxide is chosen as solvent.Described Levelling agent is polyether-modified dimethyl silicone polymer aqueous levelling agent, the one or more in aqueous polyurethane levelling agent. Preferably, levelling agent uses polyether-modified dimethyl silicone polymer aqueous levelling agent in the present embodiment.Polyether-modified poly dimethyl Siloxane aqueous levelling agent can reduce the surface tension of water-based system and promote levelling and substrate wetting.
The PH conditioning agents are N- methylethanolamines, can neutralize thermosetting property water-based acrylic resin so that thermosetting property Water-based acrylic resin has water solubility after neutralizing, and the thermosetting property water after amine neutralizes can be dissolved directly using deionized water as solvent Property acrylic resin, and do not need to add in the cosolvents such as ethyl alcohol or isopropanol, avoid due to alcohols such as ethyl alcohol or isopropanols Rate of drying caused by the addition of cosolvent is too fast, so as to which network blocking version phenomenon occur in silk-screen printing.
The adhesion promoter is silane coupling agent class adhesion promoter, titanate coupling agent class adhesive force promotes One or more in agent, resinae adhesion promoter.Adhesion promoter is for directly construction in old coating surface Aqueous latex paint, alkyd emulsion.The addition of adhesion promoter can obviously improve to various organic and inorganic substrate attachment Power.Preferably, silane coupling agent class adhesion promoter best results.
The preparation method of watersoluble plumbago alkene electrically conductive ink is as follows:20-85 parts of graphene dispersing solution is added to dispersion machine Agitator tank in, and open stirring dispersion machine, rotating speed is set as 1000-2000r/min, obtains solution A;It is relayed to agitator tank The continuous solvent for adding in 5-10 parts, 20-45 parts of binder, persistently stir 10-15 minutes, obtain solution B;By solution B from point It dissipates and is taken out in machine agitator tank, is added in grinder, the parameter of grinder is set as 1000-2000r/min, and pressure is set as 3.0-5.0MPa grinds and 4-40 parts of conductive blacks is added in the backward solution B of 30 minutes, 5-38 parts of graphite powders, and 0.1-2.9 Part antifoaming agent, 0.05-0.5 part of levelling agent, 1.0-15 parts of adhesion promoter, be ground to the fineness of electrically conductive ink≤ 5 μm, obtain slurry C;Ammonium hydroxide is added in slurry C and deionized water adjusts rotary viscosity to 2000-3000MPa s, pH value is 7.5-9, solid content are 30% up to watersoluble plumbago alkene electrically conductive ink.
Below with the further details of explanation of some embodiments.
In some embodiments, 40 parts of the expanded graphite of 200 mesh is taken to be added in the nmp solvent of 1000 parts of organic solvent, 2 h of water bath sonicator under the power of 750W uses 5 min of centrifuge(5000 r/min), then supernatant is taken to centrifuge 30 min It is graphene pretreatment fluid to remove supernatant fraction, and the nmp solvent system in removal graphene solution is filtered using cellulose membrane Graphene film is obtained, graphene film is cleaned three times with deionized water, then graphene film is placed in deionized water, ultrasound Graphene aqueous solution is made.
It counts in parts by weight, the raw material composition such as the following table 2 of watersoluble plumbago alkene electrically conductive ink:
Component Mass fraction
Graphene dispersing solution 20—80
Conductive black 2000 5—30
Solvent 5—10
Graphite powder 5—35
Binder 20—40
Antifoaming agent 0.1—2.0
Levelling agent 0.05—0.2
N- methylethanolamines 1.0—10
Adhesion promoter 1.0—10
The preparation method of watersoluble plumbago alkene electrically conductive ink with it is upper identical.
In further embodiments, 40 parts of the expanded graphite of 200 mesh is taken to be added to the nmp solvent of 1000 parts of organic solvent In, water bath sonicator 3h under the power of 750W uses 10 min of centrifuge(5000 r/min), then supernatant is taken to centrifuge 30 It is graphene pretreatment fluid that min, which removes supernatant fraction, and the nmp solvent in removal graphene solution is filtered using cellulose membrane Graphene film is made, cleans graphene film three times with deionized water, then graphene film is placed in deionized water, surpasses Graphene aqueous solution is made in sound.
It counts in parts by weight, the raw material composition such as the following table 3 of watersoluble plumbago alkene electrically conductive ink:
Table 3
Component Mass fraction
Graphene dispersing solution 20—70
Conductive black 2000 4—25
Solvent 5—8
Graphite powder 6—32
Binder 25—38
Antifoaming agent 0.4—2.0
Levelling agent 0.1—0.2
N- methylethanolamines 2.0—10
Adhesion promoter 1.0—8.5
The preparation method of watersoluble plumbago alkene electrically conductive ink with it is upper identical.
In further embodiments, 50 parts of the expanded graphite of 200 mesh is taken to be added to the nmp solvent of 1000 parts of organic solvent In, water bath sonicator 3h under the power of 750W uses 10 min of centrifuge(5000 r/min), then supernatant is taken to centrifuge 30 It is graphene pretreatment fluid that min, which removes supernatant fraction, and the nmp solvent in removal graphene solution is filtered using cellulose membrane Graphene film is made, cleans graphene film three times with deionized water, then graphene film is placed in deionized water, surpasses Graphene aqueous solution is made in sound.
It counts in parts by weight, the raw material composition such as the following table 4 of watersoluble plumbago alkene electrically conductive ink:
Table 4
Component Mass fraction
Graphene dispersing solution 20—65
Conductive black 2000 4—20
Solvent 5—7
Graphite powder 6—25
Binder 30—35
Antifoaming agent 0.5—1.5
Levelling agent 0.1—0.15
N- methylethanolamines 2.0—9.5
Adhesion promoter 1.0—5.0
The preparation method of watersoluble plumbago alkene electrically conductive ink with it is upper identical.
In further embodiments, 50 parts of the expanded graphite of 200 mesh is taken to be added to the nmp solvent of 1000 parts of organic solvent In, water bath sonicator 3h under the power of 750W uses 10 min of centrifuge(5000 r/min), then supernatant is taken to centrifuge 30 It is graphene pretreatment fluid that min, which removes supernatant fraction, and the nmp solvent in removal graphene solution is filtered using cellulose membrane Graphene film is made, cleans graphene film three times with deionized water, then graphene film is placed in deionized water, surpasses Graphene aqueous solution is made in sound.
It counts in parts by weight, the raw material composition such as the following table 5 of watersoluble plumbago alkene electrically conductive ink:
Table 5
Component Mass fraction
Graphene dispersing solution 30—40
Conductive black 2000 5—15
Solvent 6
Graphite powder 10—15
Binder 30—32
Antifoaming agent 1.0
Levelling agent 0.12
N- methylethanolamines 3.0—8.0
Adhesion promoter 2.0—3.0
The preparation method of watersoluble plumbago alkene electrically conductive ink with it is upper identical.
Embodiment 1:It counts in parts by weight, the raw material composition such as the following table 6 of watersoluble plumbago alkene electrically conductive ink:
Component Mass fraction
Graphene dispersing solution 40
Conductive black 2000 8
Solvent 15
Graphite powder 12
Binder 20
Antifoaming agent 1.0
Levelling agent 0.1
N- methylethanolamines 1.3
Adhesion promoter 2.6
The preparation method of watersoluble plumbago alkene electrically conductive ink with it is upper identical.
Embodiment 2:It counts in parts by weight, the raw material composition such as the following table 7 of watersoluble plumbago alkene electrically conductive ink:
Component Mass fraction
Graphene dispersing solution 30
Conductive black 2000 8
Solvent 20
Graphite powder 12
Binder 25
Antifoaming agent 0.9
Levelling agent 0.1
N- methylethanolamines 2.0
Adhesion promoter 2.0
The preparation method of watersoluble plumbago alkene electrically conductive ink with it is upper identical.
Embodiment 3:It counts in parts by weight, the raw material composition such as the following table 8 of watersoluble plumbago alkene electrically conductive ink:
Component Mass fraction
Graphene dispersing solution 20
Conductive black 2000 8
Solvent 25
Graphite powder 12
Binder 30
Antifoaming agent 0.9
Levelling agent 0.1
N- methylethanolamines 2.0
Adhesion promoter 2.0
The preparation method of watersoluble plumbago alkene electrically conductive ink with it is upper identical.
The watersoluble plumbago alkene electrically conductive ink embodiment 1,2,3 of the present invention and comparative example watersoluble plumbago alkene electrically conductive ink are implemented Example 1,2,3 is respectively adopted 300 mesh screen printing plates and identical shape is printed under identical printing process conditions, and 120 The range of sheet resistance value variation range≤0.5% is dried under conditions of DEG C, compares watersoluble plumbago alkene electrically conductive ink and the comparison of the present invention The rate of drying of example watersoluble plumbago alkene electrically conductive ink, sheet resistance value.
Wherein comparative example 1,2,3 is to be added without Experimental comparison's group of PH conditioning agent N- methylethanolamines, and experiment proportioning is such as Under:
Comparative example 1
It counts in parts by weight, the raw material composition such as the following table 9 of watersoluble plumbago alkene electrically conductive ink:
Comparative example 2
It counts in parts by weight, the raw material composition such as the following table 10 of watersoluble plumbago alkene electrically conductive ink:
Comparative example 3
It counts in parts by weight, the raw material composition such as the following table 11 of watersoluble plumbago alkene electrically conductive ink:
The following table 12 is the watersoluble plumbago alkene electrically conductive ink performance parameter of embodiment and comparative example
In being compared by the rate of drying and sheet resistance value of 12 embodiment 1,2,3 of table and comparative example 1,2,3, it can be deduced that conclusion:
(1) rate of drying of watersoluble plumbago alkene electrically conductive ink of the invention is dry better than comparative example at 120 DEG C, and is not needed to Screen process press is adopted and is surface-treated;
(2) watersoluble plumbago alkene electrically conductive ink sheet resistance value of the invention is significantly less than the watersoluble plumbago alkene electrically conductive ink in comparative example. The rate of drying of watersoluble plumbago alkene electrically conductive ink is too fast, not only influences its silk-screen printing performance, and it is conductive more to influence watersoluble plumbago alkene The filming performance of ink, so that sheet resistance value becomes larger.
Finally it should be noted that:The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although The present invention is described in detail with reference to the foregoing embodiments, those of ordinary skill in the art are when understanding:It still can be with It modifies to the technical solution recorded in foregoing embodiments or equivalent replacement is carried out to which part technical characteristic;And These modifications are replaced, the spirit and model of various embodiments of the present invention technical solution that it does not separate the essence of the corresponding technical solution It encloses.

Claims (10)

1. a kind of watersoluble plumbago alkene electrically conductive ink, which is characterized in that including being prepared by the raw material of following parts by weight,
Graphene dispersing solution 20-85
2000 4-40 of conductive black
Solvent 5-15
Graphite powder 5-38
Binder 20-45
Antifoaming agent 0.1-2.9
Levelling agent 0.05-0.5
Adhesion promoter 1.0-15
PH conditioning agents 0.05-0.5
The binder is aqueous thermal-curable acrylic resin, aqueous alkide resin, aqueous polyester resin, water-base epoxy tree One or more in fat, waterborne polyurethane resin;The aqueous alkyl-modified organic silicon defoamer of the antifoaming agent has The agent of machine silicone antifoams, high-molecular-weight propylene acid ester homopolymer non-silicon defoaming agent, the defoaming of low molecular weight propylene acid ester homopolymer non-silicon One or more in agent;The levelling agent is polyether-modified dimethyl silicone polymer aqueous levelling agent, aqueous poly- ammonia One or more in ester levelling agent;The adhesion promoter is silane coupling agent class adhesion promoter, metatitanic acid One or more in ester coupling agent class adhesion promoter, resinae adhesion promoter;
The solvent is deionized water, the one or more in absolute ethyl alcohol, ammonium hydroxide;
The PH conditioning agents are one or more.
2. watersoluble plumbago alkene electrically conductive ink as described in claim 1, which is characterized in that including the raw material system by following parts by weight It is standby to form,
Graphene dispersing solution 20-80
2000 5-30 of conductive black
Solvent 5-10
Graphite powder 15-35
Binder 20-40
Antifoaming agent 0.1-2.0
Levelling agent 0.05-0.2
Adhesion promoter 1.0-10.
3. watersoluble plumbago alkene electrically conductive ink as claimed in claim 2, which is characterized in that including the raw material system by following parts by weight It is standby to form,
Graphene dispersing solution 20-70
2000 4-25 of conductive black
Solvent 5-8
Graphite powder 15-35
Binder 20-40
Antifoaming agent 0.1-2.0
Levelling agent 0.05-0.2
Adhesion promoter 1.0-10.
4. watersoluble plumbago alkene electrically conductive ink as described in claim 1, which is characterized in that the conductive black is that Cabot is led One or more in electric carbon black 2000, Degussa conductive black XE2-B, acetylene carbon black.
5. watersoluble plumbago alkene electrically conductive ink as described in claim 1, which is characterized in that the binder is aqueous heat curing type Acrylic resin.
6. watersoluble plumbago alkene electrically conductive ink as described in claim 1, which is characterized in that the antifoaming agent changes for aqueous alkyl Property organic silicon defoamer.
7. watersoluble plumbago alkene electrically conductive ink as described in claim 1, which is characterized in that the solvent is ammonium hydroxide.
8. watersoluble plumbago alkene electrically conductive ink as described in claim 1, which is characterized in that the PH conditioning agents are N- methyl second Hydramine.
9. watersoluble plumbago alkene electrically conductive ink as described in claim 1, which is characterized in that the levelling agent is polyether-modified poly- One or more in dimethyl siloxane aqueous levelling agent, aqueous polyurethane levelling agent.
10. a kind of preparation method of watersoluble plumbago alkene electrically conductive ink, which is characterized in that include the following steps:
20-85 parts of graphene dispersing solution is added in the agitator tank of dispersion machine, and opens stirring dispersion machine, rotating speed is set as 1000-2000r/min obtains solution A;5-10 parts of solvent, 20-45 parts of binder are continuously added into agitator tank, is held Continuous stirring 10-15 minutes, obtains solution B;Solution B from dispersion machine agitator tank is taken out, is added in grinder, grinder Parameter be set as 1000-2000r/min, pressure is set as 3.0-5.0MPa, is added in the backward solution B of grinding 30 minutes 4-40 parts of conductive blacks, 5-38 parts of graphite powders, 0.1-2.9 parts of antifoaming agent, 0.05-0.5 part of levelling agent, 1.0-15 The adhesion promoter of part, is ground to fineness≤5 μm of electrically conductive ink, obtains slurry C;In slurry C add in ammonium hydroxide and go from Sub- water adjusts rotary viscosity to 2000-3000MPa s, and pH value is 7.5-9 to get watersoluble plumbago alkene electrically conductive ink.
CN201711449353.XA 2017-12-27 2017-12-27 Watersoluble plumbago alkene electrically conductive ink and preparation method thereof Pending CN108129913A (en)

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CN109233444A (en) * 2018-11-26 2019-01-18 北京市光翌实业有限责任公司 Water-soluble conducting ink and preparation method thereof
CN109233597A (en) * 2018-08-23 2019-01-18 中国科学院福建物质结构研究所 A kind of high throughput prepare graphite it is dilute/method of Waterborne PU Composite
CN112029342A (en) * 2020-09-25 2020-12-04 欧菲微电子技术有限公司 Conductive ink, ultrasonic fingerprint module and electronic equipment
CN113436782A (en) * 2021-04-29 2021-09-24 哈工大机器人集团(无锡)科创基地研究院 Light high-conductivity aqueous conductive slurry and preparation method thereof
CN114974660A (en) * 2022-06-14 2022-08-30 湖北文理学院 Low-resistance wear-resistant conductive carbon paste and preparation method thereof

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CN106867316A (en) * 2017-03-17 2017-06-20 青岛瑞利特新材料科技有限公司 A kind of watersoluble plumbago alkene electrically conductive ink
CN107083114A (en) * 2017-03-20 2017-08-22 北京旭碳新材料科技有限公司 Watersoluble plumbago alkene electrically conductive ink

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CN105505161A (en) * 2015-09-30 2016-04-20 无锡同创石墨烯应用科技有限公司 Graphite-modified water-based conductive coating composition and preparation method thereof
CN106867316A (en) * 2017-03-17 2017-06-20 青岛瑞利特新材料科技有限公司 A kind of watersoluble plumbago alkene electrically conductive ink
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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN109233597A (en) * 2018-08-23 2019-01-18 中国科学院福建物质结构研究所 A kind of high throughput prepare graphite it is dilute/method of Waterborne PU Composite
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CN112029342A (en) * 2020-09-25 2020-12-04 欧菲微电子技术有限公司 Conductive ink, ultrasonic fingerprint module and electronic equipment
CN113436782A (en) * 2021-04-29 2021-09-24 哈工大机器人集团(无锡)科创基地研究院 Light high-conductivity aqueous conductive slurry and preparation method thereof
CN113436782B (en) * 2021-04-29 2023-01-24 哈工大机器人集团(无锡)科创基地研究院 Light high-conductivity aqueous conductive slurry and preparation method thereof
CN114974660A (en) * 2022-06-14 2022-08-30 湖北文理学院 Low-resistance wear-resistant conductive carbon paste and preparation method thereof

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Application publication date: 20180608