CN105111824B - A kind of alcohol radical nano silver wire ink containing conductive filler - Google Patents

A kind of alcohol radical nano silver wire ink containing conductive filler Download PDF

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Publication number
CN105111824B
CN105111824B CN201510646265.3A CN201510646265A CN105111824B CN 105111824 B CN105111824 B CN 105111824B CN 201510646265 A CN201510646265 A CN 201510646265A CN 105111824 B CN105111824 B CN 105111824B
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small molecule
zonyl
conductive filler
ink
silver wire
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CN105111824A (en
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李璐
陈善勇
刘碧桃
金容�
阮海波
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Chongqing University of Arts and Sciences
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Chongqing University of Arts and Sciences
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Abstract

The invention discloses a kind of alcohol radical nano silver wire ink containing conductive filler, consisting of:Nano silver wire, 0.2 1.5%;Chlorine vinegar binary copolymerization resin, 0.2 3%;Fluorocarbon surfactant, 0.005 0.05%;Small molecule dispersant, 0.1 2%;Small molecule levelling agent, 1 3%;Small molecule NMF, 2 5%;Small molecule defoamer, 1 2%;Conductive filler, 0.2 1.5%;Organic alcohols+ketones solvent, 81.95 95.295%.Ink coating effect is good, and simple thermal treatment can remove other most auxiliary agents in addition to silver wire and conductive filler after coating, and manufactured film conductivity is high with light transmittance, mist degree is low, can be widely used in the electronics fields such as touch-screen.

Description

A kind of alcohol radical nano silver wire ink containing conductive filler
Technical field
The invention belongs to conductive ink field, and in particular to a kind of alcohol radical nano silver wire ink containing conductive filler.
Background technology
Nano silver wire is the very promising material in current flexible conductive film field.And the utilization of this material then needs to borrow Silver-colored conductive ink is helped to realize.Silver-colored conductive ink includes nano silver wire and various auxiliary agents, and ink performance then depends on various help The selection of agent.For normal, auxiliary agent more at most silver wire electric conductivity is impacted bigger.Therefore, some patents such as CN103008679A Silver wire is directly dispersing in alcohols solvent and prepares conductive ink.But the shortage of this kind of ink auxiliary agent then causes ink to coat Performance is bad, and then causes film performance bad.Therefore, people with the addition of many different types of auxiliary agents to adjust in the ink Ink performance, such as patent CN104650653A, CN103627255A and CN104464880A.But these auxiliary agents of people's selection are big It is pluronic polymer mostly, and macromolecule is difficult to remove after ink coating, and then the electric conductivity and light transmittance of film can be reduced.Solution The basic method of certainly this problem is:It is removable auxiliary agent to find energy simple process.But unfortunately, this respect works at present It is also considerably less.
Meanwhile the neutral gear between silver wire network on the one hand can be due to that can reduce the conduction of film without conductive materials Property, it on the other hand can bring the scattering of light and film is had larger mist degree.These are all unfavorable for the use of film.To solve this Individual problem, conductive materials can be filled in neutral gear.Filled with two ways:One kind is applied again thereon after the coating of silver inks water is dried One layer of conductive materials are covered, another kind is directly filled among neutral gear when being and being directly added into conductive materials in the ink and coat.It is right It is more relatively easy than can be seen that second of technique.But unfortunately, it is this have conductive filler silver-colored conductive ink it is also considerably less, Performance is also very immature, such as patent CN102527621A.
To sum up, it is asking for electric conductivity that removable auxiliary agent and solution silver wire neutral gear are brought and mist degree to find simple process Topic is to develop the premise of high performance thin film, and the problem of conductive ink industry urgent need to resolve.
The content of the invention
It is an object of the invention to provide a kind of alcohol radical nano silver wire ink containing conductive filler, solves current alcohol radical ink Water due to lack various auxiliary agents and paintability is bad, the more difficult removing of auxiliary agent and silver wire neutral gear are brought after coating electric conductivity with The problems such as mist degree defect.The silver wire ink that the present invention develops has good behaviour and its various helping of using on various substrates Agent can be by being simply heat-treated removing, and its conductive fill material is filled with the neutral gear between silver wire and makes the electric conductivity of film Rise, mist degree reduce, thus the excellent performance of its conductive film, can be widely applied in electronic information field.The ink is specific Formula is as follows:
Nano silver wire, 0.2-1.5%;
Chlorine vinegar binary copolymerization resin, 0.2-3%;
Fluorocarbon surfactant, 0.005-0.05%;
Small molecule dispersant, 0.1-2%;
Small molecule levelling agent, 1-3%;
Small molecule NMF, 2-5%;
Small molecule defoamer, 1-2%;
Conductive filler, 0.2-1.5%;
Organic alcohols+ketones solvent, 81.95-95.295%.
A diameter of 30-50nm of nano silver wire used in the present invention, length is at 10-20 μm;
Binding agent used in the present invention is chlorine vinegar binary copolymerization resin.The binding agent decomposition temperature is 120 DEG C, can be simply at heat Reason can remove;
Surfactant used in the present invention be Zonyl@FSO, Zonyl@FSP, Zonyl@FSA, Zonyl@8867L, Zonyl@8857A, Zonyl@FSN, Zonyl@FS, Zonyl@FSK, Zonyl@FSD, Zonyl@TBS, Capstone@FS etc. are One or more of mixing in row fluorocarbon surfactant;
Small molecule dispersant used in the present invention is that the high boiling liquids such as monoethanolamine, 2-amino-2-methyl-1-propanol disperse Agent;
Small molecule levelling agent used in the present invention is butyl cellosolve, isopropoxide ethanol, propylene glycol monomethyl ether, different Fo Er One or more of mixing in the high boiling solvents such as ketone, DAA, DBE;
Small molecule NMF used in the present invention is the high boiling alcoholic solvents such as glycerine, cyclohexanol, ethylene glycol;
Small molecule defoamer used in the present invention is 2- hexyl ethanol;
Conductive filler used in the present invention is metal nano ion (such as gold, silver, copper nano-particle), PEDOT:PSS, graphite One or more of combinations in the materials such as alkene, CNT, metal oxide;
Alcohols solvent used in the present invention is one kind in methanol, ethanol and isopropanol;Ketones solvent used is acetone, fourth The ketones solvents such as ketone, cyclohexanone, isophorone;
The preparation steps of ink of the present invention are:Chlorine vinegar binary copolymerization resin is dissolved in be made into ketones solvent 10% it is molten Liquid.It is determined that formula composition, calculates the amount needed for every kind of material.Then will dechlorinate outside vinegar binary copolymerization resin solution and conductive filler Other compositions be well mixed, stir 20 minutes.Then, required conductive filler is added in the ink of stirring, stirring 10 Minute.Then, chlorine vinegar binary copolymerization resin solution is slowly instilled in ink.After continuing stirring 30 minutes, according to conductive filler Length determine the membrane filtration of different pore size, obtain final ink;
Ink of the present invention can increase by one layer of top coat protective layer in the above after application, increase conductive network while protection With the adhesion of substrate;
Ink of the present invention is after application, it is only necessary to which vacuum drying, which can remove, at 120 DEG C removes the few fluorocarbon surface work of content Remaining auxiliary agent outside property agent, and the neutral gear between silver wire is then filled up completely with by remaining conductive filler.So between silver wire It is conductively connected closer, the electric conductivity of significant increase film.Meanwhile filler reduce the light scattering of silver wire network etc. it is unfavorable because Element, make the mist degree of conductive film smaller;
The present invention has the following advantages:(1) contain the auxiliary agent of a variety of not same-actions in ink, ink performance can be allocated to each Physical parameter needed for kind substrate coating, therefore, the coating effect of ink of the invention on various substrates is fine, Thin film conductive Uniformly;(2) most of all, in the ink in addition to the few fluorocarbon surfactant of content, remaining auxiliary agent can be at low temperature Remove;The performance such as the Beneficial Effect brought with reference to conductive filler, the electric conductivity of its film, translucency, mist degree is preferable;(3) Silver wire content is few, raw material is cheap, preparation process is simple, thus ink is cheap.
Brief description of the drawings
Fig. 1:The silver wire network formed after ink coating of the present invention;
Specific embodiment
Embodiment:
The use of a diameter of 30-50nm, length in 10-20 μm of nano silver wire is conductive materials.From chlorine vinegar binary copolymerization Resin is binding agent, Zonyl@FSO-100 are surfactant, 2-amino-2-methyl-1-propanol is scattered anti-settling agent, the third two Alcohol methyl ether is levelling agent, cyclohexanol is NMF, 2- hexyl ethanol is defoamer, PEDOT:PSS is conducting filler, isopropanol Slurry is prepared with butanone is solvent;
[chlorine vinegar binary copolymerization resin is dissolved in be made into butanone 10% solution.It is determined that formula composition, calculates every kind of material Required amount.Then will dechlorination vinegar binary copolymerization resin solution and PEDOT:Other compositions outside PSS are well mixed, and stir 20 points Clock.Then, by required PEDOT:PSS is added in the ink of stirring, is stirred 10 minutes.Then, by chlorine vinegar binary copolymerization tree Lipoprotein solution is slowly instilled in ink.After continuing stirring 30 minutes, with the membrane filtration in 20 μm of apertures, final ink is obtained.
Presently preferred embodiments of the present invention described in detail above.It should be appreciated that the ordinary skill people of this area
Member makes many modifications and variations without creative work can according to the design of the present invention.All the art Middle technical staff under this invention's idea on the basis of existing technology can be with by logical analysis, reasoning, or a limited experiment Obtained experiment and technical scheme, all should be in the protection domain being defined in the patent claims.

Claims (1)

1. a kind of alcohol radical nano silver wire ink containing conductive filler, it is characterised in that its formula includes:
Nano silver wire, 0.2-1.5%;A diameter of 30-50nm of nano silver wire used, length is at 10-20 μm;
Chlorine vinegar binary copolymerization resin, 0.2-3%;
Fluorocarbon surfactant, 0.005-0.05%;Surfactant used be Zonyl@FSO, Zonyl@FSP, Zonyl@FSA, Zonyl@8867L、Zonyl@8857A、Zonyl@FSN、Zonyl@FS、Zonyl@FSK、Zonyl@FSD、Zonyl@ TBS、 One or more of mixing in Capstone@FS fluorocarbon surfactants;
Small molecule dispersant, 0.1-2%;Small molecule dispersant used is monoethanolamine, 2-amino-2-methyl-1-propanol higher boiling liquid Body dispersant;
Small molecule levelling agent, 1-3%;Small molecule levelling agent used be butyl cellosolve, isopropoxide ethanol, propylene glycol monomethyl ether, One or more of mixing in isophorone, DAA, DBE high boiling solvents;
Small molecule NMF, 2-5%;Small molecule NMF used is glycerine, cyclohexanol, ethylene glycol higher boiling alcohols solvent;
Small molecule defoamer, 1-2%;Small molecule defoamer used is 2- hexyl ethanol;
Conductive filler, 0.2-1.5%;Conductive filler used is gold, silver, the metal nanoparticle of copper nano-particle, PEDOT:PSS、 One or more of combinations in graphene, CNT, metal oxide;
Organic alcohols+ketones solvent, 81.95-95.295%;Alcohols solvent used is one kind in methanol, ethanol and isopropanol; Ketones solvent used is one kind in acetone, butanone, cyclohexanone, isophorone;
The preparation steps of above-mentioned ink are:Chlorine vinegar binary copolymerization resin is dissolved in be made into ketones solvent 10% solution, it is determined that matching somebody with somebody Fang Zucheng, calculate the amount needed for every kind of material, then by dechlorinate outside vinegar binary copolymerization resin solution and conductive filler other into Divide and be well mixed, stir 20 minutes, then, required conductive filler is added in the ink of stirring, stir 10 minutes, connect , chlorine vinegar binary copolymerization resin solution is slowly instilled in ink, it is true according to the length of conductive filler after continuing stirring 30 minutes Determine the membrane filtration of different pore size, obtain final ink.
CN201510646265.3A 2015-10-09 2015-10-09 A kind of alcohol radical nano silver wire ink containing conductive filler Active CN105111824B (en)

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CN106700961B (en) * 2017-01-13 2020-04-14 合肥微晶材料科技有限公司 Electromagnetic wave shielding film and highly transparent strong electromagnetic wave shielding adhesive tape based on same
CN108641484A (en) * 2018-04-12 2018-10-12 重庆市中光电显示技术有限公司 Electrically conductive ink for touch screen and preparation method thereof and conducting wire layout method

Citations (1)

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Publication number Priority date Publication date Assignee Title
CN104650653A (en) * 2013-11-22 2015-05-27 苏州冷石纳米材料科技有限公司 Nano-conductive silver paste and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104650653A (en) * 2013-11-22 2015-05-27 苏州冷石纳米材料科技有限公司 Nano-conductive silver paste and preparation method thereof

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Application publication date: 20151202

Assignee: Chongqing Rona Technology Co., Ltd.

Assignor: Chongqing University of Arts and Sciences

Contract record no.: 2019500000001

Denomination of invention: Alcohol-based silver nano-wire ink containing conductive filler

Granted publication date: 20171205

License type: Exclusive License

Record date: 20190122