CN104599737A - Micro-nano silver/conductive polymer composite, preparation method thereof and application - Google Patents
Micro-nano silver/conductive polymer composite, preparation method thereof and application Download PDFInfo
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Abstract
The invention belongs to the technical field of composites, and discloses a micro-nano silver/conductive polymer composite, a preparation method thereof and an application. The preparation method of the composite includes the steps: (1) preparing silver-ammonia solution, adding surface-active agents into the silver-ammonia solution, uniformly mixing the silver-ammonia solution and the surface-active agents to obtain emulsion, dripping reducing agent solution under the condition of stirring, performing reaction for 30-60min after dripping, washing the solution and separating deposits to obtain micro-nano silver powder; (2) weighing polyester or acrylic acid resin and dissolving the resin by solvents to obtain polymer solution, dispersing the micro-nano silver powder in the solvents to obtain silver dispersion liquid, adding the silver dispersion liquid into the polymer solution, uniformly mixing the silver dispersion liquid and the polymer solution, and dispersing the solution for 5-30min by a three-roller machine to obtain the micro-nano silver/conductive polymer composite. The composite has the advantage of fine conductivity and can be applied to the field of conductive electrodes, touch screen electrodes, thin-film conductive switches and the like.
Description
Technical field
The invention belongs to technical field of composite materials, be specifically related to a kind of micro-nano silver/conductive polymer composites and preparation method thereof and application.
Background technology
The silver small-size effect of micro Nano material, quantum size effect and surface-interface effect make it present the character such as unique optical, electrical, magnetic harmony.But because silver-colored micro Nano material has huge specific area, make it have very high activity, cause oxidizable and easy reunion etc., these greatly reduce its using value and range of application.And macromolecular material is organism paradigmatic structure, there is light quality, low price, be easy to machine-shaping and the plurality of advantages such as corrosion-resistant.In macromolecule matrix, add the micro-nano electric conducting material of suitable silver can form silver/conductive polymer nano-complex, the advantage of metallic conduction nano material and macromolecular compound can be combined like this, oxidation and the reunion of silver-colored micro-nano electric conducting material can not only be prevented, also make silver conductive nano material system have higher stability, and can be the processing forming that electrical-conductive nanometer material provides good.This compound can give full play to the specific performance of nano unit, and greatly can improve conduction and the heat conductivility of macromolecular material.Silver is micro-nano/and conductive polymer compound shows wide application prospect in fields such as electronics, optics, mechanics and biology, silver is micro-nano/and conductive silver paste prepared by conductive polymer nano-complex is by one of focus becoming composite material research field, open the application of Micron-nano composites in electric conducting material field, there is good prospects for commercial application.
Along with the high speed development of science and technology, various forms of touch-screen obtains and applies very widely in the electronic product that mobile phone, computer, pad, vehicle-mounted and digital camera etc. are different.And conductive silver paste slurry used on touch-screen is mainly through silk screen printing use as two electrodes on ITO (Indium Tin Oxide is called for short ITO) film and dielectric, connecting electrode produces electric field.Thus, conductive silver paste becomes the most critical material of touch screen technology application, and conductive silver paste prints on the touchscreen by screen printing forms, has very important impact for the touch screen performance parameter made of tin-doped indium oxide.
About silver conductive nano composite material, there is more report in prior art, as disclosed a kind of polyaniline/silver conductive nano composite material and preparation method thereof in patent document 201010199426.6, but it is complicated that this method Problems existing is preparation method, and need react under the condition of uv light irradiation.A kind of conducing composite material adding nano silver wire and preparation method thereof is disclosed in patent 200610050523.2, this method silver powder, nano silver wire and acrylic resin is carried out mixing dispersion obtain, but this method be micron-sized silver powder and nano silver wire are carried out with the use of, to reach good conductivity, and there is dispersed bad shortcoming in micron-sized silver powder.
Summary of the invention
In order to solve the shortcoming and defect part of prior art, primary and foremost purpose of the present invention is the preparation method providing a kind of micro-nano silver/conductive polymer composites.
Another object of the present invention is to provide a kind of micro-nano silver/conductive polymer composites prepared by said method.
Another object of the present invention is the application providing above-mentioned micro-nano silver/conductive polymer composites.
The object of the invention is achieved through the following technical solutions:
A preparation method for micro-nano silver/conductive polymer composites, comprises following operating procedure:
(1) prepare silver ammino solution, add surfactant and mix and obtain emulsion, then drip reductant solution under agitation, dropwise rear reaction 30 ~ 60min toward silver ammino solution in, wash, sediment separate out, obtains micro-nano silver powder;
(2) take polyester or acrylic resin, obtain polymer solution by dissolution with solvents; Micro-nano silver powder is scattered in solvent and obtains silver-colored dispersion liquid, then silver-colored dispersion liquid is joined in polymer solution and be uniformly mixed, with three-roller dispersion 5 ~ 30min, obtain micro-nano silver/conductive polymer composites.
Described in step (1), the preparation method of silver ammino solution is: be dissolved in deionized water by silver acetate or silver nitrate, be heated to 50 ~ 80 DEG C, drip ammoniacal liquor, stop dripping when the dissolving completely just of produced precipitation, solution clarification, obtain silver ammino solution; The mass ratio of described silver acetate or silver nitrate and deionized water is preferably 1:100; The addition of described surfactant is 1% ~ 5% of silver acetate or silver nitrate quality; Described surfactant preferably sodium dodecyl sulfate or dodecyl sodium sulfate.
Described reductant solution refers to the solution of one or more materials in potassium borohydride, sodium borohydride and ascorbic acid; The mixed solution of preferred potassium borohydride or sodium borohydride and ascorbic acid; More preferably the ratio of amount of substance is the potassium borohydride of 1:1 or the mixed solution of sodium borohydride and ascorbic acid.
In described reductant solution, in reducing agent and silver ammino solution, the mol ratio of silver ion is preferably 1:(0.5 ~ 2).
Described in step (2), polyester preferred molecular weight is the thermoplastic polyester of 10000 ~ 50000; Described acrylic resin preferred molecular weight is the thermoplastic acrylic resin of 100000 ~ 500000.
One or more solvent in described solvent preferred different fluorine you ketone, mixed dibasic acid ester (DBE) and butyl.
In described polymer solution, the mass ratio of polyester or acrylic resin and solvent is preferably 1:(2 ~ 5); In silver dispersion liquid, the mass ratio of micro-nano silver powder and solvent is preferably 1:10.
In micro-nano silver powder in described silver-colored dispersion liquid and polymer solution, the mass ratio of polyester or acrylic resin is preferably 1:(2 ~ 5).
A kind of micro-nano silver/conductive polymer composites, is prepared by above method.
Above-mentioned micro-nano silver/conductive polymer composites at conductive electrode, touch screen electrode, the application in the fields such as Thin film conductive switch.
Preparation principle of the present invention is: Ag+ is reduced agent and is reduced to micro Nano material, is dispersed in macromolecule resin, obtains micro-nano silver/conductive polymer composites by physical blending process (three-roller dispersion).
Had the following advantages and beneficial effect by preparation method of the present invention and the product tool that obtains:
(1) the present invention adopts one kettle way can prepare the micro-nano silver powder of particle size range at 100 ~ 1000nm, and preparation method is simple, and micro-nano silver powder footpath controllability is good;
(2) composite material that the present invention obtains has excellent electric conductivity, and its sheet resistance value is 5.0m Ω/ /mil ~ 50m Ω/ /mil, and resistivity is 0.5m Ω cm ~ 5m Ω cm;
(3) composite material that obtains of the present invention is with polyester or acrylic resin for material matrix, and with your ketone, mixed dibasic acid ester (DBE) or butyl of different fluorine for solvent, these solvents are good to the dissolubility of resin, have slow volatility;
(4) micro-nano silver/conductive polymer composites of the present invention adopts three-roller to disperse in preparation process, and micro-nano silver powder can be allowed to be dispersed in uniformly in macromolecule resin, can not damage micro-nano silver powder or resin;
(5) micro-nano silver of the present invention/conductive polymer composites uses polyester or acrylic resin to be base material, can be used for low-temperature conductive electrode.
Accompanying drawing explanation
The scanning electron microscope diagram (SEM) of the micro-nano silver powder that Fig. 1 ~ 3 obtain for embodiment 1.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) silver nitrate is dissolved in the deionized water of 100 times of quality, be heated to 60 DEG C, drip ammoniacal liquor, when produced precipitation is dissolved just completely, stop dripping during solution clarification, obtain silver ammino solution, the Surfactant SDS adding silver nitrate quality 3% in silver ammino solution mixes and obtains emulsion, then reductant solution is dripped under agitation, reductant solution is that 1:1 be mixed to get with the aqueous ascorbic acid of 0.3mol/L by potassium borohydride and the ratio of the amount of substance of ascorbic acid by the potassium borohydride aqueous solution of 0.08mol/L, in reductant solution, the amount of substance of reducing agent is 1:1 with the ratio of the amount of substance of silver ion in silver ammino solution, after reductant solution dropwises, continue stirring reaction 60min, washing sediment separate out, obtain micro-nano silver powder,
(2) take the thermoplastic polyester that molecular weight is 12000, add the solvent different fluorine that ketone of 3 times of quality, be heated to 60 DEG C, stirring 5h makes it dissolve completely and obtains polymer solution; Micro-nano silver powder is scattered in your ketone of the different fluorine of solvent of 10 times of quality and obtains silver-colored dispersion liquid, then silver-colored dispersion liquid is joined in polymer solution and be uniformly mixed, in micro-nano silver powder in silver dispersion liquid and polymer solution, the mass ratio of polyester is 1:3, disperse 15min with three-roller, obtain micro-nano silver/conductive polymer composites.
The micro-nano silver powder scanning electron microscopy that the present embodiment obtains is observed, as shown in Figures 1 to 3, as can be seen from Figure, the micro-nano silver that the present invention obtains has different patterns to result, have spherical, sheet, graininess, its particle size range is 100 ~ 1000nm;
Micro-nano silver/conductive polymer composites that the present embodiment obtains with 400 object half tone silk screen printings on base material, 45min is dried at 150 DEG C, by the conductivity of the good composite material of four point probe resistance instrument testing of printed, its sheet resistance value is 5.0m Ω/ /mil, and resistivity is 0.5m Ω cm.
Embodiment 2
(1) silver nitrate is dissolved in the deionized water of 100 times of quality, be heated to 50 DEG C, drip ammoniacal liquor, when produced precipitation is dissolved just completely, stop dripping during solution clarification, obtain silver ammino solution, the Surfactant SDS adding silver nitrate quality 5% in silver ammino solution mixes and obtains emulsion, then reductant solution is dripped under agitation, reductant solution is that 1:1 be mixed to get with the aqueous ascorbic acid of 0.1mol/L by potassium borohydride and the ratio of the amount of substance of ascorbic acid by the potassium borohydride aqueous solution of 0.05mol/L, in reductant solution, the amount of substance of reducing agent is 1:2 with the ratio of the amount of substance of silver ion in silver ammino solution, after reductant solution dropwises, continue stirring reaction 30min, washing sediment separate out, obtain micro-nano silver powder,
(2) take the thermoplastic polyester that molecular weight is 50000, add the solvent different fluorine that ketone of 2 times of quality, be heated to 40 DEG C, stirring 8h makes it dissolve completely and obtains polymer solution; Micro-nano silver powder is scattered in your ketone of the different fluorine of solvent of 10 times of quality and obtains silver-colored dispersion liquid, then silver-colored dispersion liquid is joined in polymer solution and be uniformly mixed, in micro-nano silver powder in silver dispersion liquid and polymer solution, the mass ratio of polyester is 1:2, disperse 5min with three-roller, obtain micro-nano silver/conductive polymer composites.
Micro-nano silver/conductive polymer composites that the present embodiment obtains with 500 object half tone silk screen printings on base material, 60min is dried at 120 DEG C, by the conductivity of the good composite material of four point probe resistance instrument testing of printed, its sheet resistance value is 50m Ω/ /mil, and resistivity is 5m Ω cm.
Embodiment 3
(1) silver nitrate is dissolved in the deionized water of 100 times of quality, be heated to 80 DEG C, drip ammoniacal liquor, when produced precipitation is dissolved just completely, stop dripping during solution clarification, obtain silver ammino solution, the surfactant sodium dodecyl base sodium sulfonate adding silver nitrate quality 1% in silver ammino solution mixes and obtains emulsion, then reductant solution is dripped under agitation, reductant solution is that 1:1 be mixed to get with the aqueous ascorbic acid of 0.5mol/L by potassium borohydride and the ratio of the amount of substance of ascorbic acid by the potassium borohydride aqueous solution of 0.1mol/L, in reductant solution, the amount of substance of reducing agent is 1:0.5 with the ratio of the amount of substance of silver ion in silver ammino solution, after reductant solution dropwises, continue stirring reaction 40min, washing sediment separate out, obtain micro-nano silver powder,
(2) take the thermoplastic acrylic resin that molecular weight is 500000, add the solvent dibasic acid ester (DBE) of 5 times of quality, add thermal agitation and make it dissolve completely to obtain polymer solution; Micro-nano silver powder is scattered in the solvent dibasic acid ester of 10 times of quality and obtains silver-colored dispersion liquid, then silver-colored dispersion liquid is joined in polymer solution and be uniformly mixed, in micro-nano silver powder in silver dispersion liquid and polymer solution, the mass ratio of acrylic resin is 1:5, disperse 30min with three-roller, obtain micro-nano silver/conductive polymer composites.
Micro-nano silver/conductive polymer composites that the present embodiment obtains with 300 object half tone silk screen printings on base material, 30min is dried at 160 DEG C, by the conductivity of the good composite material of four point probe resistance instrument testing of printed, its sheet resistance value is 28m Ω/ /mil, and resistivity is 2.8m Ω cm.
Embodiment 4
(1) silver acetate is dissolved in the deionized water of 100 times of quality, be heated to 60 DEG C, drip ammoniacal liquor, when produced precipitation is dissolved just completely, stop dripping during solution clarification, obtain silver ammino solution, the surfactant sodium dodecyl base sodium sulfonate adding silver acetate quality 1% in silver ammino solution mixes and obtains emulsion, then reductant solution is dripped under agitation, reductant solution is that 1:1 be mixed to get with the aqueous ascorbic acid of 0.2mol/L by potassium borohydride and the ratio of the amount of substance of ascorbic acid by the sodium borohydride aqueous solution of 0.06mol/L, in reductant solution, the amount of substance of reducing agent is 1:1 with the ratio of the amount of substance of silver ion in silver ammino solution, after reductant solution dropwises, continue stirring reaction 40min, washing sediment separate out, obtain micro-nano silver powder,
(2) take the thermoplastic acrylic resin that molecular weight is 100000, add the solvent dibasic acid ester (DBE) of 4 times of quality and the mixture of butyl, add thermal agitation and make it dissolve completely to obtain polymer solution; Micro-nano silver powder is scattered in the solvent dibasic acid ester of 10 times of quality and the mixture of butyl and obtains silver-colored dispersion liquid, then silver-colored dispersion liquid is joined in polymer solution and be uniformly mixed, in micro-nano silver powder in silver dispersion liquid and polymer solution, the mass ratio of acrylic resin is 1:4, disperse 30min with three-roller, obtain micro-nano silver/conductive polymer composites.
Micro-nano silver/conductive polymer composites that the present embodiment obtains with 400 object half tone silk screen printings on base material, 60min is dried at 150 DEG C, by the conductivity of the good composite material of four point probe resistance instrument testing of printed, its sheet resistance value is 20m Ω/ /mil, and resistivity is 2.m Ω cm.
Above-described embodiment is the present invention's preferably execution mode; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. a preparation method for micro-nano silver/conductive polymer composites, is characterized in that comprising following operating procedure:
(1) prepare silver ammino solution, add surfactant and mix and obtain emulsion, then drip reductant solution under agitation, dropwise rear reaction 30 ~ 60min toward silver ammino solution in, wash, sediment separate out, obtains micro-nano silver powder;
(2) take polyester or acrylic resin, obtain polymer solution by dissolution with solvents; Micro-nano silver powder is scattered in solvent and obtains silver-colored dispersion liquid, then silver-colored dispersion liquid is joined in polymer solution and be uniformly mixed, with three-roller dispersion 5 ~ 30min, obtain micro-nano silver/conductive polymer composites.
2. the preparation method of a kind of micro-nano silver/conductive polymer composites according to claim 1, it is characterized in that: described in step (1), the preparation method of silver ammino solution is: be dissolved in deionized water by silver acetate or silver nitrate, be heated to 50 ~ 80 DEG C, drip ammoniacal liquor, stop dripping when the dissolving completely just of produced precipitation, solution clarification, obtain silver ammino solution.
3. the preparation method of a kind of micro-nano silver/conductive polymer composites according to claim 2, is characterized in that: the mass ratio of described silver acetate or silver nitrate and deionized water is 1:100; The addition of described surfactant is 1% ~ 5% of silver acetate or silver nitrate quality.
4. the preparation method of a kind of micro-nano silver/conductive polymer composites according to claim 1, is characterized in that: described surfactant refers to lauryl sodium sulfate or dodecyl sodium sulfate; Described reductant solution refers to the mixed solution of potassium borohydride or sodium borohydride and ascorbic acid.
5. the preparation method of a kind of micro-nano silver/conductive polymer composites according to claim 4, is characterized in that: described reductant solution refers to that the ratio of amount of substance is the potassium borohydride of 1:1 or the mixed solution of sodium borohydride and ascorbic acid.
6. the preparation method of a kind of micro-nano silver/conductive polymer composites according to claim 1, is characterized in that: in described reductant solution, in reducing agent and silver ammino solution, the mol ratio of silver ion is 1:(0.5 ~ 2).
7. the preparation method of a kind of micro-nano silver/conductive polymer composites according to claim 1, is characterized in that: described polyester refers to that molecular weight is the thermoplastic polyester of 10000 ~ 50000; Described acrylic resin refers to that molecular weight is the thermoplastic acrylic resin of 100000 ~ 500000; Described solvent refers to one or more the solvent in different fluorine you ketone, mixed dibasic acid ester and butyl.
8. the preparation method of a kind of micro-nano silver/conductive polymer composites according to claim 1, is characterized in that: in described polymer solution, the mass ratio of polyester or acrylic resin and solvent is 1:(2 ~ 5); In silver dispersion liquid, the mass ratio of micro-nano silver powder and solvent is 1:10; In micro-nano silver powder in silver dispersion liquid and polymer solution, the mass ratio of polyester or acrylic resin is 1:(2 ~ 5).
9. micro-nano silver/conductive polymer composites, is characterized in that: prepared by the method described in any one of claim 1 ~ 8.
10. a kind of micro-nano silver/conductive polymer composites according to claim 9 is at conductive electrode, touch screen electrode, the application in Thin film conductive field of switches.
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| CN112980126A (en) * | 2021-02-22 | 2021-06-18 | 青岛科技大学 | Self-repairing stretchable electrode and preparation method and application thereof |
| CN114713836A (en) * | 2022-03-02 | 2022-07-08 | 上海电力大学 | Synthetic method of Cu-Ag sheet-shaped nano composite material |
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