CN105062299A - Modified graphene conductive coating and preparation method thereof - Google Patents
Modified graphene conductive coating and preparation method thereof Download PDFInfo
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- CN105062299A CN105062299A CN201510414021.2A CN201510414021A CN105062299A CN 105062299 A CN105062299 A CN 105062299A CN 201510414021 A CN201510414021 A CN 201510414021A CN 105062299 A CN105062299 A CN 105062299A
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Abstract
The invention relates to a conductive coating, particularly to a modified graphene conductive coating and a preparation method thereof. The modified graphene conductive coating comprises components of raw materials in parts by mass as follows: 10%-25% of modified graphene powder, 30%-60% of matrix resin, 0.5%-1.0% of a leveling agent, 0.5%-1.0% of a defoaming agent, 0.5%-1.0% of a dispersing agent, 0.5%-1.0% of a film coalescing aid and 20%-40% of a diluent. The amino graphene is dispersed in ethyl alcohol, a noble metal ion solution is added, a sodium borohydride solution is added while stirring is performed, and the modified graphene powder is obtained through reaction, washing and vacuum drying; all the components are mixed and then dispersed for 1-4 h, and the modified graphene conductive coating is obtained after filtration. The conductive coating is doped with graphene loaded with noble metal nanoparticles, the electronic transmission efficiency is effectively improved, and meanwhile, the mechanical strength of the conductive coating is enhanced due to addition of the graphene.
Description
Technical field
The present invention relates to electrically conducting coating, especially relate to a kind of modified graphene electrically conducting coating and preparation method thereof.
Background technology
Electrically conducting coating is the special functional coating developed rapidly with modern science and technology, about has semicentennial developing history so far.1948, the U.S. discloses made the patent of conductive resin by silver and epoxy resin, this be the earliest disclosed in electrically conducting coating.China also begins one's study in the 1950's and applies electrically conducting coating.Electrically conducting coating is applied on the grounds such as non-conductive polymer material, make it a kind of new type functional coating that there is conduction current and get rid of accumulate static charge ability, specific conductivity after film is generally greater than 10S/m, be widely applied to every field at present, the conduction as integrated circuit component connect, connect nonweldable place, shielding high frequency magnetic field plastic stent, airplane hidden material, conductive film etc.In addition, electrically conducting coating also has very large use value in electronic market, as design and reparation, automobile demist heating wire broken line repairing, the repairing of keyboard printed wiring etc. of PCB.
Graphene is a kind of New Two Dimensional Carbon Materials, the physico-chemical property of its many excellence causes the extensive concern of countries in the world, and scientists finds that Graphene has boundless application prospect in fields such as micro-nano electron device, high sensitive sensor, functional composite material energy storage, catalysis.
(the high-performance water-based graphene conductive coating and preparation method thereof such as Fang Daining, Chinese patent CN103131232B) disclose a kind of natural graphite is oxidized in oxygenant after, the graphene aqueous solution utilizing two step chemical reduction methods to obtain organic molecule to modify, by the method that solution blended process adds polyester, neutralizing agent, flow agent, defoamer, linking agent, catalyst preparing obtain waterborne conductive Graphene coating.
Zhong Xiangyu etc. (layer/polyaniline conductive coating of a kind of Graphene modification and preparation method thereof, Chinese patent CN104592857A) disclose to adopt the polyaniline of high dissolution rate and add appropriate Graphene and prepare a kind of composite electrically-conducting paint.
Summary of the invention
Object of the present invention is intended to overcome prior art defect, provides a kind of modified graphene electrically conducting coating and preparation method thereof.
Described modified graphene electrically conducting coating, raw material in mass ratio consists of:
Described modified graphene powder is synthesized by amination Graphene, sodium borohydride, precious metal ion solution; Described amination Graphene can be buied by market, the amination Graphene of as above Hypon graceful bio tech ltd production; Described precious metal ion solution can be selected from least one in hydrochloro-auric acid, Platinic chloride, Silver Nitrate etc.
Described matrix resin can be selected from the one in epoxy resin, fluorocarbon resin, urethane resin, aminoresin, acrylic resin, Synolac, vibrin etc.
The optional one in organosilicon, acrylic acid or the like, only son's ethers etc. of described flow agent.
The optional one in organic silicon defoamer, inorganic silicon defoamer, antifoaming agent of non-silicone etc. of described defoamer, the one in the Efka2018 that BYK302, BYK065, BYK20, BYK011, BYK053 of producing as German Bi Ke company or EFKA company produce.
Described dispersion agent is optional from solvent-borne type dispersion agent or wetting dispersing agent, as BYK101, BYK161, BYK163 that German Bi Ke company produces, or the Efka5044 that EFKA company produces.
Described film coalescence aid can be selected from the one in butyl Bian alcohol acetic ester, butyl glycol ether carboxylic ester, ethylene glycol phenyl ether, dibasic acid dimethyl ester, propylene glycol propyl ether, binary acids diethyl esters class etc.
Described thinner can be selected from least one in BDDE, ethylene glycol diglycidylether, acetone, dimethylbenzene, propyl carbinol, methyl iso-butyl ketone (MIBK), dehydrated alcohol, vinyl acetic monomer, N-BUTYL ACETATE etc.
The preparation method of described modified graphene electrically conducting coating, comprises the steps:
1) prepare modified graphene powder, step is as follows:
By amination graphene dispersion in ethanol, add precious metal ion solution, and under agitation add sodium borohydride solution, reaction, washing, vacuum-drying, obtains modified graphene powder;
2) electrically conducting coating is prepared: by dispersion 1 ~ 4h after each component mixing, after filtration, namely obtain modified graphene electrically conducting coating.
In step 1) in, the proportioning of described amination Graphene, ethanol, precious metal ion solution, sodium borohydride solution can be (10 ~ 40) g: 1L: (10 ~ 50) mL: (10 ~ 50) mL; Described precious metal ion solution can adopt the one in the hydrochloro-auric acid ethanolic soln, the Silver Nitrate ethanolic soln of 50mmol/L, the Platinic chloride ethanolic soln of 50mmol/L etc. of volumetric molar concentration 50mmol/L; Described sodium borohydride solution can adopt the ethanol solution of sodium borohydride of volumetric molar concentration 0.5mol/L;
The time of described reaction can be 12h; The available washing with alcohol of described washing 3 ~ 5 times; The described vacuum drying time can be 24h.
First the present invention has prepared a kind of modified graphene covering supported noble metal nanoparticle, 10 ~ 25 parts of modified graphene powder, 30 ~ 60 parts of matrix resins, 0.50 ~ 1.0 part of flow agent, 0.50 ~ 1.0 part of defoamer, 0.50 ~ 1.0 part of dispersion agent, 0.50 ~ 1.0 part of film coalescence aid, 20 ~ 40 parts of mixing diluents are got by the component proportioning of electrically conducting coating, dispersed on dispersion machine, can electrically conducting coating be obtained after filtration.The present invention by being doped in electrically conducting coating by the Graphene covering supported noble metal nanoparticle, effectively improves electric transmission efficiency, simultaneously Graphene add the mechanical strength that improve electrically conducting coating.
The present invention adopts amination Graphene, the surface amination of Graphene is utilized to cover the noble metal nano particles carrying the high conductivity such as gold and silver, platinum, make electric transmission not only can, via the large pi-conjugated system of Sheet Graphite alkene, the electronic conduction passage of noble metal nano particles can also be utilized to improve electric transmission efficiency.And use amination Graphene, because the existence of surface amino groups can improve the dispersiveness of Graphene in acrylic resin, epoxy resin, and be stabilized in cover carry noble metal nano particles on graphene sheet layer also thereupon Graphene can in electrically conducting coating good dispersion, not easily move in electrically conducting coating use procedure.
The invention has the beneficial effects as follows: the present invention adopts amination Graphene, the surface amination of Graphene is utilized to cover the noble metal nano particles carrying the high conductivity such as gold and silver, platinum, make electric transmission not only can, via the large pi-conjugated system of Sheet Graphite alkene, the electronic conduction passage of noble metal nano particles can also be utilized to improve electron transfer rate.And use amination Graphene, because the existence of surface amino groups can improve the dispersiveness of Graphene in acrylic resin, epoxy resin, and be stabilized in cover carry noble metal nano particles on graphene sheet layer also thereupon Graphene can in electrically conducting coating good dispersion, not easily move in electrically conducting coating use procedure.Thus the electrically conducting coating prepared by the present invention can obtain high conductivity, simultaneously Graphene add the mechanical property that effectively can improve electrically conducting coating.
Accompanying drawing explanation
Fig. 1 to be the magnification of modified graphene electrically conducting coating prepared by embodiment 1 be SEM figure of 8000 times.In FIG, scale is 10 μm.
Embodiment
Following examples will the present invention is further illustrated by reference to the accompanying drawings.
Embodiment 1
(1) modified graphene powder is prepared
By 10g amination graphene dispersion in 1L ethanol, add 10ml chlorauric acid solution, and under agitation add 10ml sodium borohydride solution, reaction 12h, by washing with alcohol 3 times, vacuum-drying 24h, obtains modified graphene powder.
(2) modified graphene electrically conducting coating is prepared
Get 10 parts of modified graphene powder, 30 parts of epoxy resin, 0.5 part of organosilicon, 0.50 part of defoamer BYK302,0.50 part of dispersant B YK101,0.50 part of ethylene glycol phenyl ether, 20 part 1,4-butanediol diglycidyl ether mixes, dispersed 4h on dispersion machine, modified graphene electrically conducting coating can be obtained after filtration, its conductivity and mechanical experimental results as shown in table 1.
The magnification of modified graphene electrically conducting coating prepared by embodiment 1 is that the SEM figure of 8000 times is see Fig. 1.
Embodiment 2
(1) modified graphene powder is prepared
By 30g amination graphene dispersion in 1L ethanol, add 20ml silver nitrate solution, and be under agitation added dropwise to 30ml sodium borohydride solution, reaction 12h, by washing with alcohol 3 times, vacuum-drying 24h, obtains modified graphene powder.
(2) modified graphene electrically conducting coating is prepared
Get 15 parts of modified graphene powder, 40 parts of acrylic resins, 0.8 part of organosilicon, 0.60 part of defoamer BYK302,0.60 part of dispersant B YK101,0.80 part of ethylene glycol phenyl ether, 30 parts of vinyl acetic monomer mixing, dispersed 2h on dispersion machine, modified graphene electrically conducting coating can be obtained after filtration, its conductivity and mechanical experimental results as shown in table 1.
Embodiment 3
(1) modified graphene powder is prepared
By 40g amination graphene dispersion in 1L ethanol, add 50ml silver nitrate solution, and be under agitation added dropwise to 50ml sodium borohydride solution, reaction 12h, by washing with alcohol 3 times, vacuum-drying 24h, obtains modified graphene powder.
(2) modified graphene electrically conducting coating is prepared
Get 20 parts of modified graphene powder, 50 parts of acrylic resins, 0.8 part of organosilicon, 1.0 parts of defoamer BYK302,1.0 parts of dispersant B YK101,0.80 part of ethylene glycol phenyl ether, 30 parts of vinyl acetic monomer mixing, dispersed 3h on dispersion machine, modified graphene electrically conducting coating can be obtained after filtration, its conductivity and mechanical experimental results as shown in table 1.
Embodiment 4
(1) modified graphene powder is prepared with reference to embodiment 1.
(2) modified graphene electrically conducting coating is prepared
Get 25 parts of modified graphene powder, 60 parts of epoxy resin, 1.0 parts of organosilicons, 0.8 part of defoamer BYK302,0.80 part of dispersant B YK101,0.50 part of ethylene glycol phenyl ether, 40 part 1,4-butanediol diglycidyl ether mixes, dispersed 4h on dispersion machine, modified graphene electrically conducting coating can be obtained after filtration, its conductivity and mechanical experimental results as shown in table 1.
Table 1
| Embodiment | Specific conductivity (s/cm) | Sticking power (%) (square method) |
| 1 | 0.65±0.01 | 99 |
| 2 | 0.61±0.01 | 99 |
| 3 | 0.68±0.01 | 99 |
| 4 | 0.60±0.01 | 99 |
In embodiment 1 ~ 4, the conductivity of electrically conducting coating and mechanical experimental results table are see table 1.
Claims (10)
1. a modified graphene electrically conducting coating, is characterized in that its raw material in mass ratio consists of:
2. a kind of modified graphene electrically conducting coating as claimed in claim 1, is characterized in that described modified graphene powder is synthesized by amination Graphene, sodium borohydride, precious metal ion solution; Described precious metal ion solution can be selected from least one in hydrochloro-auric acid, Platinic chloride, Silver Nitrate.
3. a kind of modified graphene electrically conducting coating as claimed in claim 1, is characterized in that described matrix resin is selected from the one in epoxy resin, fluorocarbon resin, urethane resin, aminoresin, acrylic resin, Synolac, vibrin.
4. a kind of modified graphene electrically conducting coating as claimed in claim 1, is characterized in that described flow agent is selected from the one in organosilicon, acrylic acid or the like, only son's ethers.
5. a kind of modified graphene electrically conducting coating as claimed in claim 1, is characterized in that described defoamer is selected from the one in silicone based defoamer, inorganic silicon defoamer, antifoaming agent of non-silicone.
6. a kind of modified graphene electrically conducting coating as claimed in claim 1, is characterized in that described dispersion agent is selected from solvent-borne type dispersion agent or wetting dispersing agent.
7. a kind of modified graphene electrically conducting coating as claimed in claim 1, is characterized in that described film coalescence aid is selected from the one in butyl Bian alcohol acetic ester, butyl glycol ether carboxylic ester, ethylene glycol phenyl ether, dibasic acid dimethyl ester, propylene glycol propyl ether, binary acids diethyl esters class.
8. a kind of modified graphene electrically conducting coating as claimed in claim 1, it is characterized in that described thinner is selected from least one in BDDE, ethylene glycol diglycidylether, acetone, dimethylbenzene, propyl carbinol, methyl iso-butyl ketone (MIBK), dehydrated alcohol, vinyl acetic monomer, N-BUTYL ACETATE.
9., as the preparation method of a kind of modified graphene electrically conducting coating as described in arbitrary in claim 1 ~ 8, it is characterized in that comprising the steps:
1) prepare modified graphene powder, step is as follows:
By amination graphene dispersion in ethanol, add precious metal ion solution, and under agitation add sodium borohydride solution, reaction, washing, vacuum-drying, obtains modified graphene powder;
2) electrically conducting coating is prepared: by dispersion 1 ~ 4h after each component mixing, after filtration, namely obtain modified graphene electrically conducting coating.
10. the preparation method of a kind of modified graphene electrically conducting coating as claimed in claim 9, it is characterized in that in step 1), the proportioning of described amination Graphene, ethanol, precious metal ion solution, sodium borohydride solution is (10 ~ 40) g: 1L: (10 ~ 50) mL: (10 ~ 50) mL; Described precious metal ion solution can adopt the one in the Platinic chloride ethanolic soln of the Silver Nitrate ethanolic soln of the hydrochloro-auric acid ethanolic soln of volumetric molar concentration 50mmol/L, 50mmol/L, 50mmol/L; Described sodium borohydride solution can adopt the ethanol solution of sodium borohydride of volumetric molar concentration 0.5mol/L; The time of described reaction can be 12h; The available washing with alcohol of described washing 3 ~ 5 times; The described vacuum drying time can be 24h.
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