CN114702887A - Graphene silver nanowire composite slurry and preparation method thereof - Google Patents
Graphene silver nanowire composite slurry and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 122
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 80
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 78
- 239000002002 slurry Substances 0.000 title claims abstract description 43
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims description 15
- 238000007613 slurry method Methods 0.000 title description 2
- 239000002270 dispersing agent Substances 0.000 claims abstract description 29
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000006185 dispersion Substances 0.000 claims abstract description 25
- 239000002904 solvent Substances 0.000 claims abstract description 22
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 18
- 239000008103 glucose Substances 0.000 claims abstract description 18
- 229920000178 Acrylic resin Polymers 0.000 claims abstract description 15
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 15
- 239000003822 epoxy resin Substances 0.000 claims abstract description 15
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 15
- 229920005749 polyurethane resin Polymers 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 20
- 229920000570 polyether Polymers 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 16
- 238000009736 wetting Methods 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 238000001291 vacuum drying Methods 0.000 claims description 12
- 229920000058 polyacrylate Polymers 0.000 claims description 11
- 229920005646 polycarboxylate Polymers 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 8
- 239000002480 mineral oil Substances 0.000 claims description 8
- 235000010446 mineral oil Nutrition 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- -1 polydimethylsiloxane Polymers 0.000 claims description 8
- 239000012286 potassium permanganate Substances 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 8
- 239000000080 wetting agent Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000002518 antifoaming agent Substances 0.000 claims description 5
- 239000006179 pH buffering agent Substances 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 4
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 229960002887 deanol Drugs 0.000 claims description 4
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 4
- 239000012972 dimethylethanolamine Substances 0.000 claims description 4
- 239000000839 emulsion Substances 0.000 claims description 4
- 125000003916 ethylene diamine group Chemical group 0.000 claims description 4
- 238000000875 high-speed ball milling Methods 0.000 claims description 4
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 4
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 4
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 4
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 4
- 239000003273 ketjen black Substances 0.000 claims description 4
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 4
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 4
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 4
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 4
- 239000004317 sodium nitrate Substances 0.000 claims description 4
- 235000010344 sodium nitrate Nutrition 0.000 claims description 4
- HEBRGEBJCIKEKX-UHFFFAOYSA-M sodium;2-hexadecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HEBRGEBJCIKEKX-UHFFFAOYSA-M 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims 3
- 239000010703 silicon Substances 0.000 claims 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 229920000142 Sodium polycarboxylate Polymers 0.000 claims 1
- 238000000227 grinding Methods 0.000 claims 1
- 230000002209 hydrophobic effect Effects 0.000 claims 1
- 150000003109 potassium Chemical class 0.000 claims 1
- 229920005614 potassium polyacrylate Polymers 0.000 claims 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 abstract description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 3
- 125000003700 epoxy group Chemical group 0.000 abstract description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 239000011229 interlayer Substances 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 229920001296 polysiloxane Polymers 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 7
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 6
- 239000000047 product Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 150000003863 ammonium salts Chemical class 0.000 description 3
- 239000013530 defoamer Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000006174 pH buffer Substances 0.000 description 3
- 159000000000 sodium salts Chemical class 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/20—Diluents or solvents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses graphene silver nanowire composite slurry, and particularly relates to the technical field of graphene slurry, wherein the graphene silver nanowire composite slurry comprises the following raw materials: modified graphene, silver nanowires, conductive carbon black, a solvent, a waterborne polyurethane resin, a waterborne epoxy resin, a waterborne acrylic resin, glucose, a dispersant and an auxiliary agent. According to the invention, modified graphene and silver nanowires are used as raw materials, graphene is subjected to oxidation treatment to increase the interlayer spacing of graphene oxide, oxygen-containing groups are increased, the surface of graphene contains a large number of hydroxyl groups and epoxy groups, and the edge of graphene contains more carboxyl groups and carbonyl groups, so that the graphene has a better dispersion effect, the silver nanowires can be better adsorbed on the oxidized graphene, and the graphene and the silver nanowires are mixed and then reduced by glucose, so that the graphene and the silver nanowires are better dispersed and combined.
Description
Technical Field
The invention relates to the technical field of graphene slurry, in particular to graphene silver nanowire composite slurry and a preparation method thereof.
Background
The traditional conductive paste is basically prepared by adding conductive unit powder into a polymer in the form of filler, wherein the conductive unit powder mainly comprises three types of carbon, metal and compound. In order to improve the performance, the improvement of the conductive filler and the exploration and application of new materials are the development trends of the research of the conductive paste at home and abroad at present. The conductive carbon paste is prepared by mixing a carbon material and a polymer resin, has good conductivity, and is widely applied to communication products (mobile phones), computers, portable electronic products, consumer electronics, network hardware (servers and the like), medical instruments, household electronic products, aerospace, national defense and other electronic equipment. The conductive carbon paste is heated and cured to form a coating layer which has stable performance, is not easy to oxidize, resist acid, alkali and solvent corrosion and can play a role in protection and conduction. The metal conductive paste, such as gold, silver and copper paste ink, has excellent conductivity and resistivity of 10 < -2 > -10 < -3 > omega cm. The gold and silver powder ink has good performance, but the price is expensive, and the silver has the defects of easy migration, vulcanization, poor resistance to solder corrosion, easy cracking in the sintering process and the like. Under the action of air and water, the copper paste ink can generate an oxidation layer to make the conductivity unstable.
Conductive silver paste generally consists of silver powder, glass frit and organic components. The dispersion uniformity of the silver powder in the conductive silver paste has great influence on the conductivity of the conductive silver paste. The conductive silver paste has problems in conductivity: firstly, silver powder is easy to agglomerate, and secondly, a non-conductive substance glass powder exists. These often result in poor conductivity of the conductive silver paste. Although the existing conductive carbon paste has high cost performance compared with the conductive silver paste, the resistance performance of the existing conductive carbon paste is lower than that of the conductive silver paste, so that the existing conductive carbon paste has limited effect in application and is limited in application in products requiring high conductive performance. In order to obtain the slurry with excellent comprehensive performance, the graphene and the silver nanowire medium are mixed to prepare the slurry, so that the slurry has the composite performance of electric conductivity, far infrared heating and safe sterilization, and is a better technical route. However, how to well disperse graphene and silver nanowires into a slurry system and combine the graphene and silver nanowires becomes a difficult problem to be solved urgently.
Disclosure of Invention
In order to overcome the above defects in the prior art, embodiments of the present invention provide a graphene-silver nanowire composite slurry and a preparation method thereof, and the problems to be solved by the present invention are: how to improve the dispersion performance of the graphene and the silver nanowire and enable the graphene to be better combined with the silver nanowire.
In order to achieve the purpose, the invention provides the following technical scheme: the graphene silver nanowire composite slurry comprises the following raw materials in parts by weight: 30-50 parts of modified graphene, 8-16 parts of silver nanowires, 6-10 parts of conductive carbon black, 40-60 parts of solvent, 30-50 parts of waterborne polyurethane resin, 10-30 parts of waterborne epoxy resin, 5-15 parts of waterborne acrylic resin, 5-10 parts of glucose, 0.5-5 parts of dispersant and 0.5-5 parts of auxiliary agent.
In a preferred embodiment, the feed comprises the following raw materials in parts by weight: 35-45 parts of modified graphene, 11-13 parts of silver nanowires, 7-9 parts of conductive carbon black, 45-55 parts of solvent, 35-45 parts of waterborne polyurethane resin, 15-25 parts of waterborne epoxy resin, 8-12 parts of waterborne acrylic resin, 6-8 parts of glucose, 2-3 parts of dispersant and 2-3 parts of assistant.
In a preferred embodiment, the feed comprises the following raw materials in parts by weight: 40 parts of modified graphene, 12 parts of silver nanowires, 8 parts of conductive carbon black, 50 parts of solvent, 40 parts of waterborne polyurethane resin, 20 parts of waterborne epoxy resin, 10 parts of waterborne acrylic resin, 7 parts of glucose, 2.5 parts of dispersant and 2.5 parts of assistant.
In a preferred embodiment, the diameter of the silver nanowires is 80-250nm, the conductive carbon black is one of ketjen black EC-600JD and conductive carbon black BP-2000, the particle size of the conductive carbon black is 0.1-10um, and the auxiliary agents comprise a curing agent, a pH buffer, an antifoaming agent, a wetting and leveling agent and a wetting and dispersing agent.
In a preferred embodiment, the dispersant is one or more of sodium dodecyl sulfate, sodium hexadecylbenzene sulfonate, hydroxypropyl methylcellulose and sodium carboxymethylcellulose, the curing agent is ethylenediamine, the pH buffering agent is one or more of ethanolamine, diethanolamine, triethanolamine, dimethylethanolamine and methyldiethanolamine, the defoamer is one or more of polyether, mineral oil emulsion, polyether modified mineral oil or polyether modified silicone, the wetting and leveling agent is one or more of polyether modified polydimethylsiloxane, polyether modified silicone, fluorocarbon modified silicone and fluorocarbon modified polyacrylate water solution, the wetting and dispersing agent is one or more of polyacrylate sodium salt, polyacrylate potassium salt, polycarboxylate sodium salt, polycarboxylate ammonium salt, hydrophobically modified polycarboxylate potassium salt, phosphate ester complex and self-emulsifying modified polyacrylate, the solvent is absolute ethyl alcohol or ammonia water.
The invention also provides a preparation method of the graphene silver nanowire composite slurry, which comprises the following specific preparation steps:
the method comprises the following steps: preparing modified graphene, weighing a certain amount of graphene, putting the graphene into a ball mill, crushing to obtain graphene powder, adding sodium nitrate and concentrated sulfuric acid into the graphene powder, mixing and stirring uniformly, slowly adding potassium permanganate during stirring, continuing stirring for 2-4 hours after adding the potassium permanganate, keeping the temperature at 35-45 ℃ by using a water bath heating temperature after stirring, adding deionized water after keeping the temperature, then raising the temperature of the water bath to 90-100 ℃ for keeping the temperature, adding 5% of hydrogen peroxide solution after keeping the temperature, washing the mixture until the pH value is neutral by using hydrochloric acid and deionized water after reaction, and then carrying out vacuum drying to obtain modified graphene;
step two: adding deionized water into the modified graphene obtained in the step one, performing ultrasonic dispersion for 1-2 hours to obtain a modified graphene dispersion solution, then adding silver nanowires into the graphene dispersion solution, performing ultrasonic-assisted stirring, washing for 3-5 times by using the deionized water, adding glucose after washing, performing reflux stirring for 8-12 hours at 90-100 ℃, filtering, washing and drying the obtained precipitate by using the deionized water and ethanol to obtain a mixture of the modified graphene and the silver nanowires;
step three: putting the weighed conductive carbon black, solvent, dispersant, waterborne polyurethane resin, waterborne epoxy resin and waterborne acrylic resin into a reaction kettle, stirring and mixing for 1-2h, then ultrasonically dispersing for 3-8h, performing high-speed ball milling dispersion by using a ball mill after the ultrasonic dispersion is finished, and filtering to obtain premixed slurry after the ball milling dispersion is finished;
step four: and (3) adding the mixture obtained in the step two into the premixed slurry obtained in the step three, adding an auxiliary agent for defoaming, dispersing, adjusting the pH value, curing, and continuously and uniformly stirring to obtain the graphene-silver nanowire composite slurry.
In a preferred embodiment, the particle size of the graphene powder obtained after the ball mill is crushed in the first step is 2-30um, the mixing and stirring speed in the first step is 800-1200 rpm, the primary heat preservation time in the first step is 2-3h, the secondary heat preservation time is 1-2h, and the vacuum drying temperature is 50-70 ℃ and the vacuum drying time is 10-14 h.
In a preferred embodiment, the power of the ultrasonic equipment during the ultrasonic dispersion in the second step is 3000-.
In a preferred embodiment, the power of the ultrasonic equipment in the ultrasonic dispersion in the third step is 3000-.
In a preferred embodiment, the pH value is adjusted to 8 in the fourth step, the stirring rate is 300-600 rpm, and the stirring time is 2-6 h.
The invention has the technical effects and advantages that:
1. the graphene and silver nanowire composite slurry prepared by the raw material formula adopts the modified graphene and the silver nanowire as raw materials, the graphene is firstly oxidized, so that the interlayer spacing of the graphene oxide is increased, the oxygen-containing groups are increased, the surface of the graphene oxide contains a large number of hydroxyl groups and epoxy groups, the edge of the graphene oxide contains more carboxyl groups and carbonyl groups, the dispersion effect of the graphene is better, the silver nanowires can be better adsorbed on the oxidized graphene, the graphene and the silver nanowires are mixed and then reduced by glucose, so that the graphene and the silver nanowires are better combined, then under the action of a dispersant and other assistants, the dispersion effect of the graphene and the silver nanowires is better, the dispersed graphene and silver nanowires can be uniformly distributed in the slurry, so that the conductivity, the antibacterial activity and the far infrared heating uniformity of the composite slurry are enhanced;
2. according to the invention, the modified graphene, the conductive carbon black and the silver nanowires are combined for use and cooperate to further improve the conductivity of the conductive carbon slurry, and the anhydrous ethanol or ammonia water is used as a solvent, so that the modified graphene and silver nanowire mixture has a better dispersion effect.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides graphene silver nanowire composite slurry which comprises the following raw materials in parts by weight: 30 parts of modified graphene, 8 parts of silver nanowires, 6 parts of conductive carbon black, 40 parts of solvent, 30 parts of waterborne polyurethane resin, 10 parts of waterborne epoxy resin, 5 parts of waterborne acrylic resin, 5 parts of glucose, 0.5 part of dispersant and 0.5 part of assistant.
In a preferred embodiment, the diameter of the silver nanowires is 80-250nm, the conductive carbon black is one of ketjen black EC-600JD and conductive carbon black BP-2000, the particle size of the conductive carbon black is 0.1-10um, and the auxiliary agents include a curing agent, a pH buffer, an antifoaming agent, a wetting and leveling agent and a wetting and dispersing agent.
In a preferred embodiment, the dispersant is one or more of sodium dodecyl sulfate, sodium hexadecylbenzene sulfonate, hydroxypropyl methylcellulose and sodium carboxymethylcellulose, the curing agent is ethylenediamine, the pH buffering agent is one or more of ethanolamine, diethanolamine, triethanolamine, dimethylethanolamine and methyldiethanolamine, the defoamer is one or more of polyether, mineral oil emulsion, polyether modified mineral oil or polyether modified silicone, the wetting and leveling agent is one or more of polyether modified polydimethylsiloxane, polyether modified silicone, fluorocarbon modified silicone and fluorocarbon modified polyacrylate water solution, the wetting and dispersing agent is one or more of polyacrylate sodium salt, polyacrylate potassium salt, polycarboxylate sodium salt, polycarboxylate ammonium salt, hydrophobically modified polycarboxylate potassium salt, phosphate ester complex and self-emulsifying modified polyacrylate, the solvent is absolute ethyl alcohol or ammonia water.
The invention also provides a preparation method of the graphene silver nanowire composite slurry, which comprises the following specific preparation steps:
the method comprises the following steps: preparing modified graphene, weighing a certain amount of graphene, putting the graphene into a ball mill, crushing to obtain graphene powder, adding sodium nitrate and concentrated sulfuric acid into the graphene powder, mixing and stirring uniformly, slowly adding potassium permanganate during stirring, continuing stirring for 3 hours after adding the potassium permanganate, heating to 40 ℃ by using a water bath after stirring, preserving heat, adding deionized water after preserving heat, then raising the temperature of the water bath to 95 ℃ for preserving heat, adding 5% hydrogen peroxide solution after preserving heat, washing by using hydrochloric acid and deionized water after reaction until the pH value is neutral, and then carrying out vacuum drying to obtain the modified graphene;
step two: adding deionized water into the modified graphene obtained in the step one, performing ultrasonic dispersion for 2 hours to obtain a modified graphene dispersion solution, then adding silver nanowires into the graphene dispersion solution, performing ultrasonic-assisted stirring uniformly, washing for 4 times by using the deionized water, adding glucose after washing, performing reflux stirring for 10 hours at 95 ℃, filtering, washing and drying the obtained precipitate by using the deionized water and ethanol to obtain a mixture of the modified graphene and the silver nanowires;
step three: putting the weighed conductive carbon black, solvent, dispersant, waterborne polyurethane resin, waterborne epoxy resin and waterborne acrylic resin into a reaction kettle, stirring and mixing for 2h, then ultrasonically dispersing for 5h, performing high-speed ball milling and dispersion by using a ball mill after the ultrasonic dispersion is finished, and filtering to obtain premixed slurry after the ball milling and dispersion are finished;
step four: and (3) adding the mixture obtained in the step two into the premixed slurry obtained in the step three, adding an auxiliary agent for defoaming, dispersing, adjusting the pH value, curing, and continuously and uniformly stirring to obtain the graphene-silver nanowire composite slurry.
In a preferred embodiment, the particle size of the graphene powder obtained after the ball mill is crushed in the first step is 2-30um, the mixing and stirring speed in the first step is 1000 rpm, the primary heat preservation time in the first step is 2.5h, the secondary heat preservation time is 2h, and the vacuum drying temperature is 60 ℃ and the vacuum drying time is 12 h.
In a preferred embodiment, the ultrasonic device power for ultrasonic dispersion in the second step is 4000W, the ultrasonic device power for ultrasonic-assisted stirring is 3000W, and the stirring speed is 1000 rpm.
In a preferred embodiment, the power of the ultrasonic equipment for ultrasonic dispersion in the third step is 4000W, and the filter sieve in the third step is 350-mesh sieve.
In a preferred embodiment, the pH is adjusted to 8 in step four, the stirring is continued at a rate of 500 rpm for a period of 4 hours.
Example 2:
different from the embodiment 1, the material comprises the following raw materials in parts by weight: 40 parts of modified graphene, 12 parts of silver nanowires, 8 parts of conductive carbon black, 50 parts of solvent, 40 parts of waterborne polyurethane resin, 20 parts of waterborne epoxy resin, 10 parts of waterborne acrylic resin, 7 parts of glucose, 2.5 parts of dispersant and 2.5 parts of assistant.
Example 3:
different from the examples 1-2, the material comprises the following raw materials in parts by weight: 50 parts of modified graphene, 16 parts of silver nanowires, 10 parts of conductive carbon black, 60 parts of solvent, 50 parts of waterborne polyurethane resin, 30 parts of waterborne epoxy resin, 15 parts of waterborne acrylic resin, 10 parts of glucose, 5 parts of dispersant and 5 parts of assistant.
Example 4:
the graphene silver nanowire composite slurry comprises the following raw materials in parts by weight: 30 parts of modified graphene, 8 parts of silver nanowires, 6 parts of conductive carbon black, 40 parts of solvent, 30 parts of waterborne polyurethane resin, 10 parts of waterborne epoxy resin, 5 parts of waterborne acrylic resin, 0.5 part of dispersant and 0.5 part of assistant.
In a preferred embodiment, the diameter of the silver nanowires is 80-250nm, the conductive carbon black is one of ketjen black EC-600JD and conductive carbon black BP-2000, the particle size of the conductive carbon black is 0.1-10um, and the auxiliary agents comprise a curing agent, a pH buffer, an antifoaming agent, a wetting and leveling agent and a wetting and dispersing agent.
In a preferred embodiment, the dispersant is one or more of sodium dodecyl sulfate, sodium hexadecylbenzene sulfonate, hydroxypropyl methylcellulose and sodium carboxymethylcellulose, the curing agent is ethylenediamine, the pH buffering agent is one or more of ethanolamine, diethanolamine, triethanolamine, dimethylethanolamine and methyldiethanolamine, the defoamer is one or more of polyether, mineral oil emulsion, polyether modified mineral oil or polyether modified silicone, the wetting and leveling agent is one or more of polyether modified polydimethylsiloxane, polyether modified silicone, fluorocarbon modified silicone and fluorocarbon modified polyacrylate water solution, the wetting and dispersing agent is one or more of polyacrylate sodium salt, polyacrylate potassium salt, polycarboxylate sodium salt, polycarboxylate ammonium salt, hydrophobically modified polycarboxylate potassium salt, phosphate ester complex and self-emulsifying modified polyacrylate, the solvent is absolute ethyl alcohol or ammonia water.
The invention also provides a preparation method of the graphene silver nanowire composite slurry, which comprises the following specific preparation steps:
the method comprises the following steps: preparing modified graphene, weighing a certain amount of graphene, putting the graphene into a ball mill, crushing to obtain graphene powder, adding sodium nitrate and concentrated sulfuric acid into the graphene powder, mixing and stirring uniformly, slowly adding potassium permanganate during stirring, continuing stirring for 3 hours after adding the potassium permanganate, heating to 40 ℃ by using a water bath after stirring, preserving heat, adding deionized water after preserving heat, then raising the temperature of the water bath to 95 ℃ for preserving heat, adding 5% hydrogen peroxide solution after preserving heat, washing by using hydrochloric acid and deionized water after reaction until the pH value is neutral, and then carrying out vacuum drying to obtain the modified graphene;
step two: adding deionized water into the modified graphene obtained in the step one, performing ultrasonic dispersion for 2 hours to obtain a modified graphene dispersion solution, then adding silver nanowires into the graphene dispersion solution, performing ultrasonic-assisted stirring uniformly, and washing for 4 times by using the deionized water to obtain a mixture of the modified graphene and the silver nanowires;
step three: putting the weighed conductive carbon black, solvent, dispersant, waterborne polyurethane resin, waterborne epoxy resin and waterborne acrylic resin into a reaction kettle, stirring and mixing for 2h, then ultrasonically dispersing for 5h, performing high-speed ball milling and dispersion by using a ball mill after the ultrasonic dispersion is finished, and filtering to obtain premixed slurry after the ball milling and dispersion are finished;
step four: and (3) adding the mixture obtained in the step two into the premixed slurry obtained in the step three, adding an auxiliary agent for defoaming, dispersing, adjusting the pH value, curing, and continuously and uniformly stirring to obtain the graphene-silver nanowire composite slurry.
In a preferred embodiment, the particle size of the graphene powder obtained after the ball mill is crushed in the first step is 2-30um, the mixing and stirring speed in the first step is 1000 rpm, the primary heat preservation time in the first step is 2.5h, the secondary heat preservation time is 2h, and the vacuum drying temperature is 60 ℃ and the vacuum drying time is 12 h.
In a preferred embodiment, the ultrasonic device power for ultrasonic dispersion in the second step is 4000W, the ultrasonic device power for ultrasonic-assisted stirring is 3000W, and the stirring speed is 1000 rpm.
In a preferred embodiment, the power of the ultrasonic equipment for ultrasonic dispersion in the third step is 4000W, and the filter sieve in the third step is 350-mesh sieve.
In a preferred embodiment, the pH is adjusted to 8 in step four, the stirring is continued at a rate of 500 rpm for a period of 4 hours.
The graphene silver nanowire composite slurry prepared in the above examples 1 to 4 is respectively used as an experimental group 1, an experimental group 2, an experimental group 3 and an experimental group, a conventional graphene silver nanowire composite slurry is used as a control group for testing, and the selected graphene silver nanowire composite slurry is respectively tested for conductivity, adhesion, bacteriostasis rate and hydrophilicity. The test results are shown in table one:
watch 1
As can be seen from the table one, compared with the conventional graphene silver nanowire composite slurry, the graphene silver nanowire composite slurry produced by the invention has smaller sheet resistance, better adhesion and high bacteriostasis rate, and example 4 adopts modified graphene mixed with silver nanowires without glucose reduction, although the conductivity is improved compared with the conventional graphene silver nanowire composite slurry, the conductivity is obviously reduced compared with example 1, and the hydrophilic performance is better without glucose reduction, so that the invention adopts absolute ethyl alcohol as a solvent, adopts the modified graphene and silver nanowires as raw materials, the graphene is firstly oxidized to increase the lamellar spacing of the graphene oxide, increase oxygen-containing groups, contain a large amount of hydroxyl and epoxy groups on the surface, contain more carboxyl and carbonyl groups at the edge, enable the dispersion effect of the graphene to be better, and the silver nanowires can be better adsorbed on the oxidized graphene, the graphene and the silver nanowires are mixed and then reduced by glucose, so that the graphene and the silver nanowires are better combined, the dispersion effect of the graphene and the silver nanowires is better under the action of a dispersing agent and other auxiliaries, and the graphene and the silver nanowires can be uniformly distributed in the slurry after dispersion, so that the conductivity, the bacteriostasis and the far infrared heating uniformity of the composite slurry are enhanced.
And finally: the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The graphene-silver nanowire composite slurry is characterized in that: the feed comprises the following raw materials in parts by weight: 30-50 parts of modified graphene, 8-16 parts of silver nanowires, 6-10 parts of conductive carbon black, 40-60 parts of solvent, 30-50 parts of waterborne polyurethane resin, 10-30 parts of waterborne epoxy resin, 5-15 parts of waterborne acrylic resin, 5-10 parts of glucose, 0.5-5 parts of dispersant and 0.5-5 parts of auxiliary agent.
2. The graphene-silver nanowire composite paste according to claim 1, characterized in that: the feed comprises the following raw materials in parts by weight: 35-45 parts of modified graphene, 11-13 parts of silver nanowires, 7-9 parts of conductive carbon black, 45-55 parts of solvent, 35-45 parts of waterborne polyurethane resin, 15-25 parts of waterborne epoxy resin, 8-12 parts of waterborne acrylic resin, 6-8 parts of glucose, 2-3 parts of dispersant and 2-3 parts of assistant.
3. The graphene silver nanowire composite paste according to claim 1, wherein: the feed comprises the following raw materials in parts by weight: 40 parts of modified graphene, 12 parts of silver nanowires, 8 parts of conductive carbon black, 50 parts of solvent, 40 parts of waterborne polyurethane resin, 20 parts of waterborne epoxy resin, 10 parts of waterborne acrylic resin, 7 parts of glucose, 2.5 parts of dispersant and 2.5 parts of assistant.
4. The graphene silver nanowire composite paste according to claim 1, wherein: the diameter of the silver nanowire is 80-250nm, the conductive carbon black is one of Ketjen black EC-600JD and conductive carbon black BP-2000, the particle size of the conductive carbon black is 0.1-10um, and the auxiliary agent comprises a curing agent, a pH buffering agent, a defoaming agent, a wetting and leveling agent and a wetting and dispersing agent.
5. The graphene silver nanowire composite paste according to claim 4, wherein: the dispersing agent is one or more of sodium dodecyl sulfate, sodium hexadecylbenzene sulfonate, hydroxypropyl methylcellulose and sodium carboxymethylcellulose, the curing agent is ethylenediamine, the pH buffering agent is one or more of ethanolamine, diethanolamine, triethanolamine, dimethylethanolamine and methyldiethanolamine, the defoaming agent is one or more of polyether, mineral oil emulsion, polyether modified mineral oil or polyether modified organic silicon, the wetting and leveling agent is one or more of polyether modified polydimethylsiloxane, polyether modified organic silicon, fluorocarbon modified organic silicon and fluorocarbon modified polyacrylate water solution, the wetting and dispersing agent is one or more of sodium polyacrylate, potassium polyacrylate, sodium polycarboxylate, ammonium polycarboxylate, hydrophobic modified potassium polycarboxylate, phosphate compound and self-emulsifying modified polyacrylate, the solvent is absolute ethyl alcohol or ammonia water.
6. The method for preparing the graphene-silver nanowire composite paste according to any one of claims 1 to 5, wherein: the preparation method comprises the following specific steps:
the method comprises the following steps: preparing modified graphene, namely weighing a certain amount of graphene, putting the graphene into a ball mill, crushing to obtain graphene powder, adding sodium nitrate and concentrated sulfuric acid into the graphene powder, mixing and stirring uniformly, slowly adding potassium permanganate during stirring, continuing stirring for 2-4 hours after adding potassium permanganate, heating to 35-45 ℃ by using a water bath after stirring, preserving heat, adding deionized water after preserving heat, raising the temperature of the water bath to 90-100 ℃ for preserving heat, adding 5% hydrogen peroxide solution after preserving heat, washing by using hydrochloric acid and deionized water until the pH value is neutral after reaction, and then carrying out vacuum drying to obtain modified graphene;
step two: adding deionized water into the modified graphene obtained in the step one, performing ultrasonic dispersion for 1-2 hours to obtain a modified graphene dispersion solution, then adding silver nanowires into the graphene dispersion solution, performing ultrasonic-assisted stirring, washing for 3-5 times by using the deionized water, adding glucose after washing, performing reflux stirring for 8-12 hours at 90-100 ℃, filtering, washing and drying the obtained precipitate by using the deionized water and ethanol to obtain a mixture of the modified graphene and the silver nanowires;
step three: putting the weighed conductive carbon black, solvent, dispersant, waterborne polyurethane resin, waterborne epoxy resin and waterborne acrylic resin into a reaction kettle, stirring and mixing for 1-2h, then ultrasonically dispersing for 3-8h, performing high-speed ball milling dispersion by using a ball mill after the ultrasonic dispersion is finished, and filtering to obtain premixed slurry after the ball milling dispersion is finished;
step four: and (3) adding the mixture obtained in the step two into the premixed slurry obtained in the step three, adding an auxiliary agent for defoaming, dispersing, adjusting the pH value, curing, and continuously and uniformly stirring to obtain the graphene-silver nanowire composite slurry.
7. The preparation method of the graphene-silver nanowire composite paste according to claim 6, characterized by comprising the following steps: the particle size of the graphene powder obtained after the grinding of the ball mill in the first step is 2-30um, the mixing and stirring speed in the first step is 800-1200 rpm, the primary heat preservation time in the first step is 2-3h, the secondary heat preservation time is 1-2h, the vacuum drying temperature is 50-70 ℃, and the vacuum drying time is 10-14 h.
8. The preparation method of the graphene-silver nanowire composite paste according to claim 6, characterized by comprising the following steps: and the power of the ultrasonic equipment in the ultrasonic dispersion in the step two is 3000-5000W, the power of the ultrasonic equipment in the ultrasonic auxiliary stirring is 2000-4000W, and the stirring speed is 800-1200 r/min.
9. The preparation method of the graphene-silver nanowire composite paste according to claim 6, characterized by comprising the following steps: and the power of the ultrasonic equipment in the ultrasonic dispersion in the third step is 3000-5000W, and the filter sieve in the third step is a 300-400-mesh sieve.
10. The preparation method of the graphene-silver nanowire composite paste according to claim 6, characterized by comprising the following steps: in the fourth step, the pH value is adjusted to be 8, the continuous stirring speed is 300-600 revolutions per minute, and the continuous stirring time is 2-6 h.
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