CN116554734A - Nickel-based conductive ink and preparation method of conductive coating material - Google Patents
Nickel-based conductive ink and preparation method of conductive coating material Download PDFInfo
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- CN116554734A CN116554734A CN202310213711.6A CN202310213711A CN116554734A CN 116554734 A CN116554734 A CN 116554734A CN 202310213711 A CN202310213711 A CN 202310213711A CN 116554734 A CN116554734 A CN 116554734A
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- nickel
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- conductive ink
- based conductive
- nickel powder
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 238000000576 coating method Methods 0.000 title claims abstract description 46
- 239000011248 coating agent Substances 0.000 title claims abstract description 44
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000002270 dispersing agent Substances 0.000 claims abstract description 31
- 229920005989 resin Polymers 0.000 claims abstract description 28
- 239000011347 resin Substances 0.000 claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 20
- 239000000654 additive Substances 0.000 claims abstract description 18
- 230000000996 additive effect Effects 0.000 claims abstract description 18
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 17
- DIOYAVUHUXAUPX-KHPPLWFESA-N Oleoyl sarcosine Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)N(C)CC(O)=O DIOYAVUHUXAUPX-KHPPLWFESA-N 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 239000000080 wetting agent Substances 0.000 claims abstract description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims abstract description 4
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- 150000003839 salts Chemical class 0.000 claims abstract 3
- 238000003756 stirring Methods 0.000 claims description 24
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 239000011889 copper foil Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000005096 rolling process Methods 0.000 claims description 6
- 239000011265 semifinished product Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- 229920005749 polyurethane resin Polymers 0.000 claims description 4
- QYMFNZIUDRQRSA-UHFFFAOYSA-N dimethyl butanedioate;dimethyl hexanedioate;dimethyl pentanedioate Chemical compound COC(=O)CCC(=O)OC.COC(=O)CCCC(=O)OC.COC(=O)CCCCC(=O)OC QYMFNZIUDRQRSA-UHFFFAOYSA-N 0.000 claims description 3
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- 239000006229 carbon black Substances 0.000 claims 2
- 239000002994 raw material Substances 0.000 claims 2
- 238000000034 method Methods 0.000 abstract description 7
- 230000002776 aggregation Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 238000004062 sedimentation Methods 0.000 abstract description 4
- 238000004220 aggregation Methods 0.000 abstract description 3
- 239000003973 paint Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000976 ink Substances 0.000 description 42
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 229910021389 graphene Inorganic materials 0.000 description 4
- 238000011282 treatment Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 241000282320 Panthera leo Species 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- RRQYJINTUHWNHW-UHFFFAOYSA-N 1-ethoxy-2-(2-ethoxyethoxy)ethane Chemical compound CCOCCOCCOCC RRQYJINTUHWNHW-UHFFFAOYSA-N 0.000 description 2
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000011231 conductive filler Substances 0.000 description 2
- 239000002872 contrast media Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 229940019778 diethylene glycol diethyl ether Drugs 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 150000002170 ethers Chemical class 0.000 description 2
- 239000005453 ketone based solvent Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 235000013824 polyphenols Nutrition 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000005341 toughened glass Substances 0.000 description 2
- 210000002268 wool Anatomy 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000002653 magnetic therapy Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/033—Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Conductive Materials (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a preparation method of nickel-based conductive ink and a conductive coating material, which belongs to the technical field of paint, and uses 5-20 parts of film-forming resin; 30-70 parts of nickel powder; 1-5 parts of carbon material; 0.01 to 0.5 part of first dispersant oleoyl sarcosine; 0.01 to 0.5 part of second dispersant ammonium polyacrylate salt; 0.1-1 part of additive; 30-50 parts of a solvent; wherein, the particle size of the nickel powder is 1-5 microns; the additive is any one or more of wetting agent and leveling agent. The invention adopts oleoyl sarcosine to pretreat nickel powder, which can effectively disperse when resin and solvent are added in the follow-up process, thus preventing sedimentation and aggregation; has good effect on nickel powder with different production modes. The conductive ink has wide viscosity adjustment range and various coating forms. Compared with the traditional nickel-based conductive ink, the coating has lower resistivity and better coating strength.
Description
Technical Field
The invention relates to the technical field of paint, in particular to a preparation method of nickel-based conductive ink and a conductive coating material.
Background
With the rapid development of modern science and technology, the conductive ink is used as a novel special functional coating and is mainly applied to the fields of electronics, integrated circuit packaging, electromagnetic wave shielding, power transmission and transformation equipment, petrochemical industry, aerospace and the like. The conductive coating is generally used for removing static charges in the substrate, conducting current, and forming a protective layer on the surface of the substrate, so that damage of corrosive media to the substrate is effectively prevented.
Conductive inks can be categorized into two general categories, filled conductive inks and intrinsic conductive inks, according to the conductivity mechanism. The filling type conductive ink is a coating prepared by adding conductive filler into non-conductive plastic. The good dispersion performance of the conductive phase metal in the conductive ink directly influences the conductive performance of the conductive ink, and the higher the dispersion and stability of the metal, the better the performance of the conductive ink. With the continuous rising of the price of noble metals, the use of base metals instead of noble metals is a trend, wherein the metal nickel has low cost, small electron migration rate, stable process, good corrosion resistance and heat resistance, low resistivity and good impedance frequency characteristic, and is widely applied to conductive slurry, high-efficiency catalysts, special coatings, wave-absorbing materials, the fields of biological medicine, magnetic therapy and health care, and the like. The existing nickel paste conductive ink is generally prepared by blending a matrix resin material with conductive powder such as nickel powder, but has the defects of high specific gravity, easiness in sedimentation in a system, easiness in agglomeration of particles and difficulty in dispersion due to the special property of the nickel powder. The existing nickel powder is difficult to disperse in matrix resin, more conductive filler needs to be added when a good conductive path needs to be formed, the content ratio of the matrix resin is inevitably reduced, the adhesion of the conductive material to a base material is insufficient, and the phenomena of scratch, paint dropping of a coating film and the like are easy to occur. The increase of the content of the matrix resin can densify the coating film and improve the corrosion resistance, but the conductivity of the prepared conductive ink is also reduced. The common conductive ink has the characteristics of excellent conductive performance, thin thickness of a coated coating and the like, but the coating has low adhesive force and poor wear resistance, and the performance of the coating on protecting a substrate, conducting current and shielding electromagnetic is greatly reduced along with the increase of the service time.
The preparation method of the conductive ink proposed by CN110591462A and CN112646489A can reach the surface resistivity of 0.5 multiplied by 10 2 ～1×10 3 Omega, and can produce good adhesion on the surface of the plastic matrix. But has the disadvantage that the surface resistivity is notThe conductive ink can be applied to devices with high requirements on resistance, such as the fields with high requirements on electromagnetic wave shielding, such as airport navigation, radar and the like, has complex preparation process, needs an external magnetic field and has high requirements on devices, and in addition, the conductive ink prepared by singly adopting film-forming resin, graphene and chopped nanofiber has simple process, but the graphene has higher addition amount, high price and difficult application on a large scale on the market.
Under the current situation, developing a conductive ink with high wear resistance and better conductivity to meet the market demands becomes an urgent problem to be solved.
Disclosure of Invention
According to the technical problems that the prior art of the conductive ink provided by the invention is poor in nickel powder treatment, poor in wear resistance of the conductive coating and the like, the nickel-based conductive ink and the conductive coating material thereof are provided. The preparation method has the advantages of simple preparation industry, better slurry dispersibility and wider application field.
The application provides conductive ink which has good wear resistance and conductivity.
Embodiments of the present application are implemented as follows:
5-20 parts of film forming resin;
30-70 parts of nickel powder;
1 to 5 parts of carbon material
0.01 to 0.5 part of first dispersing agent;
0.01 to 0.5 part of second dispersant
0.1 to 1 part of additive
30-50 parts of solvent
Wherein, the particle size of the nickel powder is 1-5 microns;
the additive is any one or more of wetting agent and leveling agent.
Film-forming resin such as polyphenoxy resin, polyurethane resin and epoxy resin.
And the carbon material is any one or more of conductive carbon black, carbon nano tubes and graphene.
The wear resistance of the nickel-based conductive ink and the conductive coating material thereof is improved by 0.5-10 times compared with that of the contrast material.
A nickel-based conductive ink and a conductive coating material thereof, wherein the solvent comprises any one or more of ketone solvents, esters, ethers and alcohols.
Alternatively, the solvent includes, but is not limited to, a mixture of ketone solvents, esters, ethers, alcohols solvents; optionally, the ketone solvent includes, but is not limited to, any one or more of acetone, butanone, cyclohexanone; alternatively, the ester solvent includes, but is not limited to, any one or more of ethyl acetate, dibasic ester, diethylene glycol diethyl ether acetate.
The film forming resin includes epoxy phenolic epoxy resins, polyurethane resins, bisphenol a based epoxy polymers, silicone resins, and mixtures thereof.
In the application of the invention, any one or more of the above combined film forming resins can be selected, the coating property of the conductive ink is good, the coating film is stable, and the compactness is good, so that the film forming resin is preferable.
Preferably, the film-forming resin can be selected from a polyphenylene oxide resin and a polyurethane resin, and has higher strength, rigidity and toughness.
In the application, the selected use of the polyphenoxy resin can form a compact three-dimensional network structure under the normal temperature or heating condition, and the obtained coating has good mechanical property, adhesion force of a substrate and great improvement of medium resistance
The wear-resistant performance of the high wear-resistant conductive coating material is improved by 0.5-10 times compared with that of a contrast material.
The first dispersant is oleoyl sarcosine.
The second dispersant is ammonium polyacrylate.
The carbon material includes, but is not limited to, any one or more of conductive carbon black, carbon nanotubes, and graphene.
The invention also provides a preparation method of the nickel-based conductive ink and the conductive coating material thereof, which comprises the following steps,
s1, putting nickel powder and a first dispersing agent into a planetary vacuum stirrer according to a proportion, setting the rotating speed to be 30-60 r/min, and stirring for 30-60 min;
s2, vacuumizing the planetary vacuum stirrer, wherein the air pressure is-0.4 to-0.8 MPa;
s3, continuously stirring for 1-10 min at the rotating speed of 600-800 rpm;
s4, turning on a planetary vacuum stirrer, pouring the film-forming resin, the solvent, the second dispersant and the additive into the planetary vacuum stirrer according to a proportion, setting the rotating speed to be 5-15 r/min, and stirring for 1-5 min;
s5, pouring the carbon material into a planetary vacuum stirrer, and increasing the internal rotation speed to 30-60 r/min, wherein the stirring time is 10-30 min;
s8, transferring the stirred slurry semi-finished product to a three-roller dispersing machine for dispersing, wherein the roller spacing is 5-20 micrometers, and rolling for 2-5 rounds to obtain the nickel-based conductive ink.
S9, coating the nickel-based conductive ink on the copper foil, and drying to obtain the conductive coating material.
Compared with the prior art, the invention has the following advantages:
1. the invention adopts oleoyl sarcosine to pretreat nickel powder, which can effectively disperse when resin and solvent are added in the follow-up process, thus preventing sedimentation and aggregation; has good effect on nickel powder with different production modes.
2. The conductive ink disclosed by the invention has the advantages of wide viscosity adjustment range and various coating forms.
3. Compared with the traditional nickel-based conductive ink, the conductive ink provided by the invention has lower resistivity and better film strength.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to the drawings without inventive effort to a person skilled in the art.
FIG. 1 is a photograph showing the state of nickel powder in deionized water after oleoyl sarcosine treatment according to the present invention,
figure 2 is a photograph of a conductive coating material coated on a copper foil with the nickel-based conductive ink of the present invention,
fig. 3 is a microscopic photograph of the conductive coating material of the present invention.
Detailed Description
The following describes in further detail a method for preparing a nickel-based conductive ink and conductive coating material of the present application with reference to examples.
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the invention, as presented in the accompanying drawings, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the present invention, all the embodiments, implementations and features of the invention may be combined with each other without contradiction or conflict. In the present invention, conventional equipment, devices, components, etc., are either commercially available or homemade in accordance with the present disclosure. In the present invention, some conventional operations and apparatuses, devices, components are omitted or only briefly described in order to highlight the gist of the present invention.
Unless specifically stated otherwise, the procedures and treatments involved in this application are conventional in the art.
The instruments used in this application are conventional in the art, unless specifically indicated otherwise.
Example 1
S1, 50 parts of nickel powder and 0.3 part of a first dispersing agent are proportionally put into a planetary vacuum stirrer, the rotating speed is set to be 30 revolutions per minute, and stirring time is set to be minutes;
s2, vacuumizing the planetary vacuum stirrer, wherein the air pressure is-0.8 MPa;
s3, continuously stirring for 2 minutes at the rotating speed of 800 rpm;
s4, turning on a planetary vacuum stirrer, pouring 9 parts of the polyphenol oxide resin, 45 parts of diethylene glycol diethyl ether acetate solvent, 0.02 part of a second dispersing agent and 0.1 part of an additive into the planetary vacuum stirrer in proportion, setting the rotating speed to 15 r/min, and stirring for 5min;
s5, pouring 2 parts of carbon materials into a planetary vacuum stirrer, and increasing the internal rotation speed to 30 r/min, wherein the stirring time is 20min;
s8, transferring the stirred slurry semi-finished product to a three-roller dispersing machine for dispersing, wherein the roller spacing is 10 micrometers, and rolling for 3 rounds to obtain the nickel-based conductive ink.
S9, coating the nickel-based conductive ink on the copper foil, and drying to obtain the conductive coating material.
Wherein;
the nickel powder is 1 micron spherical nickel powder produced by Shanghai Panta powder materials Co.
The first dispersant is oleoyl sarcosine ESLEAM produced by Nikko Co., ltd TM 221P。
The second dispersant is DISPERBYK-130 manufactured by Pick chemistry.
The additive is a leveling agent RHEYBYK-430 produced by Pick chemistry.
The carbon material is nanometer conductive carbon black EC-600JD produced by Japanese lion king.
Example 2
S1, 50 parts of nickel powder and 0.5 part of a first dispersing agent are proportionally put into a planetary vacuum stirrer, the rotating speed is set to be 30 revolutions per minute, and stirring time is set to be minutes;
s2, vacuumizing the planetary vacuum stirrer, wherein the air pressure is-0.8 MPa;
s3, continuously stirring for 2 minutes at the rotating speed of 800 rpm;
s4, turning on a planetary vacuum stirrer, pouring 9 parts of film-forming resin, 60 parts of ethyl acetate solvent, 0.02 part of second dispersing agent and 0.1 part of additive into the planetary vacuum stirrer in proportion, setting the rotating speed to 15 revolutions per minute, and stirring for 5 minutes;
s5, pouring 2 parts of carbon materials into a planetary vacuum stirrer, and increasing the internal rotation speed to 30 r/min, wherein the stirring time is 20min;
s8, transferring the stirred slurry semi-finished product to a three-roller dispersing machine for dispersing, wherein the roller spacing is 5 micrometers, and rolling for 3 rounds to obtain the nickel-based conductive ink.
S9, coating the nickel-based conductive ink on the copper foil, and drying to obtain the conductive coating material.
Wherein;
the nickel powder is 1 micron spherical nickel powder produced by Shanghai Panta powder materials Co.
The first dispersant is oleoyl sarcosine ESLEAM produced by Nikko Co., ltd TM 221P。
The second dispersant is DISPERBYK-130 manufactured by Pick chemistry.
The additive is a leveling agent RHEYBYK-430 produced by Pick chemistry.
The film-forming resin is produced by Lubo5719 TPU。
The carbon material is nanometer conductive carbon black EC-600JD produced by Japanese lion king.
Example 3
S1, putting 60 parts of nickel powder and 0.6 part of a first dispersing agent into a planetary vacuum stirrer according to a proportion, setting the rotating speed to be 30 revolutions per minute, and stirring for a period of minutes;
s2, vacuumizing the planetary vacuum stirrer, wherein the air pressure is-0.5 MPa;
s3, continuously stirring for 2 minutes at the rotating speed of 800 rpm;
s4, turning on a planetary vacuum stirrer, pouring 9 parts of epoxy resin, 45 parts of ethyl acetate solvent, 0.02 part of second dispersing agent and 0.1 part of additive into the planetary vacuum stirrer in proportion, setting the rotating speed to 15 revolutions per minute, and stirring for 5 minutes;
s5, pouring 2 parts of carbon materials into a planetary vacuum stirrer, and increasing the internal rotation speed to 30 r/min, wherein the stirring time is 20min;
s8, transferring the stirred slurry semi-finished product to a three-roller dispersing machine for dispersing, wherein the roller spacing is 10 micrometers, and rolling for 3 rounds to obtain the nickel-based conductive ink.
S9, coating the nickel-based conductive ink on the copper foil, and drying to obtain the conductive coating material.
Wherein;
the nickel powder is 1 micron flake nickel powder produced by Shanghai Panta powder materials Co.
The first dispersant is oleoyl sarcosine ESLEAM produced by Nikko Co., ltd TM 221P。
The second dispersant is BYKJET-9152 produced by Pick chemistry.
The additive is RHEYBYK-430 produced by Pick chemistry.
The carbon material is nanometer conductive carbon black EC-300JD produced by Japanese lion king.
Example 4
S1, 50 parts of nickel powder and 0.5 part of a first dispersing agent are proportionally put into a planetary vacuum stirrer, the rotating speed is set to be 30 revolutions per minute, and stirring time is set to be minutes;
s2, vacuumizing the planetary vacuum stirrer, wherein the air pressure is-0.8 MPa;
s3, continuously stirring for 2 minutes at the rotating speed of 800 rpm;
s4, turning on a planetary vacuum stirrer, pouring 9 parts of film-forming resin, 45 parts of DBE solvent (dibasic ester), 0.02 part of second dispersant and 0.1 part of additive into the planetary vacuum stirrer in proportion, setting the rotating speed to 15 r/min, and stirring for 5min;
s5, pouring 2 parts of carbon materials into a planetary vacuum stirrer, and increasing the internal rotation speed to 30 r/min, wherein the stirring time is 20min;
s8, transferring the stirred slurry semi-finished product to a three-roller dispersing machine for dispersing, wherein the roller spacing is 10 micrometers, and rolling for 3 rounds to obtain the nickel-based conductive ink.
S9, coating the nickel-based conductive ink on the copper foil, and drying to obtain the conductive coating material.
Wherein;
the nickel powder is 1 micron spherical nickel powder produced by Shanghai Panta powder materials Co.
The first dispersant is oleoyl sarcosine ESLEAM produced by Nikko Co., ltd TM 221P。
The second dispersant is ISPRBYK-130, manufactured by Pick chemistry.
The additive is wetting agent BYKJET-9152 produced by Pick chemistry. .
The film-forming resin is produced by Lubo5719 TPU。
The carbon material is SP conductive carbon black.
Fig. 1 shows the nickel powder and the first dispersant after treatment, the nickel powder is loose, can be effectively dispersed when resin and solvent are added subsequently, and can prevent sedimentation and aggregation, thereby ensuring the performance.
The detection method according to the specific embodiment of the present application is as follows:
the coatings prepared using the method of the present invention were tested for surface resistivity as shown in fig. 2 and 3:
test sample preparation: and (3) scraping the prepared conductive ink onto the toughened glass with the surface treated by using automatic scraping equipment, baking the toughened glass at 140 ℃ for 10 minutes, taking out a sample plate, and testing the surface resistivity of the coating on the surface of the sample plate.
Testing the surface resistivity of the coating by using a volume resistance tester;
the abrasion resistance is tested by a solvent-resistant wiper, comprising ethanol-resistant wiping and steel wool-resistant wiping;
the viscosity was measured using a cone-plate viscometer.
Table 1 comparison of properties of different examples of nickel-based conductive inks
| Nickel-based conductive ink | Example 1 | Example 2 | Example 3 | Example 4 |
| Resistivity/Ω cm | 1.86*10 -3 | 1.13*10 -3 | 1.37*10 -3 | 2.46*10 -3 |
| Coating thickness/. Mu.m | 10 | 10 | 10 | 10 |
| Ethanol resistant wiping/secondary | 3500 | 3800 | 4500 | 4470 |
| Steel wool wiping/secondary resistant | 200 | 180 | 200 | 200 |
Finally, it should be noted that: the above examples are only specific embodiments of the present invention, and are not intended to limit the scope of the present invention, but it should be understood by those skilled in the art that the present invention is not limited thereto, and that the present invention is described in detail with reference to the foregoing examples: any person skilled in the art may modify or easily conceive of the technical solution described in the foregoing embodiments, or perform equivalent substitution of some of the technical features, while remaining within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention, and are intended to be included in the scope of the present invention. Accordingly, the scope of the invention is to be protected by the following claims.
Claims (7)
1. The nickel-based conductive ink is characterized by comprising the following raw materials in parts by weight:
5-20 parts of film forming resin;
30-70 parts of nickel powder;
1-5 parts of carbon material;
0.01 to 0.5 part of first dispersant oleoyl sarcosine;
0.01 to 0.5 part of second dispersant ammonium polyacrylate salt;
0.1-1 part of additive;
30-50 parts of a solvent;
wherein, the particle size of the nickel powder is 1-5 microns;
the additive is any one or more of wetting agent and leveling agent.
2. The nickel-based conductive ink according to claim 1, wherein the solvent is selected from any one or more of an ester solvent, an ether solvent, and an alcohol solvent.
3. The nickel-based conductive ink of claim 1, wherein the film-forming resin is selected from any one of polyurethane resin, epoxy resin.
4. The nickel-based conductive ink of claim 1, wherein the carbon material is selected from any one or more of conductive carbon black, superconductive carbon black.
5. The nickel-based conductive ink of claim 1, wherein the carbon material is any one of nano conductive carbon black and superconducting carbon black.
6. The nickel-based conductive ink according to claim 1, comprising the following raw materials in parts by weight: 9 parts of film forming resin TPU;
50 parts of nickel powder;
2 parts of SP conductive carbon black;
0.5 parts of a first dispersant oleoyl sarcosine;
0.02 parts of a second dispersant ammonium polyacrylate salt;
0.1 part of additive;
45 parts of a dibasic ester;
wherein, the nickel powder is in a sphere shape of 1 micrometer;
the additive is a wetting agent.
7. A process for preparing a conductive coating material, characterized in that a nickel-based conductive ink according to any one of claims 1 to 6 is used, which comprises the following steps:
s1, putting nickel powder and a first dispersing agent into a planetary vacuum stirrer according to a proportion, setting the rotating speed to be 30-60 r/min, and stirring for 30-60 min;
s2, vacuumizing the planetary vacuum stirrer, wherein the air pressure is-0.4 to-0.8 MPa;
s3, continuously stirring for 1-10 min under the condition of 600-800 revolutions per minute;
s4, turning on a planetary vacuum stirrer, pouring the film-forming resin, the solvent, the second dispersant and the additive into the planetary vacuum stirrer according to a proportion, setting the rotating speed to be 5-15 r/min, and stirring for 1-5 min;
s5, pouring the carbon material into a planetary vacuum stirrer, and increasing the internal rotation speed to 30-60 r/min, wherein the stirring time is 10-30 min;
s8, transferring the stirred slurry semi-finished product to a three-roller dispersing machine for dispersing, wherein the roller spacing is 5-20 micrometers, and rolling for 2-5 rounds to obtain nickel-based conductive ink;
s9, coating the nickel-based conductive ink on the copper foil, and drying to obtain the conductive coating material.
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