CN111320916A - Preparation method of ceramic-based conductive coating - Google Patents
Preparation method of ceramic-based conductive coating Download PDFInfo
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- CN111320916A CN111320916A CN201811532175.1A CN201811532175A CN111320916A CN 111320916 A CN111320916 A CN 111320916A CN 201811532175 A CN201811532175 A CN 201811532175A CN 111320916 A CN111320916 A CN 111320916A
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- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- 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
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Abstract
The invention provides a preparation method of a ceramic-based conductive coating, which comprises the following steps: s1, preparing a lanthanum nitrate water solution; s2, preparing tetrabutyl titanate solution; s3, preparing a barium carbonate solution; s4, preparing lanthanum modified barium titanate; s5, adding lanthanum modified barium titanate into a silane coupling agent to obtain surface modified barium titanate, adding the surface modified barium titanate into an HCl solution, adding sodium dodecyl benzene sulfonate, stirring to be transparent, then adding an aniline n-hexane solution, uniformly mixing, stirring in an ice bath, dropwise adding an ammonium persulfate solution after uniform stirring, and obtaining polyaniline-coated barium titanate after dropwise adding; s6, heating the E-44 epoxy resin in a water bath, adding dimethylbenzene and butanol, uniformly stirring, adding 4-methylimidazole, triethylene tetramine and polyaniline-coated barium titanate, and uniformly mixing to obtain the uncured conductive coating. The conductive coating prepared by the preparation method not only has excellent conductivity, but also has corrosion resistance and high reliability.
Description
The technical field is as follows:
the invention relates to the field of conductive coatings, in particular to a preparation method of a ceramic-based conductive coating.
Background art:
an electrically conductive coating is a functional coating that has the ability to conduct electrical current and dissipate accumulated static charge. The conductive coating has important application in a plurality of fields, and can prevent electronic elements from being punctured due to electrostatic discharge in the antistatic field; the coating can be coated on the walls of an oil storage tank and a pipeline to release accumulated static charges and prevent explosion accidents; aiming at the electromagnetic interference in daily life, the conductive coating can play a role in absorbing electromagnetic waves; the conductive paint generates heat when being electrified, and can be used on the surface of some substrates needing heat as a heating paint. The conductive coating has such a wide application and development prospect, so that the conductive coating has important significance for the research of the conductive coating. Conductive coatings as fillers are less applied; at present, silver conductive paint is mostly used in the market, but when the working environment is humid, the electro-migration phenomenon of conductive filler silver can occur, so that the resistivity of the coating is increased, and the conductive performance is reduced; cu and Ni are cheap and do not generate migration phenomenon under an electric field, but Cu and Ni are active in chemical property, easy to oxidize and difficult to maintain good conductivity in the long-term use process. Therefore, the conductive coating needs to be developed and developed with new, high-reliability and high-performance conductive coatings.
The invention content is as follows:
the technical problem to be solved is as follows: the invention aims to provide a preparation method of a ceramic-based conductive coating, and the conductive coating prepared by the preparation method not only has excellent conductivity, but also has corrosion resistance and high reliability.
The technical scheme is as follows: a preparation method of a ceramic-based conductive coating comprises the following steps:
s1, adding lanthanum nitrate into deionized water, and preparing a lanthanum nitrate water solution with the concentration of 5-12 wt%;
s2, dissolving tetrabutyl titanate in ethanol containing citric acid, and stirring until the solution is transparent to obtain a tetrabutyl titanate solution with the concentration of 2-6 wt%;
s3, dissolving barium carbonate in a citric acid solution, and uniformly stirring to obtain a barium carbonate solution with the concentration of 2-6%;
s4, dropwise adding a lanthanum nitrate and tetrabutyl titanate solution into a barium carbonate solution, adjusting the pH value of the solution to 6-8, stirring in a water bath at 75-90 ℃ to obtain sol, and then calcining the sol in a muffle furnace at 800-1000 ℃ for 4-6h to obtain lanthanum modified barium titanate;
s5, adding lanthanum modified barium titanate into a silane coupling agent to obtain surface modified barium titanate, adding the surface modified barium titanate into 1mol/L HCl solution, adding sodium dodecyl benzene sulfonate, stirring to be transparent, then adding aniline in n-hexane solution, uniformly mixing, stirring in ice bath at the temperature of 1-5 ℃, dropwise adding ammonium persulfate solution after uniform stirring, and reacting for 2-5 hours after dropwise adding to obtain polyaniline-coated barium titanate;
s6, heating the E-44 epoxy resin in a water bath, adding dimethylbenzene and butanol, uniformly stirring, adding 4-methylimidazole, triethylene tetramine and polyaniline-coated barium titanate, and uniformly mixing to obtain the uncured conductive coating. Further, in the step S3, the molar ratio of lanthanum nitrate, tetrabutyl titanate and barium carbonate is 0.2-0.5:0.5-0.8: 1.
Further, the silane coupling agent in the step S4 is a KH-560 silane coupling agent.
Further, in the step S4, the mass ratio of the E-44 epoxy resin, the xylene, the butanol, the 4-methylimidazole, the triethylene tetramine and the polyaniline-coated barium titanate is 80-120:5-12:3-6:5-12:8-15: 40-60.
Has the advantages that: the invention has the following advantages: according to the invention, the ceramic material is used as a conductive matrix, polyaniline is generated by an in-situ polymerization method, the stability of the material structure is facilitated, the polyaniline is conductive and has a three-dimensional network structure, and the excellent salt corrosion resistance of the polyaniline is found.
The specific implementation mode is as follows:
example 1
A preparation method of a ceramic-based conductive coating comprises the following steps:
s1, adding lanthanum nitrate into deionized water, and preparing a lanthanum nitrate water solution with the concentration of 5 wt%;
s2, dissolving tetrabutyl titanate in ethanol containing citric acid, and stirring until the solution is transparent to obtain a tetrabutyl titanate solution with the concentration of 2 wt%;
s3, dissolving barium carbonate in a citric acid solution, and uniformly stirring to obtain a barium carbonate solution with the concentration of 2-6%, wherein the molar ratio of lanthanum nitrate to tetrabutyl titanate to barium carbonate is 0.2:0.5: 1;
s4, dropwise adding a lanthanum nitrate and tetrabutyl titanate solution into a barium carbonate solution, adjusting the pH of the solution to 6, stirring in a water bath at 75 ℃ to obtain sol, and then calcining the sol in a muffle furnace at 800 ℃ for 6 hours to obtain lanthanum modified barium titanate;
s5, adding lanthanum modified barium titanate into a KH-560 silane coupling agent to obtain surface modified barium titanate, adding 1mol/L HCl solution into the surface modified barium titanate, adding sodium dodecyl benzene sulfonate, stirring to be transparent, then adding aniline into n-hexane solution, uniformly mixing, stirring in an ice bath at the temperature of 1-5 ℃, dropwise adding ammonium persulfate solution after uniform stirring, and reacting for 2 hours after dropwise adding to obtain polyaniline-coated barium titanate;
s6, heating the E-44 epoxy resin in a water bath, adding dimethylbenzene and butanol, uniformly stirring, adding 4-methylimidazole, triethylene tetramine and polyaniline-coated barium titanate, and uniformly mixing to obtain the uncured conductive coating, wherein the mass ratio of the E-44 epoxy resin, the dimethylbenzene, the butanol, the 4-methylimidazole, the triethylene tetramine and the polyaniline-coated barium titanate is 80:5:6:12:8: 40.
Example 2
A preparation method of a ceramic-based conductive coating comprises the following steps:
s1, adding lanthanum nitrate into deionized water, and preparing a lanthanum nitrate water solution with the concentration of 12 wt%;
s2, dissolving tetrabutyl titanate in ethanol containing citric acid, and stirring until the solution is transparent to obtain a tetrabutyl titanate solution with the concentration of 6 wt%;
s3, dissolving barium carbonate in a citric acid solution, and uniformly stirring to obtain a barium carbonate solution with the concentration of 2-6%, wherein the molar ratio of lanthanum nitrate to tetrabutyl titanate to barium carbonate is 0.5:0.8: 1;
s4, dropwise adding a lanthanum nitrate and tetrabutyl titanate solution into a barium carbonate solution, adjusting the pH of the solution to 8, stirring in a water bath at 90 ℃ to obtain sol, and then placing the sol in a muffle furnace to calcine at 1000 ℃ for 4 hours to obtain lanthanum-modified barium titanate;
s5, adding lanthanum modified barium titanate into a KH-560 silane coupling agent to obtain surface modified barium titanate, adding 1mol/L HCl solution into the surface modified barium titanate, adding sodium dodecyl benzene sulfonate, stirring to be transparent, then adding aniline into n-hexane solution, uniformly mixing, stirring in an ice bath at the temperature of 1-5 ℃, dropwise adding ammonium persulfate solution after uniform stirring, and reacting for 5 hours after dropwise adding to obtain polyaniline-coated barium titanate;
s6, heating the E-44 epoxy resin in a water bath, adding dimethylbenzene and butanol, uniformly stirring, adding 4-methylimidazole, triethylene tetramine and polyaniline-coated barium titanate, and uniformly mixing to obtain the uncured conductive coating, wherein the mass ratio of the E-44 epoxy resin, the dimethylbenzene, the butanol, the 4-methylimidazole, the triethylene tetramine and the polyaniline-coated barium titanate is 120:12:3: 15: 60.
Example 3
A preparation method of a ceramic-based conductive coating comprises the following steps:
s1, adding lanthanum nitrate into deionized water, and preparing a lanthanum nitrate water solution with the concentration of 9 wt%;
s2, dissolving tetrabutyl titanate in ethanol containing citric acid, and stirring until the solution is transparent to obtain a tetrabutyl titanate solution with the concentration of 4 wt%;
s3, dissolving barium carbonate in a citric acid solution, and uniformly stirring to obtain a barium carbonate solution with the concentration of 4%, wherein the molar ratio of lanthanum nitrate to tetrabutyl titanate to barium carbonate is 0.4:0.7: 1;
s4, dropwise adding a lanthanum nitrate and tetrabutyl titanate solution into a barium carbonate solution, adjusting the pH value of the solution to 7, stirring in a water bath at 85 ℃ to obtain sol, and then calcining the sol in a muffle furnace at 900 ℃ for 5 hours to obtain lanthanum modified barium titanate;
s5, adding lanthanum modified barium titanate into a KH-560 silane coupling agent to obtain surface modified barium titanate, adding 1mol/L HCl solution into the surface modified barium titanate, adding sodium dodecyl benzene sulfonate, stirring to be transparent, then adding aniline into n-hexane solution, uniformly mixing, stirring in an ice bath at the temperature of 1-5 ℃, dropwise adding ammonium persulfate solution after uniformly stirring, and reacting for 4 hours after dropwise adding to obtain polyaniline-coated barium titanate;
s6, heating the E-44 epoxy resin in a water bath, adding dimethylbenzene and butanol, uniformly stirring, adding 4-methylimidazole, triethylene tetramine and polyaniline-coated barium titanate, and uniformly mixing to obtain the uncured conductive coating, wherein the mass ratio of the E-44 epoxy resin, the dimethylbenzene, the butanol, the 4-methylimidazole, the triethylene tetramine and the polyaniline-coated barium titanate is 100:9:5:8:12: 50.
Comparative example 1
A preparation method of a ceramic-based conductive coating comprises the following steps:
s1, adding lanthanum nitrate into deionized water, and preparing a lanthanum nitrate water solution with the concentration of 5 wt%;
s2, dissolving tetrabutyl titanate in ethanol containing citric acid, and stirring until the solution is transparent to obtain a tetrabutyl titanate solution with the concentration of 2 wt%;
s3, dissolving barium carbonate in a citric acid solution, and uniformly stirring to obtain a barium carbonate solution with the concentration of 2-6%, wherein the molar ratio of lanthanum nitrate to tetrabutyl titanate to barium carbonate is 0.2:0.5: 1;
s4, dropwise adding a lanthanum nitrate and tetrabutyl titanate solution into a barium carbonate solution, adjusting the pH of the solution to 6, stirring in a water bath at 75 ℃ to obtain sol, and then calcining the sol in a muffle furnace at 800 ℃ for 6 hours to obtain lanthanum modified barium titanate;
s5, heating the E-44 epoxy resin in a water bath, adding xylene and butanol, uniformly stirring, adding 4-methylimidazole, triethylene tetramine and lanthanum-modified barium titanate, and uniformly mixing to obtain the uncured conductive coating, wherein the mass ratio of the E-44 epoxy resin, the xylene, the butanol, the 4-methylimidazole, the triethylene tetramine and the lanthanum-modified barium titanate is 100:9:5:8:12: 50.
Comparative example 2
A preparation method of a conductive coating comprises the following steps:
heating the E-44 epoxy resin in a water bath, adding xylene and butanol, uniformly stirring, adding 4-methylimidazole, triethylene tetramine and polyaniline, and uniformly mixing to obtain the uncured conductive coating, wherein the mass ratio of the E-44 epoxy resin, the xylene, the butanol, the 4-methylimidazole, the triethylene tetramine and the polyaniline is 120:12:3: 15: 60.
And (3) performance testing:
the calculation formula of the resistivity is as follows: rho-RS/L, where rho tableResistivity (Ω · m), resistance (Ω) represented by R, and area (m) represented by S2) L represents a thickness (m);
acid and alkali resistance test of the conductive coating: preparing a sodium chloride solution with the concentration of 3%, and observing the appearance of the coating after 10 days.
| Resistivity (omega. m) | Corrosion resistance | |
| Example 1 | 0.35 | Is free of |
| Example 2 | 0.45 | Is free of |
| Example 3 | 0.32 | Is free of |
| Comparative example 1 | 23 | Small bubble (without polyaniline) |
| Comparative example 2 | 3.6 | Is free of |
Claims (4)
1. The preparation method of the ceramic-based conductive coating is characterized by comprising the following steps of:
s1, adding lanthanum nitrate into deionized water, and preparing a lanthanum nitrate water solution with the concentration of 5-12 wt%;
s2, dissolving tetrabutyl titanate in ethanol containing citric acid, and stirring until the solution is transparent to obtain a tetrabutyl titanate solution with the concentration of 2-6 wt%;
s3, dissolving barium carbonate in a citric acid solution, and uniformly stirring to obtain a barium carbonate solution with the concentration of 2-6%;
s4, dropwise adding a lanthanum nitrate and tetrabutyl titanate solution into a barium carbonate solution, adjusting the pH value of the solution to 6-8, stirring in a water bath at 75-90 ℃ to obtain sol, and then calcining the sol in a muffle furnace at 800-1000 ℃ for 4-6h to obtain lanthanum modified barium titanate;
s5, adding lanthanum modified barium titanate into a silane coupling agent to obtain surface modified barium titanate, adding the surface modified barium titanate into 1mol/L HCl solution, adding sodium dodecyl benzene sulfonate, stirring to be transparent, then adding aniline in n-hexane solution, uniformly mixing, stirring in ice bath at the temperature of 1-5 ℃, dropwise adding ammonium persulfate solution after uniform stirring, and reacting for 2-5 hours after dropwise adding to obtain polyaniline-coated barium titanate;
s6, heating the E-44 epoxy resin in a water bath, adding dimethylbenzene and butanol, uniformly stirring, adding 4-methylimidazole, triethylene tetramine and polyaniline-coated barium titanate, and uniformly mixing to obtain the uncured conductive coating.
2. The method for preparing the ceramic-based conductive coating according to claim 1, wherein the method comprises the following steps: in the step S3, the molar ratio of lanthanum nitrate, tetrabutyl titanate and barium carbonate is 0.2-0.5:0.5-0.8: 1.
3. The method for preparing the ceramic-based conductive coating according to claim 1, wherein the method comprises the following steps: the silane coupling agent in the step S4 is KH-560 silane coupling agent.
4. The method for preparing the ceramic-based conductive coating according to claim 1, wherein the method comprises the following steps: in the step S4, the mass ratio of the E-44 epoxy resin, the xylene, the butanol, the 4-methylimidazole, the triethylene tetramine and the polyaniline-coated barium titanate is 80-120:5-12:3-6:5-12:8-15: 40-60.
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| CN201811532175.1A CN111320916A (en) | 2018-12-14 | 2018-12-14 | Preparation method of ceramic-based conductive coating |
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| CN201811532175.1A CN111320916A (en) | 2018-12-14 | 2018-12-14 | Preparation method of ceramic-based conductive coating |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114678177A (en) * | 2022-03-30 | 2022-06-28 | 天津瑞肯新型材料科技有限公司 | Composite positive temperature coefficient thermistor material and preparation method thereof |
| CN117658612A (en) * | 2023-12-05 | 2024-03-08 | 宜兴市海王陶瓷研究所 | Super-induction functional material and preparation method and application thereof |
Citations (1)
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| CN101643607A (en) * | 2008-08-06 | 2010-02-10 | 中国科学院金属研究所 | Polyaniline modified metal-ceramic nano coating and preparation method thereof |
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2018
- 2018-12-14 CN CN201811532175.1A patent/CN111320916A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101643607A (en) * | 2008-08-06 | 2010-02-10 | 中国科学院金属研究所 | Polyaniline modified metal-ceramic nano coating and preparation method thereof |
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| 刘国杰: "《现代涂料与涂装技术》", 31 May 2002, 中国轻工业出版社 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114678177A (en) * | 2022-03-30 | 2022-06-28 | 天津瑞肯新型材料科技有限公司 | Composite positive temperature coefficient thermistor material and preparation method thereof |
| CN117658612A (en) * | 2023-12-05 | 2024-03-08 | 宜兴市海王陶瓷研究所 | Super-induction functional material and preparation method and application thereof |
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Application publication date: 20200623 |