CN111334230A - Preparation method of conductive carbon adhesive - Google Patents
Preparation method of conductive carbon adhesive Download PDFInfo
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- CN111334230A CN111334230A CN202010295773.2A CN202010295773A CN111334230A CN 111334230 A CN111334230 A CN 111334230A CN 202010295773 A CN202010295773 A CN 202010295773A CN 111334230 A CN111334230 A CN 111334230A
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives 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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/18—Spheres
Abstract
The invention discloses a preparation method of conductive carbon adhesive, which comprises the following steps: step one, uniformly mixing 100 parts by weight of epoxy resin, 3-5 parts by weight of dispersant and 1-10 parts by weight of organic solvent to obtain a first mixture with the viscosity of 500-2000 centipoises; step two, preparing a liquid A containing graphene oxide; step three, preparing a dispersion liquid; step four, taking the dispersion liquid to obtain microsphere powder in a spray drying mode, namely graphene oxide-polyaniline composite microspheres; and fifthly, adding the graphene oxide-polyaniline composite microspheres into the first mixture to obtain the conductive carbon adhesive. The composite microspheres are prepared from graphene oxide and polyaniline, and then are used as fillers of epoxy resin to prepare the conductive adhesive, so that the conductive adhesive has good conductivity, flexibility, tear resistance and the like.
Description
Technical Field
The invention relates to the technical field of conductive adhesive preparation, in particular to a preparation method of a conductive carbon adhesive.
Background
The conductive adhesive mainly comprises a resin matrix, conductive particles, a dispersing agent, an auxiliary agent and the like. The matrix mainly comprises epoxy resin, acrylate resin, polyvinyl chloride and the like, and most of the conductive adhesives used in the current market are filler type. Conventional conductive fillers are typically powders of gold, silver, copper, aluminum, zinc, iron, nickel, and graphite and some conductive compounds. However, the addition amount of the conductive filler in the conductive adhesive is generally over 50%, which often causes the viscosity of the resin matrix of the conductive adhesive to be greatly increased, and affects the mechanical properties of the adhesive. The metal powder is used as a filler, so that the cost is high and heavy metal pollution is easy to generate; the graphite powder has low cost and small relative density, but the prepared conductive adhesive has poor conductivity.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and to provide at least the advantages described later.
The invention also aims to provide a preparation method of the conductive carbon adhesive, which prepares the composite microspheres through graphene oxide and polyaniline and further prepares the conductive adhesive as a filler of epoxy resin, and the conductive carbon adhesive has good conductivity, flexibility, tear resistance and the like.
To achieve these objects and other advantages in accordance with the present invention, there is provided a method for preparing a conductive carbon paste, comprising the steps of:
step one, uniformly mixing 100 parts by weight of epoxy resin, 3-5 parts by weight of dispersant and 1-10 parts by weight of organic solvent to obtain a first mixture with the viscosity of 500-2000 centipoises;
step two, putting 2-5 parts by weight of graphite powder with the particle size of less than 20 mu m into 100 parts by weight of concentrated sulfuric acid, adding 2-5 parts by weight of sodium nitrate and 5-10 parts by weight of potassium permanganate while stirring, controlling the reaction temperature to be lower than 25 ℃, stirring for 30-60min, then heating to 40 ℃, stirring for 40-60min, then adding 20-40 parts by weight of oxalic acid solution, and cooling to room temperature after the solution is bright yellow to obtain liquid A containing graphene oxide;
step three, adding 10-15 parts by weight of emulsifier and 20-30 parts by weight of dimethylbenzene into the liquid A in the step two, uniformly stirring, continuously adding 20-30 parts by weight of aniline monomer, uniformly mixing to obtain a second mixture, controlling the temperature of the second mixture below 3 ℃ by adopting an ice water bath, then dropwise adding an ammonium persulfate solution with the concentration of 3-4mol/L at the speed of 5-10 seconds per drop, and stopping stirring until a dark green color appears to obtain a dispersion liquid;
step four, taking the dispersion liquid prepared in the step three, and obtaining microsphere powder in a spray drying mode, namely the graphene oxide-polyaniline composite microspheres;
and step five, adding the graphene oxide-polyaniline composite microspheres prepared in the step four into the first mixture prepared in the step one, stirring for 1-2 hours, then adding 1-2 parts by weight of a curing agent, and stirring for 1-2 hours at the temperature of 20 ℃ to obtain the conductive carbon adhesive.
Preferably, in the first step, the epoxy resin is one or more of glycidyl ester epoxy resin, alicyclic epoxy resin and aliphatic epoxy resin.
Preferably, the organic solvent in the first step is one or more of ethylene glycol diglycidyl ether, polypropylene glycol diglycidyl ether, absolute ethyl alcohol and C12-14 fatty glycidyl ether.
Preferably, in the fifth step, the curing agent is a photo-curing agent or a latent curing agent.
The invention also provides a conductive carbon adhesive prepared by the preparation method of the conductive carbon adhesive according to any one of claims 1 to 4.
The conductive carbon adhesive prepared by the invention is applied to thin film transistors and electromagnetic shielding devices.
The invention at least comprises the following beneficial effects:
the graphene oxide prepared by the invention contains abundant oxidizing functional groups, such as carboxyl, on the surface of a sheet layer. After the aniline monomer is added, the amino group on the aniline monomer reacts with the carboxyl group of the graphene oxide. When an initiator (ammonium persulfate) is added to initiate monomer polymerization, the polyaniline molecular chain starts to grow by taking the graphene oxide as one end point, and finally the graphene oxide material wrapped by the polyaniline molecules is formed. The polyaniline-coated graphene oxide microsphere powder material can be obtained by spray drying. Because the surface of the material is made of a high polymer material, the compatibility of the material with epoxy resin is improved, the conductivity of graphene oxide can be further exerted, and polyaniline is also a conductive polymer, the graphene oxide-polyaniline microspheres can be used as an excellent conductive filler to prepare conductive adhesive containing carbon materials.
When the consumption of the conductive carbon adhesive prepared by the invention is less, the conductive carbon adhesive can have the conductivity equivalent to that of the conductive adhesive containing the metal filler. Meanwhile, compared with the conductive adhesive filled with carbon materials such as carbon nanotubes and graphene, the initial raw material graphite powder of the composite microspheres has obvious cost advantage compared with the carbon nanotubes, expensive reducing agents are not needed to reduce graphene oxide into graphene, and the polyaniline wrapped on the surface has better compatibility with epoxy resin, so that the finally prepared conductive carbon adhesive has better mechanical properties such as flexibility and tear resistance.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
< example 1>
The invention provides a preparation method of conductive carbon adhesive, which comprises the following steps:
step one, uniformly mixing 100 parts by weight of epoxy resin, 3 parts by weight of dispersant and 1 part by weight of organic solvent to obtain a first mixture with the viscosity of 500 centipoises;
step two, taking 2-5 parts by weight of graphite powder with the particle size of less than 20 microns, putting the graphite powder into 100 parts by weight of concentrated sulfuric acid, adding 2 parts by weight of sodium nitrate and 5 parts by weight of potassium permanganate while stirring, controlling the reaction temperature to be lower than 25 ℃, stirring for 30min, then heating to 40 ℃, stirring for 40min, then adding 20 parts by weight of oxalic acid solution, and cooling to room temperature after the solution is bright yellow to obtain liquid A containing graphene oxide;
step three, adding 10 parts by weight of emulsifier and 20 parts by weight of dimethylbenzene into the liquid A in the step two, uniformly stirring, continuously adding 20 parts by weight of aniline monomer, uniformly mixing to obtain a second mixture, controlling the temperature of the second mixture to be below 3 ℃ by adopting an ice-water bath, then dropwise adding an ammonium persulfate solution with the concentration of 3mol/L at the speed of 5 seconds per drop, and stopping stirring until dark green appears to obtain a dispersion liquid;
step four, taking the dispersion liquid prepared in the step three, and obtaining microsphere powder in a spray drying mode, namely the graphene oxide-polyaniline composite microspheres;
and step five, adding the graphene oxide-polyaniline composite microspheres prepared in the step four into the first mixture prepared in the step one, stirring for 1 hour, then adding 1 part by weight of curing agent, and stirring for 1 hour at the temperature of lower than 20 ℃ to obtain the conductive carbon adhesive.
In the first step, the epoxy resin is glycidyl ester epoxy resin, in the first step, the organic solvent is ethylene glycol diglycidyl ether, and in the fifth step, the curing agent is a photo-curing agent.
< example 2>
The invention provides a preparation method of conductive carbon adhesive, which comprises the following steps:
step one, uniformly mixing 100 parts by weight of epoxy resin, 4 parts by weight of dispersant and 5 parts by weight of organic solvent to obtain a first mixture with the viscosity of 1500 centipoises;
step two, taking 4 parts by weight of graphite powder with the particle size of less than 20 microns, putting the graphite powder into 100 parts by weight of concentrated sulfuric acid, adding 4 parts by weight of sodium nitrate and 8 parts by weight of potassium permanganate while stirring, controlling the reaction temperature to be lower than 25 ℃, stirring for 40min, then heating to 40 ℃, stirring for 50min, then adding 30 parts by weight of oxalic acid solution, and cooling to room temperature after the solution is bright yellow to obtain liquid A containing graphene oxide;
step three, adding 12 parts by weight of emulsifier and 25 parts by weight of dimethylbenzene into the liquid A in the step two, uniformly stirring, continuously adding 25 parts by weight of aniline monomer, uniformly mixing to obtain a second mixture, controlling the temperature of the second mixture to be below 3 ℃ by adopting an ice-water bath, then dropwise adding an ammonium persulfate solution with the concentration of 4mol/L at the speed of 8 seconds per drop, and stopping stirring until dark green appears to obtain a dispersion liquid;
step four, taking the dispersion liquid prepared in the step three, and obtaining microsphere powder in a spray drying mode, namely the graphene oxide-polyaniline composite microspheres;
and step five, adding the graphene oxide-polyaniline composite microspheres prepared in the step four into the first mixture prepared in the step one, stirring for 2 hours, then adding 2 parts by weight of curing agent, and stirring for 2 hours at the temperature of lower than 20 ℃ to obtain the conductive carbon adhesive.
In the first step, the epoxy resin is glycidyl ester epoxy resin, in the first step, the organic solvent is ethylene glycol diglycidyl ether, and in the fifth step, the curing agent is a photo-curing agent.
< example 3>
The invention provides a preparation method of conductive carbon adhesive, which comprises the following steps:
step one, uniformly mixing 100 parts by weight of epoxy resin, 5 parts by weight of dispersant and 10 parts by weight of organic solvent to obtain a first mixture with the viscosity of 2000 centipoises;
step two, taking 5 parts by weight of graphite powder with the particle size of less than 20 microns, putting the graphite powder into 100 parts by weight of concentrated sulfuric acid, adding 5 parts by weight of sodium nitrate and 10 parts by weight of potassium permanganate while stirring, controlling the reaction temperature to be lower than 25 ℃, stirring for 60min, then heating to 40 ℃, stirring for 60min, then adding 40 parts by weight of oxalic acid solution, and cooling to room temperature after the solution is bright yellow to obtain liquid A containing graphene oxide;
step three, adding 15 parts by weight of emulsifier and 30 parts by weight of dimethylbenzene into the liquid A in the step two, uniformly stirring, continuously adding 30 parts by weight of aniline monomer, uniformly mixing to obtain a second mixture, controlling the temperature of the second mixture to be below 3 ℃ by adopting an ice-water bath, then dropwise adding an ammonium persulfate solution with the concentration of 4mol/L at the speed of 10 seconds per drop, and stopping stirring until dark green appears to obtain a dispersion liquid;
step four, taking the dispersion liquid prepared in the step three, and obtaining microsphere powder in a spray drying mode, namely the graphene oxide-polyaniline composite microspheres;
and step five, adding the graphene oxide-polyaniline composite microspheres prepared in the step four into the first mixture prepared in the step one, stirring for 2 hours, then adding 2 parts by weight of curing agent, and stirring for 2 hours at the temperature of lower than 20 ℃ to obtain the conductive carbon adhesive.
In the first step, the epoxy resin is glycidyl ester epoxy resin, in the first step, the organic solvent is ethylene glycol diglycidyl ether, and in the fifth step, the curing agent is a photo-curing agent.
< comparative example 1>
The graphene oxide liquid a in example 2 was replaced with carbon nanotubes, and the remaining components, preparation processes, and parameters were the same as those in example 2.
< comparative example 2>
The graphene oxide liquid a in example 2 was replaced with graphene, and the remaining components, preparation processes, and parameters were the same as those in example 2.
< comparative example 3>
And adding 60 parts by weight of nano silver powder into 100 parts by weight of epoxy resin to prepare the conductive adhesive.
The resistivity of the conductive pastes prepared in examples 1 to 3 and comparative examples 1 to 3 was measured as shown in table 1 below.
TABLE 1
Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
Resistivity (omega cm) | 6.96×10-4 | 7.11×10-4 | 7.03×10-4 | 9.54×10-5 | 8.37×10-5 | 7.02×10-4 |
As can be seen from table 1, the conductive carbon paste prepared by the present invention has comparable conductivity to conductive paste containing metal filler. Meanwhile, compared with the conductive adhesive filled with carbon materials such as carbon nano tubes, graphene and the like, the initial raw material graphite powder of the composite microspheres has obvious cost advantage compared with the carbon nano tubes, expensive reducing agents are not needed to reduce graphene oxide into graphene, and meanwhile, polyaniline wrapped on the surface of the composite microspheres has better compatibility with epoxy resin, so that the finally prepared conductive carbon adhesive has high conductivity.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (6)
1. The preparation method of the conductive carbon adhesive is characterized by comprising the following steps:
step one, uniformly mixing 100 parts by weight of epoxy resin, 3-5 parts by weight of dispersant and 1-10 parts by weight of organic solvent to obtain a first mixture with the viscosity of 500-2000 centipoises;
step two, putting 2-5 parts by weight of graphite powder with the particle size of less than 20 mu m into 100 parts by weight of concentrated sulfuric acid, adding 2-5 parts by weight of sodium nitrate and 5-10 parts by weight of potassium permanganate while stirring, controlling the reaction temperature to be lower than 25 ℃, stirring for 30-60min, then heating to 40 ℃, stirring for 40-60min, then adding 20-40 parts by weight of oxalic acid solution, and cooling to room temperature after the solution is bright yellow to obtain liquid A containing graphene oxide;
step three, adding 10-15 parts by weight of emulsifier and 20-30 parts by weight of dimethylbenzene into the liquid A in the step two, uniformly stirring, continuously adding 20-30 parts by weight of aniline monomer, uniformly mixing to obtain a second mixture, controlling the temperature of the second mixture below 3 ℃ by adopting an ice water bath, then dropwise adding an ammonium persulfate solution with the concentration of 3-4mol/L at the speed of 5-10 seconds per drop, and stopping stirring until a dark green color appears to obtain a dispersion liquid;
step four, taking the dispersion liquid prepared in the step three, and obtaining microsphere powder in a spray drying mode, namely the graphene oxide-polyaniline composite microspheres;
and step five, adding the graphene oxide-polyaniline composite microspheres prepared in the step four into the first mixture prepared in the step one, stirring for 1-2 hours, then adding 1-2 parts by weight of a curing agent, and stirring for 1-2 hours at the temperature of 20 ℃ to obtain the conductive carbon adhesive.
2. The method for preparing a conductive carbon paste according to claim 1, wherein in the first step, the epoxy resin is one or more of glycidyl ester epoxy resin, alicyclic epoxy resin and aliphatic epoxy resin.
3. The method for preparing a conductive carbon adhesive according to claim 1, wherein the organic solvent in the first step is one or more of ethylene glycol diglycidyl ether, polypropylene glycol diglycidyl ether, absolute ethyl alcohol, and C12-14 fatty glycidyl ether.
4. The method for preparing a conductive carbon adhesive according to claim 1, wherein the curing agent in the fifth step is a photo-curing type curing agent or a latent curing agent.
5. A conductive carbon paste produced by the method for producing a conductive carbon paste according to any one of claims 1 to 4.
6. The use of the conductive carbon paste of claim 1 in thin film transistors, electromagnetic shielding devices.
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Citations (6)
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---|---|---|---|---|
CN102391508A (en) * | 2011-08-30 | 2012-03-28 | 上海大学 | Graphene oxide composite material for flexible electrode and preparation method thereof |
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CN104861651A (en) * | 2015-03-27 | 2015-08-26 | 华东理工大学 | Preparation method of modified graphene oxide and polyimide in-situ grafting composite material |
CN105254875A (en) * | 2015-11-20 | 2016-01-20 | 华东交通大学 | Preparation method of N-substituted carboxylic acid polyaniline covalently grafted graphene composite material |
CN105860064A (en) * | 2016-06-17 | 2016-08-17 | 西北师范大学 | Preparation method of polyaniline/carboxylated graphene composite material |
CN110734727A (en) * | 2018-10-23 | 2020-01-31 | 嘉兴学院 | Preparation method of conductive adhesive of polyaniline modified flaky carbon powder |
-
2020
- 2020-04-15 CN CN202010295773.2A patent/CN111334230A/en active Pending
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CN102391508A (en) * | 2011-08-30 | 2012-03-28 | 上海大学 | Graphene oxide composite material for flexible electrode and preparation method thereof |
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CN104861651A (en) * | 2015-03-27 | 2015-08-26 | 华东理工大学 | Preparation method of modified graphene oxide and polyimide in-situ grafting composite material |
CN105254875A (en) * | 2015-11-20 | 2016-01-20 | 华东交通大学 | Preparation method of N-substituted carboxylic acid polyaniline covalently grafted graphene composite material |
CN105860064A (en) * | 2016-06-17 | 2016-08-17 | 西北师范大学 | Preparation method of polyaniline/carboxylated graphene composite material |
CN110734727A (en) * | 2018-10-23 | 2020-01-31 | 嘉兴学院 | Preparation method of conductive adhesive of polyaniline modified flaky carbon powder |
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