CN108877990A - A kind of graphene nano conductive silver slurry and preparation method thereof - Google Patents
A kind of graphene nano conductive silver slurry and preparation method thereof Download PDFInfo
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- CN108877990A CN108877990A CN201810505232.0A CN201810505232A CN108877990A CN 108877990 A CN108877990 A CN 108877990A CN 201810505232 A CN201810505232 A CN 201810505232A CN 108877990 A CN108877990 A CN 108877990A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/10—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material voltage responsive, i.e. varistors
- H01C7/105—Varistor cores
- H01C7/108—Metal oxide
- H01C7/112—ZnO type
Abstract
The invention belongs to electrocondution slurry fields, and in particular to a kind of graphene nano conductive silver slurry and preparation method thereof.Including following content of component：30-40 parts of graphene, 20-40 parts of nano silver, 33-60 parts of organic solvent, 8-15 parts, 15~25 parts triethanolamines of epoxy resin, 10-15 parts of dispersing agent, 1-5 parts of indium oxide, 1-6 parts of ferroso-ferric oxide, 1-3 parts of tin indium oxide, 3-6 parts of zinc oxide, 4-7 parts of butyl carbitol acetate, 5-12 parts of binder and 30-60 parts of deionized water.Material composition of the invention is simple, preparation process is simple, reduces the dosage of silver, greatly reduces production cost；And slurry uniformity produced by the present invention, dispersion are sufficiently.
Description
Technical field
The invention belongs to electrocondution slurry fields, and in particular to a kind of graphene nano conductive silver slurry and preparation method thereof.
Background technique
Electrocondution slurry, cloth, encapsulation, the connection etc. being widely used in microelectronics industry, the miniaturization to microelectronic component
Play important use.The conductive phase of electric slurry is mostly based on the noble metal powders such as platinum, palladium, gold and silver, and silver-colored price is relatively
It is low, so the commercialized degree highest of silver paste.Silver-colored price was higher and higher in recent years, and the production cost of silver paste also increases therewith
Add, in addition silver ion migration problem existing for silver paste itself.
Graphene (Graphene) is the only one layer of atomic thickness for being stripped out from graphite material, being made of carbon atom
Two dimensional crystal, the bidimensional period honeycomb lattice structure that it is made of carbon hexatomic ring can be warped into the fullerene of zero dimension
(fullerene), it is rolled into one-dimensional carbon nanotube (carbon nano-tube, CNT) or is stacked to three-dimensional graphite
(graphite), ideal graphene-structured is plane hexagonal lattice, can be regarded as one layer of graphitic molecules being stripped, often
A carbon atom is sp2 hydridization, and contributes and electronically form big pi bond on a remaining p track, and pi-electron can move freely, and assign
Give the good electric conductivity of graphene.But there is difficult dispersion as slurry in graphene, the problem of easily unity.
Notification number is that the patent of invention of 103500812B discloses a kind of preparation of doped graphene preparation high-conductivity slurry
Method is stirred by the way that the electrocondution slurry of different quality part, graphene, dispersing agent, deionized water are put into de-airing mixer in batches
It mixes, finally obtains doped graphene preparation high-conductivity slurry, this method simple process, but the graphene in the preparation method is deposited
In dispersion and agglomeration traits, poor dispersion causes graphene to be reunited.The patent of invention of Publication No. CN106469582A discloses
A kind of electrocondution slurry of containing graphene and preparation method thereof, the patent of invention starch graphene with dispersing agent and shear
Material carries out decentralized processing, but the dispersibility of the resulting graphene of the invention is not good enough, and cost of material is high, is not suitable for industry
Metaplasia produces.
Summary of the invention
For the deficiencies in the prior art, the present invention provides a kind of material for zinc oxide varistor preparation
And preparation method thereof, the resulting material property for zinc oxide varistor preparation of the invention preparation method is excellent, and this
Toxic Element Lead is free of in invention, it is environmentally protective, and during the preparation process, energy consumption is small, meets energy-saving and environment-friendly requirement.
In order to achieve the above-mentioned object of the invention, the invention adopts the following technical scheme：
A kind of graphene nano conductive silver slurry, including following content of component：30-40 parts of graphene, nano silver 20-40
Part, 33-60 parts of organic solvent, 8-15 parts, 15~25 parts triethanolamines of epoxy resin, 10-15 parts of dispersing agent, 1-5 parts of indium oxide,
1-6 parts of ferroso-ferric oxide, 1-3 parts of tin indium oxide, 3-6 parts of zinc oxide, 4-7 parts of butyl carbitol acetate, 5-12 parts of binder
With 30-60 parts of deionized water.
Preferably, the graphene nano conductive silver slurry includes following content of component：38 parts of graphene, nano silver
32 parts, 44 parts of organic solvent, 7 parts, 22 parts triethanolamines of epoxy resin, 13 parts of dispersing agent, 3 parts of indium oxide, ferroso-ferric oxide 4
Part, 2 parts of tin indium oxide, 5 parts of zinc oxide, 6 parts of butyl carbitol acetate, 11 parts of binder and 55 parts of deionized water.
Preferably, the nano silver is 60-100 nanometers.
A kind of preparation method of graphene nano conductive silver slurry, includes the following steps：Step 1, raw material is weighed；Step 2,
Graphene, nano silver and deionized water are put into grinding distribution in colloid mill after mixing and obtain dispersion liquid, it later will dispersion
Liquid is sent into cooling in material barrel；Step 3, it cools down and dispersion liquid is transported to homogenization in high pressure homogenizer, homogenization 3 times,
20-30 minutes every time；Step 4, toward will in the dispersion liquid after homogenization be added organic solvent, epoxy resin, triethanolamine, point
Powder, indium oxide, ferroso-ferric oxide, tin indium oxide, zinc oxide and butyl carbitol acetate are ultrasonically treated 40-50 minutes, add
Enter binder, obtains graphene nano conductive silver slurry.
Preferably, the ultrasonic treatment frequency is 22000-25000 hertz.
Compared with prior art, the invention has the advantages that：
Material composition of the invention is simple, preparation process is simple, reduces the dosage of silver, greatly reduces production cost；
And slurry uniformity produced by the present invention, dispersion are sufficiently.
Specific embodiment
Below by specific embodiment, invention is further described in detail.But those skilled in the art will manage
Solution, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Specific skill is not specified in embodiment
Art or condition person, described technology or conditions carry out to specifications according to the literature in the art.Agents useful for same or instrument
Production firm person is not specified, being can be with conventional products that are commercially available.
Embodiment 1
A kind of graphene nano conductive silver slurry, including following content of component：30 parts of graphene, has 20 parts of nano silver
33 parts of solvent, 8 parts of epoxy resin, 15 parts of triethanolamine, 10 parts of dispersing agent, 1 part of indium oxide, 1 part of ferroso-ferric oxide, indium oxide
1 part of tin, 3 parts of zinc oxide, 4 parts of butyl carbitol acetate, 5 parts of binder and 30 parts of deionized water.
The nano silver is 100 nanometers.
A kind of preparation method of graphene nano conductive silver slurry, includes the following steps：Step 1, raw material is weighed；Step 2,
Graphene, nano silver and deionized water are put into grinding distribution in colloid mill after mixing and obtain dispersion liquid, it later will dispersion
Liquid is sent into cooling in material barrel；Step 3, it cools down and dispersion liquid is transported to homogenization in high pressure homogenizer, homogenization 3 times,
20 minutes every time；Step 4, toward will in the dispersion liquid after homogenization be added organic solvent, epoxy resin, triethanolamine, dispersion
Agent, indium oxide, ferroso-ferric oxide, tin indium oxide, zinc oxide and butyl carbitol acetate are ultrasonically treated 40 minutes, are added viscous
Agent is tied, graphene nano conductive silver slurry is obtained.
The ultrasonic treatment frequency is 22000 hertz.
Embodiment 2
A kind of graphene nano conductive silver slurry, including following content of component：40 parts of graphene, has 40 parts of nano silver
60 parts of solvent, 15 parts of epoxy resin, 25 parts of triethanolamine, 15 parts of dispersing agent, 5 parts of indium oxide, 6 parts of ferroso-ferric oxide, oxidation
3 parts of indium tin, 6 parts of zinc oxide, 7 parts of butyl carbitol acetate, 12 parts of binder and 60 parts of deionized water.
The nano silver is 80 nanometers.
A kind of preparation method of graphene nano conductive silver slurry, includes the following steps：Step 1, raw material is weighed；Step 2,
Graphene, nano silver and deionized water are put into grinding distribution in colloid mill after mixing and obtain dispersion liquid, it later will dispersion
Liquid is sent into cooling in material barrel；Step 3, it cools down and dispersion liquid is transported to homogenization in high pressure homogenizer, homogenization 3 times,
30 minutes every time；Step 4, toward will in the dispersion liquid after homogenization be added organic solvent, epoxy resin, triethanolamine, dispersion
Agent, indium oxide, ferroso-ferric oxide, tin indium oxide, zinc oxide and butyl carbitol acetate are ultrasonically treated 50 minutes, are added viscous
Agent is tied, graphene nano conductive silver slurry is obtained.
The ultrasonic treatment frequency is 25000 hertz.
Embodiment 3
A kind of graphene nano conductive silver slurry, including following content of component：38 parts of graphene, has 32 parts of nano silver
44 parts of solvent, 7 parts of epoxy resin, 22 parts of triethanolamine, 13 parts of dispersing agent, 3 parts of indium oxide, 4 parts of ferroso-ferric oxide, indium oxide
2 parts of tin, 5 parts of zinc oxide, 6 parts of butyl carbitol acetate, 11 parts of binder and 55 parts of deionized water.
The nano silver is 60 nanometers.
A kind of preparation method of graphene nano conductive silver slurry, includes the following steps：Step 1, raw material is weighed；Step 2,
Graphene, nano silver and deionized water are put into grinding distribution in colloid mill after mixing and obtain dispersion liquid, it later will dispersion
Liquid is sent into cooling in material barrel；Step 3, it cools down and dispersion liquid is transported to homogenization in high pressure homogenizer, homogenization 3 times,
28 minutes every time；Step 4, toward will in the dispersion liquid after homogenization be added organic solvent, epoxy resin, triethanolamine, dispersion
Agent, indium oxide, ferroso-ferric oxide, tin indium oxide, zinc oxide and butyl carbitol acetate are ultrasonically treated 48 minutes, are added viscous
Agent is tied, graphene nano conductive silver slurry is obtained.
The ultrasonic treatment frequency is 24000 hertz.
Comparative example 1
Step is with embodiment 1, the difference is that being not added with nano silver.
A kind of graphene nano conductive silver slurry, including following content of component：30 parts of graphene, 33 parts of organic solvent,
8 parts of epoxy resin, 15 parts of triethanolamine, 10 parts of dispersing agent, 1 part of indium oxide, 1 part of ferroso-ferric oxide, 1 part of tin indium oxide, oxidation
3 parts of zinc, 4 parts of butyl carbitol acetate, 5 parts of binder and 30 parts of deionized water.
A kind of preparation method of graphene nano conductive silver slurry, includes the following steps：Step 1, raw material is weighed；Step 2,
Graphene and deionized water are put into grinding distribution in colloid mill after mixing and obtain dispersion liquid, dispersion liquid is sent into object later
It is cooling in charging basket；Step 3, it cools down and dispersion liquid is transported to homogenization in high pressure homogenizer, homogenization 3 times, every time 20 points
Clock；Step 4, toward will in the dispersion liquid after homogenization be added organic solvent, epoxy resin, triethanolamine, dispersing agent, oxidation
Indium, ferroso-ferric oxide, tin indium oxide, zinc oxide and butyl carbitol acetate are ultrasonically treated 40 minutes, and binder is added, obtains
To graphene conductive slurry.
The ultrasonic treatment frequency is 22000 hertz.
Comparative example 2
Step is with embodiment 2, the difference is that homogenization 1 time.
A kind of graphene nano conductive silver slurry, including following content of component：40 parts of graphene, has 40 parts of nano silver
60 parts of solvent, 15 parts of epoxy resin, 25 parts of triethanolamine, 15 parts of dispersing agent, 5 parts of indium oxide, 6 parts of ferroso-ferric oxide, oxidation
3 parts of indium tin, 6 parts of zinc oxide, 7 parts of butyl carbitol acetate, 12 parts of binder and 60 parts of deionized water.
The nano silver is 80 nanometers.
A kind of preparation method of graphene nano conductive silver slurry, includes the following steps：Step 1, raw material is weighed；Step 2,
Graphene, nano silver and deionized water are put into grinding distribution in colloid mill after mixing and obtain dispersion liquid, it later will dispersion
Liquid is sent into cooling in material barrel；Step 3, it cools down and dispersion liquid is transported to homogenization in high pressure homogenizer, homogenization 1 time,
The processing time 30 minutes；Step 4, toward will in the dispersion liquid after homogenization be added organic solvent, epoxy resin, triethanolamine,
Dispersing agent, indium oxide, ferroso-ferric oxide, tin indium oxide, zinc oxide and butyl carbitol acetate are ultrasonically treated 50 minutes, add
Enter binder, obtains graphene nano conductive silver slurry.
The ultrasonic treatment frequency is 25000 hertz.
Comparative example 3
Step is with embodiment 3, the difference is that being not added with butyl carbitol acetate.
A kind of graphene nano conductive silver slurry, including following content of component：38 parts of graphene, has 32 parts of nano silver
44 parts of solvent, 7 parts of epoxy resin, 22 parts of triethanolamine, 13 parts of dispersing agent, 3 parts of indium oxide, 4 parts of ferroso-ferric oxide, indium oxide
2 parts of tin, 5 parts of zinc oxide, 11 parts of binder and 55 parts of deionized water.
The nano silver is 60 nanometers.
A kind of preparation method of graphene nano conductive silver slurry, includes the following steps：Step 1, raw material is weighed；Step 2,
Graphene, nano silver and deionized water are put into grinding distribution in colloid mill after mixing and obtain dispersion liquid, it later will dispersion
Liquid is sent into cooling in material barrel；Step 3, it cools down and dispersion liquid is transported to homogenization in high pressure homogenizer, homogenization 3 times,
28 minutes every time；Step 4, toward will in the dispersion liquid after homogenization be added organic solvent, epoxy resin, triethanolamine, dispersion
Agent, indium oxide, ferroso-ferric oxide, tin indium oxide and zinc oxide are ultrasonically treated 48 minutes, and binder is added, obtains graphene and receives
Rice conductive silver slurry.
The ultrasonic treatment frequency is 24000 hertz.
The resulting material for being used for zinc oxide varistor preparation of embodiment 1-3 and comparative example 1-3 is subjected to performance survey
Examination, acquired results are as shown in the table：
Table as above is visible：Material composition of the invention is simple, preparation process is simple, reduces the dosage of silver, substantially reduces
Production cost；And slurry uniformity produced by the present invention, dispersion are sufficiently.
The above is only preferred embodiments of the present invention, is not intended to limit the scope of the present invention,
Therefore any trickle amendment, equivalent variations and modification made to the above embodiment according to the technical essence of the invention, belong to
In the range of technical solution of the present invention.
Claims (5)
1. a kind of graphene nano conductive silver slurry, which is characterized in that including following content of component：30-40 parts of graphene is received
Rice 20-40 parts of silver, 33-60 parts of organic solvent, 8-15 parts, 15~25 parts triethanolamines of epoxy resin, 10-15 parts of dispersing agent, oxygen
Change indium 1-5 parts, 1-6 parts of ferroso-ferric oxide, 1-3 parts of tin indium oxide, 3-6 parts of zinc oxide, 4-7 parts of butyl carbitol acetate, glue
Agent 5-12 parts and deionized water 30-60 parts of knot.
2. a kind of graphene nano conductive silver slurry according to claim 1, which is characterized in that including following mass parts group
Point：38 parts of graphene, 32 parts of nano silver, 44 parts of organic solvent, 7 parts, 22 parts triethanolamines of epoxy resin, 13 parts of dispersing agent, oxygen
Change 3 parts of indium, 4 parts of ferroso-ferric oxide, 2 parts of tin indium oxide, 5 parts of zinc oxide, 6 parts of butyl carbitol acetate, 11 parts of binder and
55 parts of deionized water.
3. a kind of graphene nano conductive silver slurry according to claim 1, which is characterized in that the nano silver is 60-
100 nanometers.
4. a kind of preparation method of graphene nano conductive silver slurry described in claim 1, which is characterized in that including following step
Suddenly：Step 1, raw material is weighed；Step 2, graphene, nano silver and deionized water are put into grinding point in colloid mill after mixing
It dissipates and obtains dispersion liquid, be later sent into dispersion liquid cooling in material barrel；Step 3, it cools down and dispersion liquid is transported to high pressure homogenizer
Interior homogenization, it is homogenization 3 times, 20-30 minutes each；Step 4, organic molten toward will be added in the dispersion liquid after homogenization
Agent, epoxy resin, triethanolamine, dispersing agent, indium oxide, ferroso-ferric oxide, tin indium oxide, zinc oxide and butyl carbitol acetic acid
Ester is ultrasonically treated 40-50 minutes, and binder is added, obtains graphene nano conductive silver slurry.
5. a kind of preparation method of graphene nano conductive silver slurry according to claim 4, which is characterized in that described super
Acoustic treatment frequency is 22000-25000 hertz.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109688641A (en) * | 2019-01-17 | 2019-04-26 | 佛山市昂达电器有限公司 | Heater and preparation method thereof and exothermic material and electric heating towel rack |
| CN114603133A (en) * | 2022-04-02 | 2022-06-10 | 苏州博濬新材料科技有限公司 | Conductive silver paste containing multilevel-structure nano filler and preparation method thereof |
| CN116355540A (en) * | 2021-12-28 | 2023-06-30 | 阿特斯阳光电力集团股份有限公司 | POE packaging adhesive film and preparation method and application thereof |
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| CN104178053A (en) * | 2013-05-28 | 2014-12-03 | 北京中科纳通电子技术有限公司 | Graphene composite conductive adhesive |
| CN105255422A (en) * | 2015-11-17 | 2016-01-20 | 张建刚 | Electrically conductive and thermally conductive graphene slurry and preparation method thereof |
| CN106952675A (en) * | 2017-03-22 | 2017-07-14 | 西北大学 | Graphene-based organic carrier and preparation method thereof, electric slurry and preparation method thereof |
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| US20080241507A1 (en) * | 2007-03-30 | 2008-10-02 | Tsinghua University | Conductive tape and method for making the same |
| CN104178053A (en) * | 2013-05-28 | 2014-12-03 | 北京中科纳通电子技术有限公司 | Graphene composite conductive adhesive |
| CN105255422A (en) * | 2015-11-17 | 2016-01-20 | 张建刚 | Electrically conductive and thermally conductive graphene slurry and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109688641A (en) * | 2019-01-17 | 2019-04-26 | 佛山市昂达电器有限公司 | Heater and preparation method thereof and exothermic material and electric heating towel rack |
| CN116355540A (en) * | 2021-12-28 | 2023-06-30 | 阿特斯阳光电力集团股份有限公司 | POE packaging adhesive film and preparation method and application thereof |
| CN114603133A (en) * | 2022-04-02 | 2022-06-10 | 苏州博濬新材料科技有限公司 | Conductive silver paste containing multilevel-structure nano filler and preparation method thereof |
| CN114603133B (en) * | 2022-04-02 | 2024-04-12 | 苏州博濬新材料科技有限公司 | Conductive silver paste containing nano filler with multilevel structure and preparation method thereof |
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Application publication date: 20181123 |