CN107240438A - A kind of graphene electronic conduction slurry and automatic production process - Google Patents

A kind of graphene electronic conduction slurry and automatic production process Download PDF

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Publication number
CN107240438A
CN107240438A CN201710534047.XA CN201710534047A CN107240438A CN 107240438 A CN107240438 A CN 107240438A CN 201710534047 A CN201710534047 A CN 201710534047A CN 107240438 A CN107240438 A CN 107240438A
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China
Prior art keywords
parts
slurry
electronic conduction
dispersant
organic solvent
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CN201710534047.XA
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Chinese (zh)
Inventor
祝德光
祝楠
迟玲
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Qingdao Henglide Graphite Co Ltd
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Qingdao Henglide Graphite Co Ltd
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Priority to CN201710534047.XA priority Critical patent/CN107240438A/en
Publication of CN107240438A publication Critical patent/CN107240438A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20Conductive material dispersed in non-conductive organic material
    • H01B1/24Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Conductive Materials (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a kind of graphene electronic conduction slurry and automatic production process, electrocondution slurry component includes 8 20 parts of 40 60 parts of nano-graphite particle, 8 15 parts of epoxy resin, 5 10 parts of dispersant, 10 15 parts of silane coupler, 10 20 parts of organic solvent and deionized water by weight, preparation technology of the present invention is simple, obtained electrocondution slurry has superior decay resistance, also there is excellent conduction, heat conductivility simultaneously, production efficiency is high.

Description

A kind of graphene electronic conduction slurry and automatic production process
Technical field
The present invention relates to electrocondution slurry preparing technical field, specially a kind of graphene electronic conduction slurry and automatic metaplasia Production. art.
Background technology
Electric slurry is different by purposes, is divided into dielectric paste, resistance slurry and conductor paste:It is divided into electronics by substrate species Slurry ceramic substrate, polymer matrix film, glass substrate and metal-insulator substrate electric slurry etc.;It is different by sintering temperature, it can divide For high temperature, in gentle low temperature drying electric slurry;It is different by purposes, universal electric slurry can be divided into and (make general thick film Circuit) and special electronic slurry (stainless steel substrate electric slurry, Thermistor);It is divided into noble metal by the price of conductive phase Electric slurry (silver-colored palladium, ruthenium system and gold paste etc.) and base metal electric slurry (molybdenum manganese slurry).
Graphite is the important mineral resources of China, has and constantly researches and develops and the space lifted and development, in conductive field Its important effect is played, current graphite is to replace the conductive materials such as copper and iron, the conductive new material as a new generation uses graphite Not only technique is simple for the black lead wash of development, and environmental protection more has efficient conducting function, accelerates productivity ratio, improves the matter of industry Amount, quality guarantee is a very promising environmental-friendly natural material, has obtained consistent favorable comment and the trust of professional.It is existing Obtained electric slurry conduction, heat conductivility are poor in technology, cause electronic device service life short.
The content of the invention
It is above-mentioned to solve it is an object of the invention to provide a kind of graphene electronic conduction slurry and automatic production process The problem of being proposed in background technology.
To achieve the above object, the present invention provides following technical scheme:A kind of graphene electronic conduction slurry, electrocondution slurry Component includes 40-60 parts of nano-graphite particle, 8-15 parts of epoxy resin, 5-10 parts of dispersant, silane coupler by weight 8-20 parts of 10-15 parts, 10-20 parts of organic solvent and deionized water.
It is preferred that, the preferred component proportioning of electrocondution slurry is:50 parts of nano-graphite particle, 12 parts of epoxy resin, dispersant 8 Part, 12 parts of silane coupler, 15 parts of organic solvent and 14 parts of deionized water.
It is preferred that, the dispersant is by 20% polyvinyl alcohol, 20% polyethylene glycol, 30% butadiene-styrene rubber, 20% carboxymethyl cellulose Plain sodium, 5% cetyl ammonium bromide, 5% dodecyl sodium sulfate mixture composition.
It is preferred that, the organic solvent uses isopropanol, methyl methacrylate and butyl acetate mixture.
It is preferred that, its production technology comprises the following steps:
A, nano-graphite particle, epoxy resin, dispersant, organic solvent added into the double dimension grinders grindings of rod nail type after mixing, Mixed slurry A is obtained after grinding a period of time;
B, addition silane coupler and deionized water in mixed slurry A, add in heating tank after mixing and heat, in heating process Nitrogen is constantly passed through, nitrogen flow is 50-100ml/min, and heating-up temperature is 60 DEG C -80 DEG C, slow cold after constant temperature 30min afterwards But to room temperature, mixed slurry B is obtained;
C, will in mixed slurry B add ultrasonic machine in carry out ultrasonic vibration, 1h-2h is stood afterwards;
D, the mixed slurry for finally obtaining step C add stirring ball mill and carry out ball-milling treatment;Pass through pipeline-type emulsifying machine Mechanical damage processing is carried out, electrocondution slurry is finally given.
It is preferred that, ultrasonic acc power is 500-1500W in the step C, and ultrasonic time is 20min-40min.
Compared with prior art, the beneficial effects of the invention are as follows:Preparation technology of the present invention is simple, and production cost is low, without dirt Dye, obtained electrocondution slurry has superior decay resistance, while also having excellent conduction, heat conductivility, production efficiency It is high;Using the electronic device of electrocondution slurry formation, particularly energy storage device, the electric product of such as lithium has excellent conductive, heat conduction Performance, and the performance such as its power density, rate capability, tap density, cyclical stability, service life is also greatly improved;This Outside, in production technology of the present invention, nitrogen protection is constantly passed through in heating process, effectively can prevent graphite material from aoxidizing, Influence electrocondution slurry performance.
Embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment Only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area The every other embodiment that art personnel are obtained under the premise of creative work is not made, belongs to the model that the present invention is protected Enclose.
The present invention provides following technical scheme:A kind of graphene electronic conduction slurry, electrocondution slurry component is by weight Including 40-60 parts of nano-graphite particle, 8-15 parts of epoxy resin, 5-10 parts of dispersant, 10-15 parts of silane coupler, You Jirong 8-20 parts of 10-20 parts of agent and deionized water;Wherein, dispersant by 20% polyvinyl alcohol, 20% polyethylene glycol, 30% butadiene-styrene rubber, 20% sodium carboxymethylcellulose, 5% cetyl ammonium bromide, 5% dodecyl sodium sulfate mixture composition;Organic solvent is using different Propyl alcohol, methyl methacrylate and butyl acetate mixture.
Embodiment one:
Electrocondution slurry component includes 40 parts of nano-graphite particle by weight, 8 parts of epoxy resin, 5 parts of dispersant, silane coupled 8 parts of 10 parts of agent, 10 parts of organic solvent and deionized water.
The production technology of the present embodiment comprises the following steps:
A, nano-graphite particle, epoxy resin, dispersant, organic solvent added into the double dimension grinders grindings of rod nail type after mixing, Mixed slurry A is obtained after grinding a period of time;
B, addition silane coupler and deionized water in mixed slurry A, add in heating tank after mixing and heat, in heating process Nitrogen is constantly passed through, nitrogen flow is 50ml/min, and heating-up temperature is 60 DEG C, is slowly cooled to room temperature afterwards after constant temperature 30min, Obtain mixed slurry B;
C, will in mixed slurry B add ultrasonic machine in carry out ultrasonic vibration, 1h is stood afterwards;
D, the mixed slurry for finally obtaining step C add stirring ball mill and carry out ball-milling treatment;Pass through pipeline-type emulsifying machine Mechanical damage processing is carried out, electrocondution slurry is finally given.
In the present embodiment, ultrasonic acc power is 500W in step C, and ultrasonic time is 20min.
Embodiment two:
It is even that electrocondution slurry component includes 60 parts of nano-graphite particle, 15 parts of epoxy resin, 10 parts of dispersant, silane by weight Join 20 parts of 15 parts of agent, 20 parts of organic solvent and deionized water.
The production technology of the present embodiment comprises the following steps:
A, nano-graphite particle, epoxy resin, dispersant, organic solvent added into the double dimension grinders grindings of rod nail type after mixing, Mixed slurry A is obtained after grinding a period of time;
B, addition silane coupler and deionized water in mixed slurry A, add in heating tank after mixing and heat, in heating process Nitrogen is constantly passed through, nitrogen flow is 100ml/min, and heating-up temperature is 80 DEG C, slowly cools to room after constant temperature 30min afterwards Temperature, obtains mixed slurry B;
C, will in mixed slurry B add ultrasonic machine in carry out ultrasonic vibration, 2h is stood afterwards;
D, the mixed slurry for finally obtaining step C add stirring ball mill and carry out ball-milling treatment;Pass through pipeline-type emulsifying machine Mechanical damage processing is carried out, electrocondution slurry is finally given.
In the present embodiment, ultrasonic acc power is 1500W in step C, and ultrasonic time is 40min.
Embodiment three:
It is even that electrocondution slurry component includes 45 parts of nano-graphite particle, 10 parts of epoxy resin, 6 parts of dispersant, silane by weight Join 10 parts of 11 parts of agent, 12 parts of organic solvent and deionized water.
The production technology of the present embodiment comprises the following steps:
A, nano-graphite particle, epoxy resin, dispersant, organic solvent added into the double dimension grinders grindings of rod nail type after mixing, Mixed slurry A is obtained after grinding a period of time;
B, addition silane coupler and deionized water in mixed slurry A, add in heating tank after mixing and heat, in heating process Nitrogen is constantly passed through, nitrogen flow is 60ml/min, and heating-up temperature is 65 DEG C, is slowly cooled to room temperature afterwards after constant temperature 30min, Obtain mixed slurry B;
C, will in mixed slurry B add ultrasonic machine in carry out ultrasonic vibration, 1.2h is stood afterwards;
D, the mixed slurry for finally obtaining step C add stirring ball mill and carry out ball-milling treatment;Pass through pipeline-type emulsifying machine Mechanical damage processing is carried out, electrocondution slurry is finally given.
In the present embodiment, ultrasonic acc power is 600W in step C, and ultrasonic time is 25min.
Example IV:
It is even that electrocondution slurry component includes 55 parts of nano-graphite particle, 13 parts of epoxy resin, 8 parts of dispersant, silane by weight Join 18 parts of 14 parts of agent, 18 parts of organic solvent and deionized water.
The production technology of the present embodiment comprises the following steps:
A, nano-graphite particle, epoxy resin, dispersant, organic solvent added into the double dimension grinders grindings of rod nail type after mixing, Mixed slurry A is obtained after grinding a period of time;
B, addition silane coupler and deionized water in mixed slurry A, add in heating tank after mixing and heat, in heating process Nitrogen is constantly passed through, nitrogen flow is 90ml/min, and heating-up temperature is 75 DEG C, is slowly cooled to room temperature afterwards after constant temperature 30min, Obtain mixed slurry B;
C, will in mixed slurry B add ultrasonic machine in carry out ultrasonic vibration, 1.8h is stood afterwards;
D, the mixed slurry for finally obtaining step C add stirring ball mill and carry out ball-milling treatment;Pass through pipeline-type emulsifying machine Mechanical damage processing is carried out, electrocondution slurry is finally given.
In the present embodiment, ultrasonic acc power is 1300W in step C, and ultrasonic time is 35min.
Embodiment five:
It is even that electrocondution slurry component includes 48 parts of nano-graphite particle, 12 parts of epoxy resin, 8 parts of dispersant, silane by weight Join 15 parts of 12 parts of agent, 16 parts of organic solvent and deionized water.
The production technology of the present embodiment comprises the following steps:
A, nano-graphite particle, epoxy resin, dispersant, organic solvent added into the double dimension grinders grindings of rod nail type after mixing, Mixed slurry A is obtained after grinding a period of time;
B, addition silane coupler and deionized water in mixed slurry A, add in heating tank after mixing and heat, in heating process Nitrogen is constantly passed through, nitrogen flow is 70ml/min, and heating-up temperature is 68 DEG C, is slowly cooled to room temperature afterwards after constant temperature 30min, Obtain mixed slurry B;
C, will in mixed slurry B add ultrasonic machine in carry out ultrasonic vibration, 1.3h is stood afterwards;
D, the mixed slurry for finally obtaining step C add stirring ball mill and carry out ball-milling treatment;Pass through pipeline-type emulsifying machine Mechanical damage processing is carried out, electrocondution slurry is finally given.
In the present embodiment, ultrasonic acc power is 1200W in step C, and ultrasonic time is 38min.
Embodiment six:
It is even that electrocondution slurry component includes 50 parts of nano-graphite particle, 12 parts of epoxy resin, 8 parts of dispersant, silane by weight Join 14 parts of 12 parts of agent, 15 parts of organic solvent and deionized water.
The production technology of the present embodiment comprises the following steps:
A, nano-graphite particle, epoxy resin, dispersant, organic solvent added into the double dimension grinders grindings of rod nail type after mixing, Mixed slurry A is obtained after grinding a period of time;
B, addition silane coupler and deionized water in mixed slurry A, add in heating tank after mixing and heat, in heating process Nitrogen is constantly passed through, nitrogen flow is 75ml/min, and heating-up temperature is 70 DEG C, is slowly cooled to room temperature afterwards after constant temperature 30min, Obtain mixed slurry B;
C, will in mixed slurry B add ultrasonic machine in carry out ultrasonic vibration, 1.5h is stood afterwards;
D, the mixed slurry for finally obtaining step C add stirring ball mill and carry out ball-milling treatment;Pass through pipeline-type emulsifying machine Mechanical damage processing is carried out, electrocondution slurry is finally given.
In the present embodiment, ultrasonic acc power is 1000W in step C, and ultrasonic time is 30min.
Experimental example:
Electrical conductivity and viscosity are carried out with electrocondution slurry made from conventional method using electrocondution slurry made from various embodiments of the present invention Experiment, obtains data such as following table:
From above table data, electrocondution slurry can reach optimum performance made from embodiment six.
Preparation technology of the present invention is simple, and production cost is low, pollution-free, and obtained electrocondution slurry has superior corrosion resistance Can, while also having excellent conduction, heat conductivility, production efficiency is high;The electronic device formed using the electrocondution slurry, especially Energy storage device, the electric product of such as lithium has excellent conductive, a heat conductivility, and its power density, rate capability, tap density, The performances such as cyclical stability, service life are also greatly improved;In addition, in production technology of the present invention, in heating process constantly Nitrogen protection is passed through, effectively can prevent graphite material from aoxidizing, electrocondution slurry performance is influenceed.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding And modification, the scope of the present invention is defined by the appended.

Claims (6)

1. a kind of graphene electronic conduction slurry, it is characterised in that:Electrocondution slurry component includes nano-graphite grain by weight Sub- 40-60 parts, 8-15 parts of epoxy resin, 5-10 parts of dispersant, 10-15 parts of silane coupler, 10-20 parts of organic solvent and go 8-20 parts of ionized water.
2. a kind of graphene electronic conduction slurry according to claim 1, it is characterised in that:The preferred component of electrocondution slurry Match and be:50 parts of nano-graphite particle, 12 parts of epoxy resin, 8 parts of dispersant, 12 parts of silane coupler, 15 parts of organic solvent with And 14 parts of deionized water.
3. a kind of graphene electronic conduction slurry according to claim 1, it is characterised in that:The dispersant is gathered by 20% Vinyl alcohol, 20% polyethylene glycol, 30% butadiene-styrene rubber, 20% sodium carboxymethylcellulose, 5% cetyl ammonium bromide, 5% dodecyl Azochlorosulfonate acid sodium mixture is constituted.
4. a kind of graphene electronic conduction slurry according to claim 1, it is characterised in that:The organic solvent is using different Propyl alcohol, methyl methacrylate and butyl acetate mixture.
5. realize a kind of production technology of graphene electronic conduction slurry described in claim 1, it is characterised in that:It produces work Skill comprises the following steps:
A, nano-graphite particle, epoxy resin, dispersant, organic solvent added into the double dimension grinders grindings of rod nail type after mixing, Mixed slurry A is obtained after grinding a period of time;
B, addition silane coupler and deionized water in mixed slurry A, add in heating tank after mixing and heat, in heating process Nitrogen is constantly passed through, nitrogen flow is 50-100ml/min, and heating-up temperature is 60 DEG C -80 DEG C, slow cold after constant temperature 30min afterwards But to room temperature, mixed slurry B is obtained;
C, will in mixed slurry B add ultrasonic machine in carry out ultrasonic vibration, 1h-2h is stood afterwards;
D, the mixed slurry for finally obtaining step C add stirring ball mill and carry out ball-milling treatment;Pass through pipeline-type emulsifying machine Mechanical damage processing is carried out, electrocondution slurry is finally given.
6. a kind of production technology of graphene electronic conduction slurry according to claim 5, it is characterised in that:The step Ultrasonic acc power is 500-1500W in C, and ultrasonic time is 20min-40min.
CN201710534047.XA 2017-07-03 2017-07-03 A kind of graphene electronic conduction slurry and automatic production process Pending CN107240438A (en)

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Application Number Priority Date Filing Date Title
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102254584A (en) * 2011-05-12 2011-11-23 中国科学院宁波材料技术与工程研究所 General electronic paste based on graphene filler
CN104966837A (en) * 2015-04-24 2015-10-07 深圳市德方纳米科技股份有限公司 Graphene conductive liquid as well as preparation method and application thereof
CN106141499A (en) * 2016-08-05 2016-11-23 雷春生 A kind of grounding grid heat release welding preparation method of ultra-fine welding powder
CN106893012A (en) * 2017-04-17 2017-06-27 山东本源晶体科技有限公司 A kind of Nano Silver modified graphene crystal composite material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102254584A (en) * 2011-05-12 2011-11-23 中国科学院宁波材料技术与工程研究所 General electronic paste based on graphene filler
CN104966837A (en) * 2015-04-24 2015-10-07 深圳市德方纳米科技股份有限公司 Graphene conductive liquid as well as preparation method and application thereof
CN106141499A (en) * 2016-08-05 2016-11-23 雷春生 A kind of grounding grid heat release welding preparation method of ultra-fine welding powder
CN106893012A (en) * 2017-04-17 2017-06-27 山东本源晶体科技有限公司 A kind of Nano Silver modified graphene crystal composite material and preparation method thereof

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Application publication date: 20171010