CN110408267A - A kind of Graphene conductive ink and preparation method thereof - Google Patents

A kind of Graphene conductive ink and preparation method thereof Download PDF

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Publication number
CN110408267A
CN110408267A CN201910764706.8A CN201910764706A CN110408267A CN 110408267 A CN110408267 A CN 110408267A CN 201910764706 A CN201910764706 A CN 201910764706A CN 110408267 A CN110408267 A CN 110408267A
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graphene
parts
conductive ink
ink
graphene conductive
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CN201910764706.8A
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Inventor
冯岩
徐小芳
汤文龙
胡慧忠
陆海峰
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Tai Ning Environmental Protection Technology (zhejiang) Co Ltd
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Tai Ning Environmental Protection Technology (zhejiang) Co Ltd
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Priority to CN201910764706.8A priority Critical patent/CN110408267A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/52Electrically conductive inks

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)

Abstract

The invention discloses a kind of Graphene conductive inks, are made of the raw material for including following parts by weight: 80~100 parts of ink, 3~4.5 parts of graphene, 1.1~1.4 parts of levelling agent, 0.9~1.2 part of defoaming agent, 2.2~2.8 parts of dispersing agent, 12~18 parts of cosolvent;The graphene is nano-graphene microplate;The graphene with a thickness of 1~10nm.Graphene conductive ink of the invention is made up of selected raw material, and optimize each material content, ink, graphene, levelling agent, defoaming agent, dispersing agent and the cosolvent of appropriate proportion are selected, for Graphene conductive ink obtained compared with common conductive ink, Graphene conductive ink electric conductivity of the invention is obviously more preferable;Fastness to rubbing is higher.

Description

A kind of Graphene conductive ink and preparation method thereof
Technical field
The present invention relates to ink areas, and in particular to a kind of Graphene conductive ink and preparation method thereof.
Background technique
Graphene have excellent optics, electricity, mechanical characteristic, materialogy, micro-nano technology, the energy, biomedicine and Drug delivery etc. is with important application prospects, it is considered to be a kind of future revolutionary material.Carbon is former inside graphene The arrangement mode of son, with sp2 hybridized orbit bonding, and has the characteristics that as follows as graphite monoatomic layer: carbon atom has 4 valences Electronics, wherein 3 are electronically generated sp2 key, i.e., each carbon atom contributes the non-bonding electrons being located on pz track, neighbour The pz track and plane of atom can form pi bond at vertical direction, and the pi bond newly formed is in partly to fill up state.Research confirmation, graphene The ligancy of middle carbon atom is 3, and the bond distance between every two adjacent carbon atom is 1.42 × 10-10 meters, the angle between key and key It is 120 °.Other than σ key and other carbon atom chains are connected into the cellular layer structure of hexagonal ring, each carbon atom perpendicular to layer The pz track of plane can form polyatomic big pi bond (similar with phenyl ring) through holostrome, thus with excellent conduction and Optical property.
Basic material of the electrically conductive ink as printed electronics technology, exploitation profound significance with practical.It is silver-colored conductive Ink is one of research direction most with prospects due to its high conduction performance, good stability and relatively low cost.It receives Meter Yin is prepared by liquid phase reduction, and the growth of its granularity is controlled using protective agent.Since most end-capping reagent is all organic insulation Body, end-capping reagent are adsorbed on a nanometer silver surface and prevent charge in intermetallic transmitting, so the circuit directly printed by nano silver Resistance is usually all very big.The common practice is that high temperature sintering is carried out to printed circuit, and on the one hand sintering makes nanometer silver surface Organic end-capping reagent removing;On the other hand, sintering melts nanoparticle, and the physical contact of script is made to become metal bonding, reduces Contact resistance improves electric conductivity.But the printable fabric for flexible circuit is usually thermosensitive plastic or organic film. Currently, sintering temperature is generally at 200 DEG C or higher, on the glass transition temperature of organic film, sintering, which will lead to, is held Print the destruction of material.
But used electrically conductive ink there is problems at present:
1, the conductive filler in ink is difficult to be uniformly dispersed, and causes electric conductivity poor;
2, the conductive filler in ink and matrix composition binding force is weak or ink adhesive force itself is lower, leads to rub resistance Fastness is lower.
Based on the above situation, the invention proposes a kind of Graphene conductive ink and preparation method thereof, can effectively solve with Upper problem.
Summary of the invention
The purpose of the present invention is to provide a kind of Graphene conductive inks and preparation method thereof.Graphene conductive of the invention Ink is made up of selected raw material, and optimizes each material content, has selected the ink, graphene, levelling agent, defoaming of appropriate proportion Agent, dispersing agent and cosolvent, Graphene conductive ink obtained is compared with common conductive ink, graphene conductive of the invention Ink electric conductivity (resistivity to measure) is obvious more preferable;Fastness to rubbing is higher (Rubbing number).
In order to solve the above technical problems, present invention provide the technical scheme that
A kind of Graphene conductive ink is made: 80~100 parts of ink, graphene (institute of the raw material for including following parts by weight Stating graphene is nano-graphene microplate;The graphene with a thickness of 1~10nm;It is former in Graphene conductive ink of the invention Come in system, dispersion performance is good, is uniformly dispersed, and Graphene conductive ink of the invention is made to conduct electricity very well) 3~4.5 parts, stream 1.1~1.4 parts of flat agent, 0.9~1.2 part of defoaming agent, 2.2~2.8 parts of dispersing agent, 12~18 parts of cosolvent;The graphene is Nano-graphene microplate;The graphene with a thickness of 1~10nm.
Graphene conductive ink of the invention is made up of selected raw material, and optimizes each material content, has selected suitably to match Ink, graphene, levelling agent, defoaming agent, dispersing agent and the cosolvent of ratio, Graphene conductive ink obtained and common conductive oil Ink is compared, and Graphene conductive ink electric conductivity of the invention (resistivity to measure) is obvious more preferable;Fastness to rubbing is higher (Rubbing number).
Preferably, the Graphene conductive ink is by including that the raw material of following parts by weight is made: 90 parts of ink, graphene 3.7 parts, 1.3 parts of levelling agent, 1.1 parts of defoaming agent, 2.5 parts of dispersing agent, 14 parts of cosolvent;The graphene is that nano-graphene is micro- Piece;The graphene with a thickness of 2~8nm.
Preferably, the levelling agent is any one or a few in diglycol, isopropanol and acetylenic glycols.
Preferably, the defoaming agent is tributyl phosphate or defoaming agent BYK088.
Preferably, the dispersing agent is polycarboxylate sodium.
Preferably, the cosolvent is isophorone, cyclohexanone, butyl acetate, ethylene glycol ether acetate and ethylene glycol Any one or a few in monobutyl ether.
Preferably, the ink is UV501 ink.
Preferably, the Graphene conductive ink further includes the raw material of following parts by weight: 0.7~1.1 part of photoinitiator;Institute Stating photoinitiator is bis- (2,4,6- trimethylbenzoyl) phenyl phosphine oxides.
The present invention also provides the preparation methods of the Graphene conductive ink described in one kind, including the following steps:
A, each raw material is weighed respectively according to parts by weight;
B, the raw material in addition to graphene is mixed, 30~40min is stirred under 600~800r/min revolving speed;
C, graphene is then added, shearing 10~15min of dispersion is described to get arriving under 1600~2000r/min revolving speed Graphene conductive ink.
Compared with prior art, the present invention have the following advantages that and the utility model has the advantages that
Graphene conductive ink of the invention is made up of selected raw material, and optimizes each material content, has selected suitably to match Ink, graphene, levelling agent, defoaming agent, dispersing agent and the cosolvent of ratio, Graphene conductive ink obtained and common conductive oil Ink is compared, and Graphene conductive ink electric conductivity of the invention (resistivity to measure) is obvious more preferable;Fastness to rubbing is higher (Rubbing number).
Preparation method simple process of the invention, it is easy to operate, save manpower and equipment cost.
Specific embodiment
It is right combined with specific embodiments below in order to make those skilled in the art more fully understand technical solution of the present invention The preferred embodiments of the invention are described, but should not be understood as the limitation to this patent.
Test method described in following embodiments or test method are unless otherwise specified conventional method;The reagent And material is obtained from routine business approach, or prepare in conventional manner unless otherwise specified.
Embodiment 1:
A kind of Graphene conductive ink is made of the raw material for including following parts by weight: 80~100 parts of ink, graphene 3~ 4.5 parts, 1.1~1.4 parts of levelling agent, 0.9~1.2 part of defoaming agent, 2.2~2.8 parts of dispersing agent, 12~18 parts of cosolvent;It is described Graphene is nano-graphene microplate;The graphene with a thickness of 1~10nm.
Preferably, the Graphene conductive ink is by including that the raw material of following parts by weight is made: 90 parts of ink, graphene 3.7 parts, 1.3 parts of levelling agent, 1.1 parts of defoaming agent, 2.5 parts of dispersing agent, 14 parts of cosolvent;The graphene is that nano-graphene is micro- Piece;The graphene with a thickness of 2~8nm.
Preferably, the levelling agent is any one or a few in diglycol, isopropanol and acetylenic glycols.
Preferably, the defoaming agent is tributyl phosphate or defoaming agent BYK088.
Preferably, the dispersing agent is polycarboxylate sodium.
Preferably, the cosolvent is isophorone, cyclohexanone, butyl acetate, ethylene glycol ether acetate and ethylene glycol Any one or a few in monobutyl ether.
Preferably, the ink is UV501 ink.
Preferably, the Graphene conductive ink further includes the raw material of following parts by weight: 0.7~1.1 part of photoinitiator;Institute Stating photoinitiator is bis- (2,4,6- trimethylbenzoyl) phenyl phosphine oxides.
The present invention also provides the preparation methods of the Graphene conductive ink described in one kind, including the following steps:
A, each raw material is weighed respectively according to parts by weight;
B, the raw material in addition to graphene is mixed, 30~40min is stirred under 600~800r/min revolving speed;
C, graphene is then added, shearing 10~15min of dispersion is described to get arriving under 1600~2000r/min revolving speed Graphene conductive ink.
Embodiment 2:
A kind of Graphene conductive ink is made: 80 parts of ink, 3 parts of graphene, levelling of the raw material for including following parts by weight 1.1 parts of agent, 0.9 part of defoaming agent, 2.2 parts of dispersing agent, 12 parts of cosolvent;The graphene is nano-graphene microplate;The stone Black alkene with a thickness of 1~10nm.
In the present embodiment, the levelling agent is diglycol.
In the present embodiment, the defoaming agent is tributyl phosphate.
In the present embodiment, the dispersing agent is polycarboxylate sodium.
In the present embodiment, the cosolvent is isophorone.
In the present embodiment, the ink is UV501 ink.
In the present embodiment, the Graphene conductive ink further includes the raw material of following parts by weight: 0.7 part of photoinitiator; The photoinitiator is bis- (2,4,6- trimethylbenzoyl) phenyl phosphine oxides.
In the present embodiment, the preparation method of the Graphene conductive ink, including the following steps:
A, each raw material is weighed respectively according to parts by weight;
B, the raw material in addition to graphene is mixed, stirs 40min under 600r/min revolving speed;
C, graphene is then added, shearing disperses 15min to get the graphene conductive is arrived under 1600r/min revolving speed Ink.
Embodiment 3:
A kind of Graphene conductive ink, by include following parts by weight raw material be made: 100 parts of ink, 4.5 parts of graphene, 1.4 parts of levelling agent, 1.2 parts of defoaming agent, 2.8 parts of dispersing agent, 18 parts of cosolvent;The graphene is nano-graphene microplate;Institute State graphene with a thickness of 1~10nm.
In the present embodiment, the levelling agent is isopropanol.
In the present embodiment, the defoaming agent is defoaming agent BYK088.
In the present embodiment, the dispersing agent is polycarboxylate sodium.
In the present embodiment, the cosolvent is ethylene glycol ether acetate.
In the present embodiment, the ink is UV501 ink.
In the present embodiment, the Graphene conductive ink further includes the raw material of following parts by weight: 1.1 parts of photoinitiator; The photoinitiator is bis- (2,4,6- trimethylbenzoyl) phenyl phosphine oxides.
In the present embodiment, the preparation method of the Graphene conductive ink, including the following steps:
A, each raw material is weighed respectively according to parts by weight;
B, the raw material in addition to graphene is mixed, stirs 30min under 800r/min revolving speed;
C, graphene is then added, shearing disperses 10min to get the graphene conductive is arrived under 2000r/min revolving speed Ink.
Embodiment 4:
A kind of Graphene conductive ink is made of the raw material for including following parts by weight: 90 parts of ink, 3.7 parts of graphene, stream 1.3 parts of flat agent, 1.1 parts of defoaming agent, 2.5 parts of dispersing agent, 14 parts of cosolvent;The graphene is nano-graphene microplate;It is described Graphene with a thickness of 2~8nm.
In the present embodiment, the levelling agent is the diglycol and acetylenic glycols that mass ratio is 1:1.
In the present embodiment, the defoaming agent is defoaming agent BYK088.
In the present embodiment, the dispersing agent is polycarboxylate sodium.
In the present embodiment, the cosolvent is cyclohexanone, butyl acetate and the ethylene glycol only son that mass ratio is 1:1:1 Ether.
In the present embodiment, the ink is UV501 ink.
In the present embodiment, the Graphene conductive ink further includes the raw material of following parts by weight: 0.9 part of photoinitiator; The photoinitiator is bis- (2,4,6- trimethylbenzoyl) phenyl phosphine oxides.
In the present embodiment, the preparation method of the Graphene conductive ink, including the following steps:
A, each raw material is weighed respectively according to parts by weight;
B, the raw material in addition to graphene is mixed, stirs 35min under 700r/min revolving speed;
C, graphene is then added, shearing disperses 12min to get the graphene conductive is arrived under 1800r/min revolving speed Ink.
The Graphene conductive ink and the progress of common conductive ink that the embodiment of the present invention 2 to embodiment 4 is obtained below Performance test, test result are as shown in table 1:
Table 1
As can be seen from the above table, Graphene conductive ink of the invention has the advantage that compared with common conductive ink, Graphene conductive ink electric conductivity of the invention (resistivity to measure) is obvious more preferable;Higher (the friction time of fastness to rubbing Number).
The above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair Limitation of the invention, protection scope of the present invention should be defined by the scope defined by the claims..For the art For those of ordinary skill, without departing from the spirit and scope of the present invention, several improvements and modifications can also be made, these change It also should be regarded as protection scope of the present invention into retouching.

Claims (9)

1. a kind of Graphene conductive ink, which is characterized in that be made of the raw material for including following parts by weight: 80~100 parts of ink, 3~4.5 parts of graphene, 1.1~1.4 parts of levelling agent, 0.9~1.2 part of defoaming agent, 2.2~2.8 parts of dispersing agent, cosolvent 12~ 18 parts;The graphene is nano-graphene microplate;The graphene with a thickness of 1~10nm.
2. Graphene conductive ink according to claim 1, which is characterized in that the Graphene conductive ink by include with The raw material of lower parts by weight is made: 90 parts of ink, 3.7 parts of graphene, 1.3 parts of levelling agent, 1.1 parts of defoaming agent, 2.5 parts of dispersing agent, 14 parts of cosolvent;The graphene is nano-graphene microplate;The graphene with a thickness of 2~8nm.
3. Graphene conductive ink according to claim 1, which is characterized in that the levelling agent be diglycol, Any one or a few in isopropanol and acetylenic glycols.
4. Graphene conductive ink according to claim 1, which is characterized in that the defoaming agent is tributyl phosphate or disappears Infusion BYK088.
5. Graphene conductive ink according to claim 1, which is characterized in that the dispersing agent is polycarboxylate sodium.
6. Graphene conductive ink according to claim 1, which is characterized in that the cosolvent is isophorone, hexamethylene Any one or a few in ketone, butyl acetate, ethylene glycol ether acetate and ethylene glycol monobutyl ether.
7. Graphene conductive ink according to claim 1, which is characterized in that the ink is UV501 ink.
8. Graphene conductive ink according to claim 8, which is characterized in that the Graphene conductive ink further include with The raw material of lower parts by weight: 0.7~1.1 part of photoinitiator;The photoinitiator is bis- (2,4,6- trimethylbenzoyl) phenyl Phosphine oxide.
9. a kind of preparation method of Graphene conductive ink as claimed in any one of claims 1 to 8, which is characterized in that including The following steps:
A, each raw material is weighed respectively according to parts by weight;
B, the raw material in addition to graphene is mixed, 30~40min is stirred under 600~800r/min revolving speed;
C, graphene is then added, shearing disperses 10~15min to get the graphite is arrived under 1600~2000r/min revolving speed Alkene electrically conductive ink.
CN201910764706.8A 2019-08-19 2019-08-19 A kind of Graphene conductive ink and preparation method thereof Pending CN110408267A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110917982A (en) * 2019-12-23 2020-03-27 珠海斗门超毅实业有限公司 Pretreatment method and device for circuit board heat dissipation ink

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Publication number Priority date Publication date Assignee Title
CN105936771A (en) * 2016-07-12 2016-09-14 深圳华云科技实业有限公司 Graphene printing ink and preparation method thereof
CN106752385A (en) * 2017-01-11 2017-05-31 青岛瑞利特新材料科技有限公司 A kind of Graphene modified water-soluble electrically conductive ink and preparation method thereof
CN106883681A (en) * 2017-03-17 2017-06-23 青岛瑞利特新材料科技有限公司 A kind of electrically conductive ink containing flake graphite alkene and composition metal filler
CN107674505A (en) * 2017-11-23 2018-02-09 深圳市国创珈伟石墨烯科技有限公司 A kind of Graphene conductive ink and preparation method thereof
CN108276825A (en) * 2018-02-11 2018-07-13 安徽省中彩印务有限公司 A kind of environmental protection stable type cured printing ink and preparation method thereof
CN109943150A (en) * 2019-02-01 2019-06-28 广东华祐新材料有限公司 A kind of electrically conductive ink and its preparation method and application

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105936771A (en) * 2016-07-12 2016-09-14 深圳华云科技实业有限公司 Graphene printing ink and preparation method thereof
CN106752385A (en) * 2017-01-11 2017-05-31 青岛瑞利特新材料科技有限公司 A kind of Graphene modified water-soluble electrically conductive ink and preparation method thereof
CN106883681A (en) * 2017-03-17 2017-06-23 青岛瑞利特新材料科技有限公司 A kind of electrically conductive ink containing flake graphite alkene and composition metal filler
CN107674505A (en) * 2017-11-23 2018-02-09 深圳市国创珈伟石墨烯科技有限公司 A kind of Graphene conductive ink and preparation method thereof
CN108276825A (en) * 2018-02-11 2018-07-13 安徽省中彩印务有限公司 A kind of environmental protection stable type cured printing ink and preparation method thereof
CN109943150A (en) * 2019-02-01 2019-06-28 广东华祐新材料有限公司 A kind of electrically conductive ink and its preparation method and application

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110917982A (en) * 2019-12-23 2020-03-27 珠海斗门超毅实业有限公司 Pretreatment method and device for circuit board heat dissipation ink

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Application publication date: 20191105