CN106519804A - Graphene conductive ink as well as preparing method and application thereof - Google Patents

Graphene conductive ink as well as preparing method and application thereof Download PDF

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Publication number
CN106519804A
CN106519804A CN201610928360.7A CN201610928360A CN106519804A CN 106519804 A CN106519804 A CN 106519804A CN 201610928360 A CN201610928360 A CN 201610928360A CN 106519804 A CN106519804 A CN 106519804A
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solvent
centrifugation
conductive ink
preparation
graphene
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CN106519804B (en
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邓吨英
石珉滈
冯烁
王洋
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Aerospace Science and Industry Changsha New Materials Research Institute Co Ltd
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Hunan Aerospace New Material Technology Inst Co Ltd
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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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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • Wood Science & Technology (AREA)
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Abstract

The invention discloses graphene conductive ink as well as a preparing method and an application thereof. The preparing method comprises the following steps: 1, ultrasonically dispersing a dispersant and a graphite flake in a first solution so as to obtain a mixture A; 2, carrying out first centrifuging on the mixture A, and carrying out secondary centrifuging on upper-layer dispersion liquid which is obtained after first centrifuging so as to obtain precipitates B; 3, dispersing the precipitates B in a second solvent so as to obtain dispersion liquid C; 4, adding solvents and additives for the conductive ink into the dispersion liquid C; and 5, removing the second solvent so as to obtain the graphene conductive ink. In the method, the graphene is obtained through in-situ preparation, so that the influence of graphene flaws on conductive performance is avoided. The graphene conductive ink which is high in concentration and high in conductivity can be obtained.

Description

A kind of graphene conductive ink and its preparation method and application
Technical field
The present invention relates to a kind of graphene conductive ink and its preparation method and application, belongs to electronic information material and printing Electronic applications.
Background technology
Conductive ink is the basis for developing electronic devices and components, is the critical material of encapsulation, electrode and interconnection, be collection it is metallurgical, Chemical industry, electronic technology in a kind of high-tech electronics functional material of one, mainly for the manufacture of thick film integrated circuit, film crystal Pipe(TFT), sensor, organic photovoltaic, solaode, flexible display, wireless radio frequency identification mark(RFID), wearable electricity The every field of the electron trade such as sub- product and memorizer.Conductive filler in conductive ink typically by noble metal Au, Ag or Base metal Cu, Ni, Al etc. are constituted.The general good conductivity of noble metal, it is not oxidizable, but if using noble metal in a large number, produce into This rising;And base metal is easier oxidation, after metal oxidation, the electric conductivity of conductive ink will be affected.Other base metal slurry Sintering typically carry out under nitrogen or vacuum condition, this technique increases can cost, while operating process is complicated.
Grapheme material has highest electrical conductivity 200,000cm2/ V s, electric current density carry up to 108A/cm2, most Big mechanical strength, best heat conductivity and high-temperature stability.And the manufacturing cost of Graphene is well below nano metal Grain.
Patent US2015/0072162 A1 discloses a kind of method for preparing high concentration graphene conductive ink, using super Sound wave liquid phase stripping prepares Graphene, using the aqueous solution containing NaCl by Graphene precipitation, cleaning NaCl and drying, then will Graphene dispersion prepares the graphene conductive ink of 3.4mg/ml, and graphene conductive body prepared by this kind of method is not Height, all has a significant impact containing substantial amounts of dispersant, the viscosity of conductive ink and dried electric conductivity.
The content of the invention
Present invention solves the technical problem that being to improve the concentration of graphene conductive ink, reduce in graphene conductive ink The content of dispersant.Graphene dispersing solution is prepared by using dispersant, solvent and graphite flake original position, by graphene dispersing solution Multi-layer graphene is removed by centrifugation, then is removed dispersant excessive in graphene dispersing solution by high speed centrifugation, plus Enter conductive ink solvent and auxiliary agent, the method replaced by solvent obtains the graphene conductive ink of high concentration.
The technical scheme is that, there is provided a kind of preparation method of graphene conductive ink, comprise the steps of:
(1)Dispersant, graphite flake are scattered in the first solvent, supersound process obtains mixture A;
(2)Mixture A is carried out into first time centrifugation, the upper strata dispersion liquid after first time is centrifuged carries out second centrifugation again, obtains Precipitate B;
(3)Precipitate B is scattered in the second solvent, dispersion liquid C is obtained;
(4)Conductive ink solvent and auxiliary agent is added in dispersion liquid C;
(5)The second solvent is removed, graphene conductive ink is obtained.
Wherein, step(2)In first time centrifugation adopt low-speed centrifugal, its centrifugal speed be for can so that mixture A in Multi-layer graphite, graphite pellet, and the non-setting speed of part Graphene;Second centrifugation adopts high speed centrifugation, centrifugation speed Rate is the speed for causing Graphene precipitation.
Preferably, first solvent is the solvent that can dissolve the dispersant;It is preferred that water, ethanol, normal propyl alcohol, isopropanol Deng alcohols one or several.
Preferably, second centrifugation is carried out again after the upper strata dispersion liquid dilution after be centrifuged first time;Preferably, it is described dilute It is the first solvent to release the solvent for using;Preferably, more than 2 times of the dilution;It is highly preferred that 5-10 times of dilution.
Preferably, second solvent is the solvent of energy dispersed graphite alkene;Preferably, the second solvent be ethanol, normal propyl alcohol, The alcohols such as isopropanol one or several.
Preferably, the graphite flake is the naturally occurring graphite such as crystalline flake graphite, micro crystal graphite.
Preferably, the step(5)In take the mode of revolving to remove the second solvent.The dispersant is cellulose family thing Matter;In preferred, ethyl, hydroxyethyl cellulose, hydroxypropyl methyl cellulose one or several, as the same of dispersant When play a part of aid in intercalation.
Preferably, the step(1)In, the weight ratio of dispersant and the first solvent is 0.001-0.1:1;The graphite flake Weight ratio with the first solvent is 0.001-0.2:1.
Preferably, the step(1)In, ultrasonic time is 1-8 hours, and supersonic frequency is 20-40kHz.It is centrifuged for second Centrifugation rate more than for the first time centrifugation centrifugation rate;Preferably, for the first time the centrifugation rate of centrifugation be 5000-7500 turn/ Point, centrifugation time is 5-25min;The centrifugation rate of centrifugation is more than 11000 revs/min for the first time, and centrifugation time is 1-4 hours.
Preferably, conductive ink solvent be can dissolve each other with the second solvent, and can dispersed graphite alkene solvent, such as Oleum Pini One or several in alcohol, Ketohexamethylene and toluene.Conductive ink used additives are the conductive ink usual auxiliaries such as thixotropic agent.
The present invention further provides the graphene conductive ink that above-mentioned preparation method is obtained.
The present invention provides the graphene conductive ink in 3D inkjet printing electronic circuits, solaode, RF identification Application on label, printed circuit board and various flexible electronic products.The graphene conductive ink of the high concentration for preparing Middle Graphene concentration can reach 5-20mg/ml, and in below 30cp, for 3D inkjet printing electronic circuits, 250 DEG C sinter viscosity Afterwards, sheet resistance 1-150 Ω/, can be used in solaode, RFID tag, printed circuit board and various flexible electrical On sub- product.
The present invention prepares graphene dispersing solution by original position, and the dispersant of the excess added during preparing Graphene leads to Cross and be centrifuged off at a high speed, and then the method replaced by solvent obtains the graphene conductive ink of high concentration.
A kind of method of graphene conductive ink for preparing high concentration in situ of the present invention, with advantages below:
1. original position prepares Graphene, it is to avoid impact of the presence of Graphene defect to electric conductivity;
2., during high speed centrifugation, Graphene sinks to bottom, and excessive dispersant is in the solvent of upper strata, therefore the dispersant of excess Can be removed by ultracentrifugal method, so as to obtain the graphene conductive ink of high connductivity;
3. solvent displacement is carried out by the method for rotary evaporation, the graphene conductive ink of higher concentration can be obtained.
Description of the drawings
The flow chart that Fig. 1 represents the preparation method of 2 graphene conductive ink of embodiment.
Specific embodiment
With reference to embodiment, the invention will be further described.
For making the object, technical solutions and advantages of the present invention clearer, below the embodiments of the present invention are carried out Detailed elaboration.Example is served only for the explanation present invention, is not intended to limit the scope of the present invention.
Embodiment 1
The ethyl cellulose of 1g is dissolved in 100ml ethanol, after dissolving, in above-mentioned solution, adds 5g crystalline flake graphites ultrasound 4 little When, the centrifugation 15 minutes of 7500 revs/min of upper solution is taken, is taken after the supernatant liquid after centrifugation dilutes 10 times 11000 Rev/min centrifugal condition under be centrifuged 2 hours, remove supernatant liquid, the precipitation being centrifuged be dispersed in 100ml ethanol, plus Enter terpineol 1ml and Ketohexamethylene 9ml, at 50 revs/min, ethanol is evaporated under conditions of 50 DEG C, the Graphene for obtaining high concentration is led Electric ink, the content of Graphene is 10mg/ml, and viscosity is 18cps.Conductive ink be used for 3D inkjet printing electronic circuits, 250 DEG C After sintering, 98 Ω of sheet resistance/.
Embodiment 2
The hydroxyethyl cellulose of 1g is dissolved in 100ml water, after dissolving, in above-mentioned solution, adds 5g crystalline flake graphites ultrasound 4 little When, the centrifugation 15 minutes of 7500 revs/min of upper solution is taken, is taken after the supernatant liquid after centrifugation dilutes 10 times 11000 Rev/min centrifugal condition under be centrifuged 2 hours, remove supernatant liquid, the precipitation being centrifuged be dispersed in 100ml ethanol, plus Enter terpineol 1ml and Ketohexamethylene 9ml, at 50 revs/min, ethanol is evaporated under conditions of 50 DEG C, the Graphene for obtaining high concentration is led Electric ink, the content of Graphene is 10mg/ml, and viscosity is 18cps.Conductive ink be used for 3D inkjet printing electronic circuits, 250 DEG C After sintering, 98 Ω of sheet resistance/.
Embodiment 3
The ethyl cellulose of 2g is dissolved in 100ml ethanol, after dissolving, in above-mentioned solution, adds 10g crystalline flake graphites ultrasound 4 little When, the centrifugation 15 minutes of 7500 revs/min of upper solution is taken, is taken after the supernatant liquid after centrifugation dilutes 10 times 11000 Rev/min centrifugal condition under be centrifuged 2 hours, remove supernatant liquid, the precipitation being centrifuged be dispersed in 100ml ethanol, plus Enter terpineol 1ml and Ketohexamethylene 9ml, at 50 revs/min, ethanol is evaporated under conditions of 50 DEG C, the Graphene for obtaining high concentration is led Electric ink, the content of Graphene is 15mg/ml, and viscosity is 25cps.Conductive ink be used for 3D inkjet printing electronic circuits, 250 DEG C After sintering, 90 Ω of sheet resistance/.
Embodiment 4
The hydroxyethyl cellulose of 2g is dissolved in 100ml water, after dissolving, in above-mentioned solution, adds 10g crystalline flake graphites ultrasound 4 little When, the centrifugation 15 minutes of 7500 revs/min of upper solution is taken, is taken after the supernatant liquid after centrifugation dilutes 10 times 11000 Rev/min centrifugal condition under be centrifuged 2 hours, remove supernatant liquid, the precipitation being centrifuged be dispersed in 100ml ethanol, plus Enter terpineol 1ml and Ketohexamethylene 9ml, at 50 revs/min, ethanol is evaporated under conditions of 50 DEG C, the Graphene for obtaining high concentration is led Electric ink, the content of Graphene is 15mg/ml, and viscosity is 25cps.Conductive ink be used for 3D inkjet printing electronic circuits, 250 DEG C After sintering, 90 Ω of sheet resistance/.
Above the step of various methods divide, be intended merely to description it is clear, can merge into when realizing a step or Some steps are split, multiple steps are decomposed into, as long as comprising identical logical relation, all in the protection domain of this patent It is interior;To adding inessential modification in algorithm or in flow process or introducing inessential design, but its algorithm is not changed With the core design of flow process all in the protection domain of the patent.
It will be understood by those skilled in the art that the respective embodiments described above are to realize the specific embodiment of the present invention, And in actual applications, can to which, various changes can be made in the form and details, without departing from the spirit and scope of the present invention.

Claims (11)

1. a kind of preparation method of graphene conductive ink, it is characterised in that comprise the steps of:
(1)Dispersant, graphite flake are scattered in the first solvent, supersound process obtains mixture A;
(2)Mixture A is carried out into first time centrifugation, the upper strata dispersion liquid after first time is centrifuged carries out second centrifugation again, obtains Precipitate B;
(3)Precipitate B is scattered in the second solvent, dispersion liquid C is obtained;
(4)Conductive ink solvent and auxiliary agent is added in dispersion liquid C;
(5)The second solvent is removed, graphene conductive ink is obtained.
2. preparation method as claimed in claim 1, it is characterised in that first solvent is to dissolve the molten of the dispersant Agent;It is preferred that one or several in water, ethanol, normal propyl alcohol, isopropanol.
3. preparation method as claimed in claim 1 or 2, it is characterised in that the upper strata dispersion liquid dilution after being centrifuged for the first time Carry out second centrifugation afterwards again;Preferably, the solvent for using that dilutes is the first solvent;Preferably, it is described dilution 2 times with On;It is highly preferred that 5-10 times of dilution.
4. the preparation method as described in any one of claim 1-3, it is characterised in that second solvent is for can dispersed graphite alkene Solvent;Preferably, the second solvent is water, ethanol, normal propyl alcohol, one or several in isopropanol.
5. the preparation method as described in any one of claim 1-4, it is characterised in that the step(5)In take the side of revolving Formula removes the second solvent.
6. dispersant described in is cellulose substances;In preferred, ethyl, hydroxyethyl cellulose, hydroxypropyl methyl cellulose One or several.
7. the preparation method as described in any one of claim 1-5, it is characterised in that the step(1)In, dispersant and first The weight ratio of solvent is 0.001-0.1:1;The weight ratio of the graphite flake and the first solvent is 0.001-0.2:1.
8. the preparation method as described in any one of claim 1-6, it is characterised in that the step(1)In, ultrasonic time is 1- 8 hours, supersonic frequency was 20-40kHz;Centrifugation rate of the centrifugation rate of second centrifugation more than centrifugation for the first time;Preferably, The centrifugation rate of centrifugation is 5000-7500 rev/min for the first time, and centrifugation time is 5-25min;The centrifugation rate of centrifugation is for the first time More than 11000 revs/min, centrifugation time is 1-4 hours.
9. the preparation method as described in any one of claim 1-7, it is characterised in that conductive ink solvent is can be molten with second It is that agent is dissolved each other, and can dispersed graphite alkene solvent;Preferably, it is one or several in terpineol, Ketohexamethylene and toluene; Conductive ink used additives are the conductive ink usual auxiliaries such as thixotropic agent.
10. the graphene conductive ink that the preparation method described in any one of claim 1-8 is obtained, stone in graphene conductive ink Black alkene concentration is 5-20mg/ml, and viscosity is in below 30cps.
Graphene conductive ink described in 11. claim 9 is in 3D inkjet printing electronic circuits, solaode, radio frequency identification marking Application on label, printed circuit board and various flexible electronic products.
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CN109817382A (en) * 2017-11-21 2019-05-28 山东欧铂新材料有限公司 A kind of preparation method of high-stability graphene electrocondution slurry
CN109830512A (en) * 2019-01-30 2019-05-31 合肥鑫晟光电科技有限公司 Display base plate, the preparation method of display base plate, display device
CN110117440A (en) * 2019-05-10 2019-08-13 齐鲁工业大学 A kind of conductive ink and preparation method thereof
CN110165366A (en) * 2019-04-22 2019-08-23 浙江大学 A kind of graphene antenna of thermal transfer and its preparation method and application
CN110183908A (en) * 2019-03-19 2019-08-30 浙江省海洋开发研究院 A kind of electrically conductive ink and preparation method thereof of containing graphene compound
CN110895998A (en) * 2019-11-22 2020-03-20 西安交通大学 Electrode material ink, preparation method and method for preparing miniature super capacitor by using electrode material ink
CN111560188A (en) * 2020-06-01 2020-08-21 南京林业大学 Nano-silver/graphene composite electromagnetic shielding ink and preparation method thereof

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CN107197545B (en) * 2017-06-20 2020-09-01 广西大学 Nano-cellulose graphene composite electrothermal film and green preparation process thereof

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109817382A (en) * 2017-11-21 2019-05-28 山东欧铂新材料有限公司 A kind of preparation method of high-stability graphene electrocondution slurry
CN109830512A (en) * 2019-01-30 2019-05-31 合肥鑫晟光电科技有限公司 Display base plate, the preparation method of display base plate, display device
CN110183908A (en) * 2019-03-19 2019-08-30 浙江省海洋开发研究院 A kind of electrically conductive ink and preparation method thereof of containing graphene compound
CN110183908B (en) * 2019-03-19 2022-03-22 浙江省海洋开发研究院 Conductive ink containing graphene compound and preparation method thereof
CN110165366A (en) * 2019-04-22 2019-08-23 浙江大学 A kind of graphene antenna of thermal transfer and its preparation method and application
CN110117440A (en) * 2019-05-10 2019-08-13 齐鲁工业大学 A kind of conductive ink and preparation method thereof
CN110895998A (en) * 2019-11-22 2020-03-20 西安交通大学 Electrode material ink, preparation method and method for preparing miniature super capacitor by using electrode material ink
CN111560188A (en) * 2020-06-01 2020-08-21 南京林业大学 Nano-silver/graphene composite electromagnetic shielding ink and preparation method thereof

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