CN108305716A - A kind of preparation method of graphene conductive slurry and its conductive coating of preparation - Google Patents
A kind of preparation method of graphene conductive slurry and its conductive coating of preparation Download PDFInfo
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- CN108305716A CN108305716A CN201810055442.4A CN201810055442A CN108305716A CN 108305716 A CN108305716 A CN 108305716A CN 201810055442 A CN201810055442 A CN 201810055442A CN 108305716 A CN108305716 A CN 108305716A
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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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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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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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Abstract
The present invention uses graphene for conductive filler, uses cryogenic glass powder for binder, and the graphene conductive slurry for providing elevated temperature cohesiveness energy is mixed with other organic solvents and additive.And be coated onto potsherd surface, by high temperature sintering for a period of time after, potsherd surface obtain one layer with excellent binding force and superior electrical conductivity can graphene conductive coating.
Description
Technical field
The present invention relates to conductive coatings more particularly to a kind of graphene conductive slurry and ceramic matrix surface graphene to lead
The preparation of electrocoat.
Background technology
Electrocondution slurry (electrically conductive paste) be collect material, metallurgy, chemical industry, electronic technology in
The electronic functional material of one, is hydrid integrated circuit, sensing element, surface mounting technology, resistor network, display, and
The basic material of various electronic discrete devices etc..With the high speed development of information industry so that device to micromation, precise treatment and
The directions such as flexibility are developed, and lot of domestic and international scientific research institution produces great interest to the development and application of electrocondution slurry.
Electrocondution slurry generally includes 3 kinds of function phase, organic carrier, Binder Phase components.I.e. conductive phase (gold, silver, copper, nickel and
Tin-bismuth alloy electroplating etc.), organic carrier (organic resin and solvent) and/or permanent adhesive agent (silicate glass etc.).According to conductive paste
Expect that the property of composition, electrocondution slurry are broadly divided into organic type electrocondution slurry, inorganic type electrocondution slurry and compound-type conducting slurry.Its
In, for compound-type conducting slurry using conductive metal particles as conductive phase, high molecular polymer is Binder Phase, has excellent electric conductivity
And mechanical performance, process is relatively easy, and repeatability and conductive stability are stronger, and the stable storing phase is longer, has higher
Practicability, have a wide range of applications, at present on the market most of electrocondution slurry be it is such.
Carbon conductive filler (including carbon black, graphite, carbon fiber and its mixture) is usually used in electrically conductive ink.In recent ten years
The research of carbon series conductive ink is concentrated mainly on influence of the factors such as the pattern by conductive filler, proportioning to electrically conductive ink performance
Rule.Ma Xiaoxu etc. (referring to Ma Xiaoxu, Wei Xianfu, Huang Beiqing, waits electric conductivity to fill out by conductive filler of carbon black, graphite and silver powder
Expect influence [J] the Beijing Printing Institute journal to Electric radiant Heating Film electrically conductive ink performance, 2011,19 (2)：16-18.), Xiao Shuan etc.
Using different-shape and the carbon dust of proportioning, as conductive filler, (referring to Xiao Shuan, Du Yong states, Liu Qicheng waits function in carbon series conductive ink
Influence [J] electrical materials of opposite ink performance, 2013 (1)：27-31.), shown that the type of conductive phase, pattern starch carbon
The influence of the performances such as viscosity, resistance.Novel carbon conductive filler includes carbon nanotube (CNTs) and graphene, because having big π
Key and have excellent electric conductivity, but in the application exist stablize separation and scattering problem.Grandson waits quietly utilizing under the conditions of sand milling
Sun/nonionic surfactant compounding dispersing Nano carbon tubes (wait carbon nanotube fillers referring to Sun Jing, Liu Jiahong, bear Gao Hu
Electrostatic self-assembled prepares and application [J] coatings industries in conductive coating, 2011,41 (10)：25-29.), with mica or two
Titanium oxide is compound, hence it is evident that improves the dispersibility of CNTs, more traditional carbon nano tube surface absorption charged ion or organic matter etc. side
Method dispersibility is more preferable.
As a kind of new carbon, graphene itself has high conductivity and high-termal conductivity, theoretically its electron transfer
Rate can reach 2 × 105cm2/ Vs, 140 times of electron mobility about in silicon, 20 times of GaAs, temperature stability is high, reason
By upper, conductivity is up to 108S/m, it is lower than copper, silver, it is conductive best material at room temperature.With graphene as conductive paste
Conductive phase (conductive filler) in material, can reduce the cost of electrocondution slurry.But made of current graphene conductive slurry
The cohesive force of coating and ceramic surface is generally insufficient, it is necessary to further be improved.
Invention content
For disadvantages mentioned above, patent of the present invention uses graphene for conductive filler, uses cryogenic glass powder for binder, with
Other organic solvents and additive are mixed with the graphene conductive slurry for providing elevated temperature cohesiveness energy.And it is coated onto pottery
Tile surface, by high temperature sintering for a period of time after, potsherd surface obtain one layer have excellent binding force and excellent conduction
The graphene conductive coating of performance.
Specifically, the present invention provides a kind of preparation method of the graphene conductive slurry of high temperature bond performance, including it is as follows
Step：
(1) under the conditions of 60~80 DEG C, by magnetic agitation respectively by the antifoaming agent of 1~5wt.% and 1~5wt.%
Thickener is dissolved in terpinol.
(2) under the conditions of 60~80 DEG C, by magnetic agitation, proportionally successively addition 1~2wt.% dispersants, 1~
3wt.% levelling agents, 1~2wt.% plasticizer, mixing time be 12~for 24 hours, obtain the organic carrier phase of the electrocondution slurry.
(3) organic carrier for weighing certain mass is mutually placed in vacuum stirring kettle, in 200~500r/min stirring at low speed
Under the conditions of, be then added uniformly mixed graphene powder and glass powder with low melting point in batches, addition graphene, organic carrier and
The mass ratio of glass powder is 40~65: 25~55: 5~10.
(4) it is 120~160 DEG C above-mentioned tentatively uniformly mixed presoma to be placed in temperature, and vacuum degree is the perseverance of -0.1Mpa
In warm vacuum drying oven, 1~2h is heated, maturation process is carried out to presoma.
(5) presoma after above-mentioned curing is placed in the de-airing mixer that vacuum degree is -0.1Mpa with 500~
The rotating speed of 1500r/min persistently stirs 24~72h, you can obtains the graphene conductive slurry of stable dispersion.
Preferably, the graphene is prepared by liquid phase ultrasound stripping method.
Preferably, the antifoaming agent is tributyl phosphate.
Preferably, the thickener is ethyl cellulose.
Preferably, the dispersant is selected from silane coupling agent or titanate coupling agent, further preferably silane coupling agent.
Preferably, the levelling agent is selected from dimethicone or butyl cellosolve.
Preferably, the plasticizer is selected from dibutyl phthalate.
The present invention also provides a kind of preparation methods of graphene conductive coating, include the following steps：
(1) electrocondution slurry prepared uniformly being coated into matrix surface in a manner of drop coating, control coated area is 2.5 ×
2.5cm2。
(2) matrix for having coated electrocondution slurry is placed in the Muffle furnace that temperature is 350~450 DEG C, is sintered 0.5~2h,
It can be obtained the matrix for covering conductive coating.
Preferably, described matrix is potsherd.
Beneficial effects of the present invention：
(1) graphene conductive coating can be sintered in 350~450 DEG C of temperature range in patent of the present invention, sintering
The sintering temperature of the more conventional electrocondution slurry of temperature is low, more energy conservation and environmental protection.
(2) present invention is mostly conductive bodies using the graphene powder of high conductivity, compares conventional conductive silver slurry,
Cost is more cheap.
(3) patent of the present invention uses glass powder with low melting point as Binder Phase so that graphene can be combined preferably and made pottery
Porcelain basal body surface solves adhesion problem of the graphene in matrix surface.
Description of the drawings
In Fig. 1, (a) graphene SEM spectrum, (b) graphene powder Raman collection of illustrative plates, (c) blank ceramic matrix, (d) coating
The ceramic matrix of graphene conductive coating after sintering processes, the graphene conductive coating SEM figures after (e) being sintered, (d)-(e) are
The picture concerned of 1# samples in embodiment one；
Specific implementation mode
Below in conjunction with specific embodiment and attached drawing, the present invention is described in detail, and wherein graphene contains graphite by Hunan state
Science and Technology Ltd. provides.
Embodiment one：
The preparation of graphene conductive slurry, includes the following steps：
(1) under the conditions of 80 DEG C, by magnetic agitation respectively by the tributyl phosphate of 2wt.% (antifoaming agent) and 5wt.%
Ethyl cellulose (thickener) be dissolved in terpinol.
(2) under the conditions of 80 DEG C, by magnetic agitation, proportionally addition 2wt.% silane coupling agents (dispersion successively
Agent), 3wt.% dimethicones (levelling agent), 1wt.% dibutyl phthalates (plasticizer), mixing time 12h obtains
To the organic carrier phase of the electrocondution slurry.
(3) organic carrier for weighing certain mass is mutually placed in vacuum stirring kettle, in the condition of 500r/min stirring at low speed
Under, uniformly mixed graphene powder and glass powder with low melting point, addition graphene, organic carrier and glass are then added in batches
The ratio of powder is 45: 50: 5.
(4) it is 150 DEG C above-mentioned tentatively uniformly mixed presoma to be placed in temperature, and vacuum degree is that the constant temperature of -0.1Mpa is true
In empty baking oven, 1h is heated, maturation process is carried out to presoma.
(5) presoma after above-mentioned curing is placed in the de-airing mixer that vacuum degree is -0.1Mpa with 1000r/min
Rotating speed persistently stir 48h, you can obtain the graphene conductive slurry of stable dispersion.
The preparation of graphene conductive coating, includes the following steps：
(1) by the electrocondution slurry prepared in a manner of drop coating uniform coated ceramic piece surface, control coated area be 2.5 ×
2.5cm2。
(2) potsherd for having coated electrocondution slurry is placed in the Muffle furnace that temperature is 450 DEG C, is sintered 0.5h, you can
To the potsherd for covering conductive coating.
After specific test is using the test sintering of DIGITAL MULTIMETER VC480C+ type digital display resistance meters
Surface resistivity, every time test 3 parallel samples.It is tested and is burnt according to the method for ASTMD 3359-2002 coating surfaces scribing line
The face coat binding force of sample after knot, tests 3 parallel samples every time, and corresponding data refer to table 1.
The electric conductivity and adhesive property of 1 graphene conductive coating surface of table
| Sample number into spectrum | Surface resistivity/Ω | Adhesive force (ASTMD 3359-2002) |
| 1# | 0.447 | ≥4B |
| 2# | 0.395 | ≥4B |
| 3# | 0.428 | ≥4B |
Graphene conductive coating photo made from the present embodiment one is as shown in Figure 1 d, the scanning electron microscope of graphene conductive coating
Collection of illustrative plates is as shown in 1e.It can be seen that graphene is coated in potsherd matrix surface well from Fig. 1 d, and show that planarization is good.
It can be seen that graphene microchip is covered in matrix surface in a manner of tiling well from Fig. 1 e, efficiently led in order to be formed
Electric network, and then reach highly conductive property.The electric conductivity and caking property of graphene conductive coating made from the present embodiment one
As shown in table 1.The surface resistivity of the graphene conductive coating is 0.395~0.447 ohm as can be seen from Table 1, that is, is led
It is electrically fabulous.Force test method is combined using the surfaces ASTMD 3359-2002, it is found that the intersection in scribing line has the oil of part
Paint falls off, but the gross area that falls off is less than 1%, i.e. coating adhesion can reach 4B grades.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than the present invention is protected
The limitation of range is protected, although being explained in detail to the present invention with reference to preferred embodiment, those skilled in the art answer
Work as understanding, technical scheme of the present invention can be modified or replaced equivalently, without departing from the reality of technical solution of the present invention
Matter and range.
Claims (10)
1. a kind of preparation method of the graphene conductive slurry of high temperature bond performance, which is characterized in that include the following steps：
（1）It is respectively that the thickener of the antifoaming agent of 1 ~ 5 wt.% and 1 ~ 5 wt.% is molten by magnetic agitation under the conditions of 60 ~ 80 DEG C
In terpinol；
（2）Under the conditions of 60 ~ 80 DEG C, by magnetic agitation, 1 ~ 2 wt.% dispersants, 1 ~ 3 wt.% are proportionally added successively
Levelling agent, 1 ~ 2 wt.% plasticizer, mixing time are 12 ~ 24 h, obtain the organic carrier phase of the electrocondution slurry；
（3）The organic carrier for weighing certain mass is mutually placed in vacuum stirring kettle, in the condition of 200 ~ 500 r/min stirring at low speed
Under, uniformly mixed graphene powder and glass powder with low melting point, addition graphene, organic carrier and glass are then added in batches
The mass ratio of powder is 40 ~ 65:25~55:5~10；
（4）It is 120 ~ 160 DEG C that above-mentioned tentatively uniformly mixed presoma, which is placed in temperature, and vacuum degree is that the constant temperature of -0.1Mpa is true
In empty baking oven, 1 ~ 2 h is heated, maturation process is carried out to presoma；
（5）Presoma after above-mentioned curing is placed in the de-airing mixer that vacuum degree is -0.1 Mpa with 500 ~ 1500 r/
The rotating speed of min persistently stirs 24 ~ 72 h, you can obtains the graphene conductive slurry of stable dispersion.
2. according to the method described in claim 1, the graphene is prepared by liquid phase ultrasound stripping method.
3. according to the method described in claim 1, the antifoaming agent is tributyl phosphate.
4. according to the method described in claim 1, the thickener is ethyl cellulose.
5. according to the method described in claim 1, the dispersant be selected from silane coupling agent or titanate coupling agent, further it is excellent
It is selected as silane coupling agent.
6. according to the method described in claim 1, the levelling agent is selected from dimethicone or butyl cellosolve.
7. according to the method described in claim 1, the plasticizer is selected from dibutyl phthalate.
8. a kind of graphene conductive slurry is prepared by claim 1-7 any one of them methods.
9. a kind of preparation method of graphene conductive coating, includes the following steps：
（1）Electrocondution slurry according to any one of claims 8 is uniformly coated into matrix surface in a manner of drop coating, control coated area is 2.5
×2.5 cm2；
（2）The matrix for having coated electrocondution slurry is placed in the Muffle furnace that temperature is 350 ~ 450 DEG C, is sintered 0.5 ~ 2 h, you can
To the matrix for covering conductive coating.
10. preparation method according to claim 9, described matrix is potsherd.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110401990A (en) * | 2019-01-13 | 2019-11-01 | 北京烯研科技有限公司 | A kind of high-efficiency heat conduction graphene Far infrared heating membrane and preparation method thereof |
| CN110798915A (en) * | 2019-11-09 | 2020-02-14 | 王成斌 | High temperature resistance graphite alkene hot plate |
| CN110818379A (en) * | 2018-08-11 | 2020-02-21 | 中环海化(厦门)船舶智能涂料有限公司 | Graphene slurry modified inorganic low-voltage heating coating for power battery |
| CN110964358A (en) * | 2019-11-29 | 2020-04-07 | 西安戴森电子技术有限公司 | Conductive coating and preparation method thereof |
| CN112646489A (en) * | 2020-12-22 | 2021-04-13 | 松山湖材料实验室 | Conductive coating and preparation method thereof |
| CN115732117A (en) * | 2022-03-08 | 2023-03-03 | 重庆恩辰新材料科技有限责任公司 | Conductive silver paste for ceramic surface circuit printing and preparation method and application thereof |
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| CN102664259A (en) * | 2012-05-02 | 2012-09-12 | 中国科学院宁波材料技术与工程研究所 | Method for preparing cathode material of lithium ion battery |
| CN106128553A (en) * | 2016-09-23 | 2016-11-16 | 苏州柏特瑞新材料有限公司 | A kind of high-performance Pb-free crystal silicon solar batteries back electrode silver slurry and preparation method thereof |
| CN106887271A (en) * | 2017-03-16 | 2017-06-23 | 西安晶晟光电科技有限公司 | Modified lead-free silver slurry of a kind of Graphene 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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| CN102664259A (en) * | 2012-05-02 | 2012-09-12 | 中国科学院宁波材料技术与工程研究所 | Method for preparing cathode material of lithium ion battery |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110818379A (en) * | 2018-08-11 | 2020-02-21 | 中环海化(厦门)船舶智能涂料有限公司 | Graphene slurry modified inorganic low-voltage heating coating for power battery |
| CN110401990A (en) * | 2019-01-13 | 2019-11-01 | 北京烯研科技有限公司 | A kind of high-efficiency heat conduction graphene Far infrared heating membrane and preparation method thereof |
| CN110401990B (en) * | 2019-01-13 | 2022-06-14 | 北京烯研科技有限公司 | Efficient heat-conducting graphene far-infrared heating film and preparation method thereof |
| CN110798915A (en) * | 2019-11-09 | 2020-02-14 | 王成斌 | High temperature resistance graphite alkene hot plate |
| CN110964358A (en) * | 2019-11-29 | 2020-04-07 | 西安戴森电子技术有限公司 | Conductive coating and preparation method thereof |
| CN112646489A (en) * | 2020-12-22 | 2021-04-13 | 松山湖材料实验室 | Conductive coating and preparation method thereof |
| CN115732117A (en) * | 2022-03-08 | 2023-03-03 | 重庆恩辰新材料科技有限责任公司 | Conductive silver paste for ceramic surface circuit printing and preparation method and application thereof |
| CN115732117B (en) * | 2022-03-08 | 2024-01-19 | 重庆恩辰新材料科技有限责任公司 | Conductive silver paste for ceramic surface circuit printing and preparation method and application thereof |
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Application publication date: 20180720 |