CN107103962A - A kind of preparation method of graphene film conductive material - Google Patents
A kind of preparation method of graphene film conductive material Download PDFInfo
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- CN107103962A CN107103962A CN201710384175.0A CN201710384175A CN107103962A CN 107103962 A CN107103962 A CN 107103962A CN 201710384175 A CN201710384175 A CN 201710384175A CN 107103962 A CN107103962 A CN 107103962A
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- graphene
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- conductive material
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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
- 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
Abstract
The invention discloses a kind of preparation method of graphene film conductive material, the preparation method includes：1）Prepare tentatively scattered graphene dispersing solution；2）Prepare the alkali-activated carbonatite solution of graphene dispersion；3）Prepare compound geopolymer powder；4）Prepare the first conductive geopolymer；5）Prepare the intrinsic microporous polymer of second polymer (PIM)；6）First polymer and second polymer film forming is blended.Based on graphene and intrinsic microporous polymer (PIM), conducting membrane material is prepared.Obtain excellent conductive performance, mechanical property simultaneously, take into account gas permeability.
Description
Technical field
The present invention relates to conducting function membrane material, relate more specifically to a kind of preparation method of graphene film conductive material.
Background technology
Graphene is two-dimentional carbon nano-structured material, and by its larger specific surface area, lighter weight, intensity is higher to wait special
Point so that when graphene has been broken in tradition using graphite as filler, the bottleneck that consumption is higher but performance is relatively low.Graphene is being led
Application in electricity, heat conduction, anti-corrosion, antistatic, fire-retardant and other field of functional coatings oneself through tentatively achieving some achievements.
Graphene possesses a series of unique physics and chemical characteristic, wherein most prominent is his electronic effect.Graphite
Alkene is the material for having now been found that resistivity is minimum, and it possesses very high electron mobility.Conventional electrically-conducting paint passes through addition
Conductive material makes film conductive, wherein main to add silver powder, copper powder, based on zinc oxide, wherein effect most preferably silver powder,
But silver powder is prohibitively expensive therefore can not be used widely.Compared with silver powder, graphene is except with excellent electric conductivity
Can be outer, mechanical performance, hot property etc. also show excellent, are good electrically-conducting paint additives, will start the new of electrically-conducting paint
Epoch.
The graphene/silicon acrylic emulsion composite coating of the preparations such as huge great ripple possesses relatively low percolation threshold, and (mass fraction is
0.5%), when the consumption of graphene is more than 0.9%, its electric conductivity, which there has also been, to be obviously improved.
Huang Kun etc. is using graphene powder as filler, and it is conductive that epoxy E-44 have developed a kind of epoxy composite anti-corrosion as base-material
Coating, when adding the amount of graphene 1% or so, this composite coating possesses relatively stable electric conductivity, and preferably anti-corrosion
Performance, adhesive force is also showed well, can be applied as a kind of new static conductive anticorrosive paint.
Graphene film is distributed in photo curable SU-8 resins by Sangermano etc., and research finds graphene filler pair
The mobility of polymer chain has stopping effect.When the mass fraction of functionalized graphite's alkene piece (FGS) in composite is 3%-
When 4%, the electric conductivity of coating can be significantly improved.
In existing achievement in research and open source literature, not yet find be with graphene and intrinsic microporous polymer (PIM)
Basis, prepares conducting membrane material, while ensureing the method for its electric conductivity and mechanical property.
The content of the invention
1st, goal of the invention.
The present invention proposes a kind of preparation method of graphene film conductive material, with graphene and intrinsic microporous polymer
(PIM) based on, it is ensured that its electric conductivity, mechanical property, its gas permeability is also ensured.
2nd, the technical solution adopted in the present invention.
A kind of preparation method of graphene film conductive material proposed by the present invention, its preparation process includes：1) prepare preliminary
Scattered graphene dispersing solution；2) the alkali-activated carbonatite solution of graphene dispersion is prepared；3) compound geopolymer powder is prepared；4)
Prepare the first conductive geopolymer；5) the intrinsic microporous polymer of second polymer is prepared；6) first polymer and second is blended
Polymer film forming.
Wherein step 1）：Graphene, polyvinylpyrrolidone and water are pressed 1：(0.1-0.5)：The weight of (4-6) is than mixed
Close, grinding, scattered tentatively scattered graphene dispersing solution.
Wherein step 2)：By alkali metal silicate solutions and step 1) in obtained graphene dispersing solution by 1：(0.05-
0.3) weight is stirring evenly and then adding into the 0.05-1% of above-mentioned mixed liquor gross weight Sodium Polyacrylate than mixing, grinds, divides
Dissipate graphene dispersion alkali-activated carbonatite solution, the moduluses of the alkali metal silicate solutions is 1-4, and solid content is 30-60%.
Wherein step 3)：Sa raw material and granulated blast-furnace slag are pressed 1：The weight of (0.1-0.2) is than mixing, after grinding
Produce compound geopolymer powder.
Wherein step 4)：By step 3) in obtained compound geopolymer powder and step 2) in obtained graphene dispersion
Alkali-activated carbonatite solution with 1：The weight ratio of (1.1-2.5) is mixed evenly, and produces conductive geopolymer.
Wherein step 5):Intrinsic microporous polymer (PIM) have combined with contortion site based on dibenzodioxin alkane
The repeat unit of trapezoidal-structure, contortion site can be the site with spiral shell center or high steric-hindrance amino；PIM structure prevents intensive chain
Filling, so as to produce sizable accessible free volume, it is ensured that its gas permeability.
Wherein step 6):By step 4) and step 5）In two kinds of polymer be dissolved in or aaerosol solution in, solution can be
Deposited on substrate and drying form film, film is conserved 5-15 days under 15-25 DEG C of environment temperature, 85-95% ambient humidities, it is ensured that
Its mechanical property.
3rd, the technique effect produced by the present invention.
The present invention passes through many experiments, draws preparation technology and the proportioning, with graphene and intrinsic microporous polymer
(PIM) based on, conducting membrane material is prepared, excellent conductive performance, mechanical property is being obtained simultaneously, is taking into account gas permeability.
Brief description of the drawings
Fig. 1 is the intrinsic microporous polymer structure unit in embodiment 1.
Embodiment
Embodiment
1) tentatively scattered graphene dispersing solution is prepared.It is 1.2nm to take thickness, and extension size is 4 μm, the matter of oxygen
The graphene 110g that content is 20% is measured, polyvinylpyrrolidone 22g and water 440g are separately taken, by 1:0.2 ：4 weight is than mixed
Close, be placed in grinding distribution 1 in the nanometer sand mill that grinding aid medium is high-strength glass pearl, grinding rotating speed is 2000 revs/min small
When, it is placed in the high frequency ultrasound dispersion machine sonic oscillation that vibration frequency is 50kHZ again afterwards and disperses 30 minutes, is tentatively disperseed
Graphene dispersing solution.
2) the alkali-activated carbonatite solution of graphene dispersion is prepared.It is 2.2 to take silicon modulus, and solid content is 50% liquid sodium silicate
Solution 2200g, tentatively scattered graphene dispersing solution 550g, by 1:0.25 weight is than mixing, stirring, then into mixed solution
Add the 0.08% Sodium Polyacrylate 2.2g for accounting for mixed solution weight.It is again placed in grinding distribution 1 in foregoing nanometer sand mill
Hour, ultrasonic vibration is scattered 3 minutes in high frequency ultrasound dispersion machine, produces the alkali-activated carbonatite solution of graphene dispersion.
3) compound geopolymer powder is prepared.It is 0.1-10 μm, the higher ridge through 900 DEG C of high-temperature calcinations to take particle size
Native 1000g, by the Class F fly ash of 0.1-10 μm of itself and 400g particle sizes and 280g S105 level granulated blast-furnace slags with
1：0.4：0.28 weight is than mixing, and the ground and mixed 2 hours in rotating speed is 400 revs/min of planetary ball mill is produced multiple
Close geopolymer powder.
4) the first conductive geopolymer is prepared.Take step 3) in obtained 1000g be combined geopolymer powder, step 2）
In the obtained alkali-activated carbonatite solution of 2200g graphene dispersions, with 1：2.2 weight is than mixing, with 40 in high-shear impeller
Rev/min stirring at low speed mix 6 minutes after, then switch to and stir 5 minutes with 600 revs/min of high shear mode, i.e.,
Obtain the conductive geopolymer that graphene is modified.
5) the selection intrinsic microporous polymer of second polymer (PIM).With being combined with contortion site based on dibenzo two
The repeat unit of the trapezoidal-structure of oxane, contortion site can be the site with spiral shell center or high steric-hindrance amino.PIM structure prevents close
The chain filling of collection, so as to produce sizable accessible free volume and high gas permeability.PIM construction units such as Fig. 1 institutes
Show, wherein n is the integer that can be changed as needed.N is typically larger than 1 or more than 5, and usually 10 to 10000 or 10 to
1000 or 10 to 500.
6) blending first polymer and second polymer film forming.10 are conserved under 20 DEG C of environment temperatures, 90% ambient humidity
My god.
It is about 50-70 Ω .m to measure resistivity, and cubic compressive strength is about 40-44MPa, it is ensured that graphene film is conductive
The electric conductivity and mechanical property of material, and taken into account its gas permeability.
Claims (7)
1. a kind of preparation method of graphene film conductive material, it is characterised in that：Including preparation process：1) prepare preliminary scattered
Graphene dispersing solution；2) the alkali-activated carbonatite solution of graphene dispersion is prepared；3) compound geopolymer powder is prepared；4) prepare
First conductive geopolymer；5) the intrinsic microporous polymer of second polymer is prepared；6) blending first polymer and the second polymerization
Thing film forming.
2. a kind of preparation method of graphene film conductive material according to claim 1, it is characterised in that：By graphene,
Polyvinylpyrrolidone presses 1 with water：(0.1-0.5)：The weight of (4-6) is ground, disperseed than mixing, so as to prepare preliminary scattered
Graphene dispersing solution.
3. a kind of preparation method of graphene film conductive material according to claim 1, it is characterised in that：By alkali metal silicon
Acid salt solution and step 1) in obtained graphene dispersing solution by 1：The weight of (0.05-0.3) is stirring evenly and then adding into than mixing
The 0.05-1% of above-mentioned mixed liquor gross weight Sodium Polyacrylate, grinding, the alkali-activated carbonatite solution of scattered graphene dispersion are described
The modulus of alkali metal silicate solutions is 1-4, and solid content is 30-60%.
4. a kind of preparation method of graphene film conductive material according to claim 1, it is characterised in that：Sa is former
Material presses 1 with granulated blast-furnace slag：The weight of (0.1-0.2) produces compound geopolymer powder than mixing after grinding.
5. a kind of preparation method of graphene film conductive material according to claim 1, it is characterised in that：By step 3) in
Obtained compound geopolymer powder and step 2) in the obtained alkali-activated carbonatite solution of graphene dispersion with 1：The weight of (1.1-2.5)
Amount ratio is mixed evenly, and produces conductive geopolymer.
6. a kind of preparation method of graphene film conductive material according to claim 1, it is characterised in that：Intrinsic micropore gathers
Compound (PIM) has the repeat unit of the trapezoidal-structure based on dibenzodioxin alkane combined with contortion site, and contortion site can
For the site with spiral shell center or high steric-hindrance amino；PIM structure prevents intensive chain filling, so as to produce sizable accessible
Free volume.
7. a kind of preparation method of graphene film conductive material according to claim 1, it is characterised in that：By step 4) and
Step 5）In two kinds of polymer be dissolved in or aaerosol solution in, solution can be deposited on substrate and drying forms film, and film is existed
Conserved 5-15 days under 15-25 DEG C of environment temperature, 85-95% ambient humidities.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108275673A (en) * | 2018-04-07 | 2018-07-13 | 蒋黎婷 | A kind of preparation method of high-performance porous graphene film |
| CN111018414A (en) * | 2019-11-26 | 2020-04-17 | 东华大学 | Electromagnetic shielding geopolymer composite material and preparation and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102112203A (en) * | 2008-07-02 | 2011-06-29 | 环球油品公司 | Mixed matrix membranes incorporating microporous polymers as fillers |
| CN105218004A (en) * | 2015-09-17 | 2016-01-06 | 浙江大学 | A kind of preparation method of polymkeric substance conductively |
| US20160243525A1 (en) * | 2016-05-02 | 2016-08-25 | LiSo Plastics, L.L.C. | Multilayer Polymeric Membrane and Process |
-
2017
- 2017-05-26 CN CN201710384175.0A patent/CN107103962A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102112203A (en) * | 2008-07-02 | 2011-06-29 | 环球油品公司 | Mixed matrix membranes incorporating microporous polymers as fillers |
| CN105218004A (en) * | 2015-09-17 | 2016-01-06 | 浙江大学 | A kind of preparation method of polymkeric substance conductively |
| US20160243525A1 (en) * | 2016-05-02 | 2016-08-25 | LiSo Plastics, L.L.C. | Multilayer Polymeric Membrane and Process |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108275673A (en) * | 2018-04-07 | 2018-07-13 | 蒋黎婷 | A kind of preparation method of high-performance porous graphene film |
| CN111018414A (en) * | 2019-11-26 | 2020-04-17 | 东华大学 | Electromagnetic shielding geopolymer composite material and preparation and application thereof |
| CN111018414B (en) * | 2019-11-26 | 2022-08-19 | 东华大学 | Electromagnetic shielding geopolymer composite material and preparation and application thereof |
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Application publication date: 20170829 |