CN104910398A - Nanocellulose-assisted preparation method of high-content graphene flexible conductive composite membrane - Google Patents
Nanocellulose-assisted preparation method of high-content graphene flexible conductive composite membrane Download PDFInfo
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Abstract
The invention aims to provide a nanocellulose-assisted preparation method of a high-content graphene flexible conductive composite membrane. The preparation method is characterized in that a low-content nanocellulose waterborne suspension is used to help disperse a graphene powder so as to obtain a uniform stable graphene/nanocellulose dispersion, and a flexible graphene composite membrane with graphene content up to 98 wt% and controllable mechanical property and conductivity can be prepared by a solvent evaporation method. The method is simple and low-cost, requires no complex equipment and is environmentally friendly. By the method, problems such as poor film-forming property of graphene, low strength, environmental pollution and the like existing in the prior art can be solved. In comparison with the prior art, the graphene membrane obtained by the method has advantages of good strength, controllable size and high conductivity.
Description
Technical field
The present invention relates to Graphene and nano-cellulose field, be specially a kind of dispersion with nano-cellulose and the conductive composite film of assisting that high-content graphene powder formation physical strength is high, flexibility is good.
Background technology
Graphene a kind ofly forms with sp2 hybridized orbital the two-dimensional material that hexangle type is honeycomb lattice by carbon atom.Because it has excellent electricity, calorifics and mechanical property, be expected to obtain application in fields such as nano electron device, transparent conductive film, matrix material, antistatic material, energy storage material and inductor blocks, thus become the new carbon got most of the attention after CNT (carbon nano-tube).
The special performance that Graphene has makes it have application prospect in novel flexible field of electrical components.Recent Graphene can large-scale production in a few countries, to expect to carry out its application as functional material.Grapheme conductive film is Graphene as closest to one of practical application, and thus production big area controllable grapheme film is the focus of current Graphene research field.Chemical Vapor deposition process prepares the most important method of graphene film, is one of the method preparing large size, high-quality graphene, can be compatible with existing semiconductor fabrication process.But the method apparatus expensive, substrate transfer process is complicated, and the electronic property of Graphene is very large by the impact of substrate.Also can obtain graphene film by SiC epitaxial growth method, but due to SiC crystal surface tissue comparatively complicated, be difficult to obtain the homogeneous Graphene of big area, thickness, and the bonding between Graphene and matrix can affect the characteristic of carbon-coating.
The graphene oxide powder dispersion of graphene powder stripping method obtained or reduction is at organic solvent (DMF, THF, N-methyl-2-pyrrolidone-NMP, Deng) or containing in the solution of tensio-active agent (Polyvinyl pyrrolidone – PVP), also can obtain graphene film by suction method.But graphene dispersing solution concentration is all lower, organic solvent has toxicity and environmental contamination etc. and is unfavorable for suitability for industrialized production.The graphite paper porous produced by pure graphene platelet, very fragile; But the graphite paper produced by the Graphene of dense oxide is then hard tough.Thus graphene oxide membrane also can be obtained conductivity and all good graphene film of mechanical property by heating or chemical reagent reduction, but there is a lot of defect in the Graphene that reduction method obtains, the reducing degree of the graphene film obtained with thermal reduction or chemical reduction graphene oxide is limited, very easily produce bubble in graphene film simultaneously, especially thermal reduction caudacoria can become more crisp, affects the final performance of film.Thus physical strength is developed and the good graphene film of snappiness is significant.
Recent research report adds the graphene oxide (~ 10wt.%) of trace graphite alkene or reduction to obtain composite and flexible transparent film in nano-cellulose matrix research.But adopt the method only to obtain for the purpose of flexible transparent film, mechanical properties strength is higher, but its Graphene content is lower, and thus specific conductivity is also lower.
Summary of the invention
The present invention adopts a kind of with low levels nano-cellulose waterborne suspension aid dispersion graphene powder, obtain uniform and stable graphene/nanometer Mierocrystalline cellulose dispersion liquid, Graphene content can be prepared up to 98wt.% and all controlled Flexible graphene composite membrane of mechanical property and conductivity by solvent evaporation method.
The invention provides a kind of method of assisting high, the flexible good conductive composite film of high-content graphene powder formation physical strength with nano-cellulose.Adopt the method can prepare the composite membrane of graphene/nanometer cellulose ratios up to 98:2, and the content of Graphene is adjustable in the wide range of 1-98%.Nano-cellulose, as natural polymer nano material, has mechanical property excellence, renewable, degradable, nontoxicity, becomes the very promising nano materials of field application such as food product pack, electronic product, biological medicine, cosmetics, matrix material.Due to nano-cellulose physical strength and film transparence high, snappiness is good, and thermal expansivity is low, has application prospect, thus develop its functional materials significant in the electron device product in future.
Of the present inventionly assist the method preparing high-content Graphene compliant conductive composite membrane with nano-cellulose, it is characterized in that: nano-cellulose powder is added to obtained nano-cellulose dispersion liquid in water (can be tap water, pure water, distilled water or deionized water etc.), graphene powder is added in nano-cellulose dispersion liquid, through stirring and obtain after supersound process the mixed solution of homodisperse nano-cellulose and Graphene, high-content Graphene compliant conductive composite membrane will be obtained after this mixed solution moisture evaporation.
Of the present inventionly assist the method preparing high-content Graphene compliant conductive composite membrane with nano-cellulose, it is characterized in that, the preparation method of described nano-cellulose powder is:
First be raw material with vegetable fibre, paraffin removal after aqueous slkali soaking, cleaning, drying, then carry out bleaching after cleaning, drying, obtain the cellulosic fibre that purity is higher; The fiber obtained is joined in concentrated sulfuric acid aqueous solution, under medium and low temperature heating condition, is aided with stirring is hydrolyzed process, then gained mixed solution is carried out centrifugal and clean, eventually pass lyophilize process and obtain nano-cellulose powder.
Of the present inventionly assist the method preparing high-content Graphene compliant conductive composite membrane with nano-cellulose, it is characterized in that: described lignocellulosic fiber source is agricultural crop straw, wood type, crudefiber crop or shell.
Of the present inventionly assist the method preparing high-content Graphene compliant conductive composite membrane with nano-cellulose, it is characterized in that, the preparation method of nano-cellulose dispersion liquid is: nano-cellulose powder is added in water, after at room temperature stirring, adopt supersound process that nano-cellulose powder is fully disperseed, obtain nano-cellulose dispersion liquid; Wherein nano-cellulose powder is added in water, make nano-cellulose powder concn be 0.1-0.5wt.%.
Of the present inventionly assist the method preparing high-content Graphene compliant conductive composite membrane with nano-cellulose, it is characterized in that: the power of supersound process equipment used is 100-1000W, treatment time 0.5-12h.
Of the present inventionly assist the method preparing high-content Graphene compliant conductive composite membrane with nano-cellulose, it is characterized in that, concrete steps are as follows:
(1), the preparation of nano-cellulose powder:
First be raw material with vegetable fibre, paraffin removal after aqueous slkali soaking, cleaning, drying, then carry out bleaching after cleaning, drying, obtain the cellulosic fibre that purity is higher; The fiber obtained is joined in concentrated sulfuric acid aqueous solution, is aided with stirring in a heated condition and is hydrolyzed process, then gained mixed solution is carried out centrifugal and clean, eventually pass lyophilize process and obtain nano-cellulose powder.
(2), the preparation of nano-cellulose and Graphene mixed solution:
Gained nano-cellulose powder is added in water, makes nano-cellulose powder concn be 0.1-0.5wt.%, at room temperature stir 0.5-12h, be aided with supersound process 0.5-12h simultaneously, plant capacity is 100-1000W, nano-cellulose powder is fully disperseed, obtains nano-cellulose dispersion liquid; Then in nano-cellulose dispersion liquid, add graphene powder, stir and supersound process 0.5-12h, plant capacity is 100-1000W, obtains the mixed solution of homodisperse nano-cellulose and Graphene;
(3), by the mixed solution of nano-cellulose and Graphene inject culture dish, after making moisture evaporation at not higher than the temperature of 100 degrees Celsius, obtain high-content Graphene compliant conductive composite membrane.
Beneficial effect of the present invention:
Selected nano-cellulose is natural polymer, and content is many on earth, distribution is wide for its starting material, and its raw material can be the stalk the like waste of wooden class, crudefiber crop, shell and farm crop.The own good mechanical property of nano-cellulose (Young's modulus 150G Pa, tensile strength 6GPa), surface is active large because being rich in hydroxy functional group, and has renewable, degradable, the advantage such as nontoxic, is eco-friendly Preen nono material.The suspension of nano-cellulose in water serves good dispersion, film forming and enhancement to graphene powder, the graphene powder (Graphene content is up to 98wt.%) of ancillary component a wider range can form complete membrane.Gained composite membrane physical strength and snappiness good, size is controlled, and conductivity is good.The method of the invention is simple, cost is low, without the need to complex apparatus, environmental friendliness, can solve that the Graphene film-forming properties existed in prior art is poor, intensity is low and the problem such as environmental pollution.Compared with prior art, the graphene film intensity that obtains of the method is good, size is controlled, specific conductivity is high.
Accompanying drawing explanation
Fig. 1 is Graphene, graphene/nanometer Mierocrystalline cellulose and the dispersion liquid of nano-cellulose in water;
Fig. 2 is the composite membrane of Graphene and nano-cellulose (Graphene and nano-cellulose ratio are 98:2), and diameter is 90mm.
Embodiment
Embodiment 1
Be illustrated in figure 2 graphene/nanometer cellulose composite membrane prepared by the present embodiment, wherein nano-cellulose is obtained by chemical hydrolysis flax fiber.0.02g nano-cellulose powder is added in the Erlenmeyer flask containing 20g water, to stir after 0.5h supersound process 0.5h under the power of 800W again, obtain the dispersion liquid (as shown in Figure 1) of nano-cellulose, then 0.98g graphene powder is added, by mixed solution under 100W power through supersound process 12h to being uniformly dispersed, then mixed solution is slowly poured in culture dish, and to be placed in temperature be that the loft drier inner drying of 80 DEG C all volatilizees to moisture, then film is taken off from culture dish and can obtain the composite membrane that Graphene content is 98wt.%, the specific conductivity of this composite membrane is 198S/cm.
Embodiment 2
Graphene/nanometer cellulose composite membrane prepared by the present embodiment, wherein nano-cellulose is obtained by chemical hydrolysis wood pulp cellulose.0.05g nano-cellulose powder is added in the Erlenmeyer flask containing 50g water, to stir after 0.5h supersound process 0.5h under the power of 800W again, obtain the dispersion liquid of nano-cellulose, then 0.95g graphene powder is added, stir this mixed solution under 100W power through supersound process 10h, then mixed solution is slowly poured in culture dish, and to be placed in temperature be that the loft drier inner drying of 60 DEG C all volatilizees to moisture, then taken off from culture dish by film and can obtain the composite membrane that Graphene content is 95wt.%, the specific conductivity of composite membrane is 185S/cm.
Embodiment 3
Graphene/nanometer cellulose composite membrane prepared by the present embodiment, wherein nano-cellulose is obtained by chemical hydrolysis shinyleaf yellowhorn fruit shell fiber.0.1g nano-cellulose powder is added in the Erlenmeyer flask containing 100g water, to stir after 12h supersound process 12h under the power of 100W again, obtain the dispersion liquid of nano-cellulose, then 0.9g graphene powder is added, stir this mixed solution under 800W power through supersound process 2h, then mixed solution is slowly poured in culture dish, and to be placed in temperature be that the loft drier inner drying of 40 DEG C all volatilizees to moisture, then taken off from culture dish by film and can obtain the composite membrane that Graphene content is 90wt.%, the specific conductivity of composite membrane is 169S/cm.
Embodiment 4
Graphene/nanometer cellulose composite membrane prepared by the present embodiment, wherein nano-cellulose is obtained by chemical hydrolysis rice straw fiber.0.9g nano-cellulose powder is added in the Erlenmeyer flask containing 450g water, to stir after 6h supersound process 6h under the power of 100W again, obtain the dispersion liquid of nano-cellulose, then 0.1g graphene powder is added, stir this mixed solution under 1000W power through supersound process 0.5h, then mixed solution is slowly poured in culture dish, and to be placed in temperature be that the loft drier inner drying of 100 DEG C all volatilizees to moisture, then taken off from culture dish by film and can obtain the composite membrane that Graphene content is 10wt.%, the specific conductivity of composite membrane is 11.6S/cm.
Embodiment 5
Graphene/nanometer cellulose composite membrane prepared by the present embodiment, wherein nano-cellulose is obtained by chemical hydrolysis shinyleaf yellowhorn fruit shell fiber.0.5g nano-cellulose powder is added in the Erlenmeyer flask containing 100g water, to stir after 12h supersound process 12h under the power of 100W again, obtain the dispersion liquid of nano-cellulose, then 0.5g graphene powder is added, stir this mixed solution under 1000W power through supersound process 1h, then mixed solution is slowly poured in culture dish, and to be placed in temperature be that the loft drier inner drying of 40 DEG C all volatilizees to moisture, then taken off from culture dish by film and can obtain the composite membrane that Graphene content is 50wt.%, the specific conductivity of composite membrane is 89S/cm.
Above-described embodiment, only for technical conceive of the present invention and feature are described, its object is to person skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences done according to spirit of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (7)
1. assist the method preparing high-content Graphene compliant conductive composite membrane with nano-cellulose for one kind, it is characterized in that: nano-cellulose powder is added to obtained nano-cellulose dispersion liquid in water, graphene powder is added in nano-cellulose dispersion liquid, through stirring and obtain after supersound process the mixed solution of homodisperse nano-cellulose and Graphene, high-content Graphene compliant conductive composite membrane will be obtained after this mixed solution moisture evaporation.
2. according to assisting the method preparing high-content Graphene compliant conductive composite membrane described in claim 1 with nano-cellulose, it is characterized in that, the preparation method of described nano-cellulose powder is:
First be raw material with vegetable fibre, paraffin removal after aqueous slkali soaking, cleaning, drying, then carry out bleaching after cleaning, drying, obtain the cellulosic fibre that purity is higher; The fiber obtained is joined in concentrated sulfuric acid aqueous solution, is aided with stirring in a heated condition and is hydrolyzed process, then gained mixed solution is carried out centrifugal and clean, eventually pass lyophilize process and obtain nano-cellulose powder.
3. according to assisting the method preparing high-content Graphene compliant conductive composite membrane described in claim 2 with nano-cellulose, it is characterized in that: the source of described vegetable fibre is agricultural crop straw, wood type, crudefiber crop or shell.
4. according to assisting the method preparing high-content Graphene compliant conductive composite membrane described in claim 1 with nano-cellulose, it is characterized in that, the preparation method of nano-cellulose dispersion liquid is: nano-cellulose powder is added in water, after at room temperature stirring, adopt supersound process that nano-cellulose powder is fully disperseed, obtain nano-cellulose dispersion liquid; Wherein nano-cellulose powder is added in water, make nano-cellulose powder concn be 0.1-0.5wt.%.
5. according to assisting the method preparing high-content Graphene compliant conductive composite membrane described in claim 1 with nano-cellulose, it is characterized in that: the power of supersound process equipment used is 100-1000W, treatment time 0.5-12h.
6., according to assisting the method preparing high-content Graphene compliant conductive composite membrane described in claim 1 with nano-cellulose, it is characterized in that, concrete steps are as follows:
(1), the preparation of nano-cellulose powder:
First be raw material with vegetable fibre, paraffin removal after aqueous slkali soaking, cleaning, drying, then carry out bleaching after cleaning, drying, obtain the cellulosic fibre that purity is higher; The fiber obtained is joined in concentrated sulfuric acid aqueous solution, is aided with stirring in a heated condition and is hydrolyzed process, then gained mixed solution is carried out centrifugal and clean, eventually pass lyophilize process and obtain nano-cellulose powder.
(2), the preparation of nano-cellulose and Graphene mixed solution:
Gained nano-cellulose powder is added in water, makes nano-cellulose powder concn be 0.1-0.5wt.%, at room temperature stir 0.5-12h, be aided with supersound process 0.5-12h simultaneously, plant capacity is 100-1000W, nano-cellulose powder is fully disperseed, obtains nano-cellulose dispersion liquid; Then in nano-cellulose dispersion liquid, add graphene powder, stir and supersound process 0.5-12h, plant capacity is 100-1000W, obtains the mixed solution of homodisperse nano-cellulose and Graphene;
(3), by the mixed solution of nano-cellulose and Graphene inject culture dish, after making moisture evaporation at not higher than the temperature of 100 degrees Celsius, obtain high-content Graphene compliant conductive composite membrane.
7. according to assisting the method preparing high-content Graphene compliant conductive composite membrane described in claim 1 with nano-cellulose, it is characterized in that: described water is tap water, pure water, distilled water or deionized water.
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