CN102786705A - Method for preparing graphene/polyaniline laminated films on basis of layer-by-layer self-assembly technique - Google Patents
Method for preparing graphene/polyaniline laminated films on basis of layer-by-layer self-assembly technique Download PDFInfo
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Abstract
The invention relates to a method for preparing graphene/polyaniline laminated films on basis of a layer-by-layer self-assembly technique and belongs to the technical field of composite material preparation. The method includes steps of treating a substrate; soaking the treated substrate in a graphene dispersing agent for a period; taking the substrate out of the graphene dispersing agent and cleaning the substrate with deionized water; soaking the cleaned substrate into polyaniline solution for a period and then taking out the substrate and cleaning the same again; and repeating the steps above to obtain uniform graphene-polyaniline laminated films having regular layer structures. The conductive graphene/polyaniline laminated films prepared by the method are uniform, regular and ultrathin and have controllable structures and properties. The method can be carried out with low-cost and simple equipment under mild conditions, and can be used for the fields of sensors, supercapacitors and the like.
Description
Technical field
The invention belongs to the Composite Preparation field, particularly relate to a kind of method for preparing the graphene/polyaniline laminated film based on layer-by-layer.
Background technology
In recent years, since the conductive film of conductive polymers because light weight, volume is little, conductivity is good and more and more come into one's own.
Graphene has particular structure and performances such as excellent electricity, calorifics, mechanics, successfully prepared since 2004, and be a research focus in the worldwide always.Compound having obtained of Graphene and conducting polymer paid close attention to widely; The long-range conjugated structure of polyaniline has been given its unique electricity and optical property; With Graphene and the compound Graphene-polyaniline composite material that obtains of polyaniline comprehensively Graphene and polyaniline performance characteristics and advantage separately, broad application prospect is all arranged in many application scenarios such as energy storage device, transmitter, diode, electrochromic devices.At present, the preparation of Graphene-polyaniline composite material often takes dual mode to prepare both at home and abroad: a kind of is chemical situ aggregation method, and a kind of in addition is electrochemical polymerization method.Preparation and performance study for Graphene-polyaniline composite material have all been made extensive work both at home and abroad; Yet also there are many deficiencies and shortcoming; No matter be to adopt chemical situ aggregation method or electrochemical polymerization method prepares Graphene-polyaniline composite material; The component concentration, arrangement mode and the compound degree that all are difficult to Graphene in the matrix material and polyaniline are controlled; Thereby be difficult to performance of composites is controlled, be difficult to from molecular level, matrix material designed and controlled preparation.Therefore, urgent need will develop a kind of new method, comes Graphene and polyaniline are carried out controlled orderly assembling and compound, realizes the regulation and control to Graphene-polyaniline composite material structure and performance, improves and expand to use in fact to be worth.
A kind ofly in recent years be called as " layer by layer " (Layer-by-Layer, LbL) technology of self-assembly has received increasing concern.The preparation method is simple for this technology; Need not complicated plant and instrument; Film forming does not receive the restriction of substrate sizes and shape, and filmogen is abundant, the having good stability of film, and can construction unit be assembled in a certain order; With composition structure, arrangement mode and the thickness of the horizontal controlling diaphragm of supramolecule, thereby the performance of resulting laminated film is controlled.If our imagination can be a structural unit with polyaniline and Graphene; Adopt layer-by-layer to be assembled into the orderly Graphene-polyaniline composite film of the construction structure of coming together to them; With the controlled orderly assembling that realizes grapheme material and polyaniline and compound; Overcome the shortcoming of existing Graphene-polyaniline composite material, further improve its performance and actual application value.Recently; The high congruent people of stone (Polymer, 2011,52; 5567) reported Graphene-polyaniline self-assembled film layer by layer; Yet the method that they adopt is to be assembled unit with graphene oxide and polyaniline, after being self-assembled into graphene oxide/polyaniline composite film layer by layer, this film is immersed in the reductive agent HI solution again graphene oxide is reduced into Graphene, thereby prepare the graphene/polyaniline composite package.This method is more loaded down with trivial details, and can all can impact the structure of self-assembled film layer by layer, performance etc. the reduction process of Graphene.Thereby need the direct easy method of a kind of comparison of development to solve the problems referred to above.
Summary of the invention
Problem to be solved by this invention provides a kind of method for preparing the graphene/polyaniline laminated film based on layer-by-layer; This method is an assembled unit with Graphene and polyaniline directly; Rely on electrostatic interaction that Graphene is assembled into polyaniline and form the graphene/polyaniline laminated film; The preparation method is simple; The thickness of the graphene/polyaniline composite package of gained and structure, performance etc. can both be controlled effectively, be expected to be used widely aspect transmitter, electrode and the ultracapacitor.
The present invention is based on a kind of layer-by-layer and prepare the method for graphene/polyaniline laminated film, comprising:
(1), the surface after the modification is had the Graphene of negative electricity and polyaniline that the surface has a positive charge and be dispersed in the dispersion liquid that preparation in the solvent is made into finite concentration, certain pH value;
(2), substrate is immersed in 10～40min in the polyaniline solutions, use a large amount of deionized water rinsings then, remove the unnecessary nano particle in surface, drying obtains the substrate of surperficial positively charged;
(3), the substrate of surperficial positively charged is immersed in Graphene dispersion liquid 10～40min, use a large amount of deionized water rinsings then, remove the unnecessary nano particle of substrate, drying obtains surperficial electronegative substrate;
(4), repeat above-mentioned step (2) and (3), thereby in substrate, prepare the graphene/polyaniline laminated film of a plurality of deposition cycle.
Be used for disposing Graphene that Graphene constructs the primitive dispersion liquid in the above-mentioned steps (1) for having carboxyl or sulfonic group, make its surface electronegative through regulating pH value, and the ability stable dispersion be in solvent through surface-treated.And polyaniline positively charged under acidic conditions, thereby Graphene and polyaniline assembled unit can rely on electrostatic interaction to mutually combine to be assembled into together.Thereby the pH value of Graphene dispersion liquid is between 5～14, and the pH value of polyaniline dispersion liquid is between 0～5, and their concentration is all between 0.01～100mg/mL.
The present invention compared with prior art, its remarkable advantage: (1) has overcome the resulting Graphene of prior art-polyaniline composite material bad dispersibility, is difficult for machine-shaping, to the back functional device construct and performance study has caused the problem of great difficulty; (2) this technology can well be controlled component concentration, arrangement mode and the compound degree of Graphene in the matrix material and polyaniline; Thereby can control performance of composites, can from molecular level, design and controlled preparation matrix material.(3) autonomous layer by layer packing technique cost is low, and mild condition is operated simple relatively.(4) laminated film of this technology preparation has good application prospects in fields such as transmitter, ultracapacitors.
Description of drawings
The uv-visible absorption spectra figure of the covalent modified graphene/polyaniline laminated film of Fig. 1.
Can find out from the uv-visible absorption spectra figure of covalent modified graphene/polyaniline laminated film: absorption peak is arranged at 270nm and 600～800nm; Can judge that Graphene and polyaniline assemble up; And increase along with the number of plies; Uv-absorbing is high more, and the increase along with the number of plies is described, composite package thickness is in continuous increase.Can find out the successfully assembling of modified graphene and polyaniline from uv-visible absorption spectra figure.
Embodiment
Below in conjunction with specific examples, further set forth the present invention.These instances only be used to the present invention is described and be not used in the restriction scope of the present invention.
Embodiment 1
The first step, with 10mg graphene oxide suspended dispersed in the 20mL ultrapure water. ultra-sonic dispersion 30min (S45D, 500W, 30% amplitude) obtains brown GO dispersion liquid.The ultrapure water of the dispersion liquid of gained and 20ml volume, the hydrazine hydrate solution of 1mL (85% massfraction), 70-145 μ L ammoniacal liquor (30% massfraction) is mixed in the flask of a 100mL.After firmly rocking or stirring several minutes, container is positioned in 95 ℃ the water-bath reaction 60min. reaction solution and is dialysing in the 0.5wt% ammoniacal liquor, is used for removing the superfluous hydrazine of residue dispersion liquid, and the surface that obtains 0.25mg/mL has the Graphene dispersion liquid of carboxyl.
In second step, the preparation of the polyaniline aqueous solution will prepare blackish green aniline and be dissolved in DMAC (N,N-DIMETHYLACETAMIDE), and preparation 120mg/mL solution stirs 48h, supersound process 8-10h then.The solution that filters preparation with 0.75 μ m filtering membrane removes some particles, with deionized water it is diluted to 0.25mg/mL.
The 3rd step was immersed in polyaniline water dispersion liquid 30min with the silicon chip after handling, and used a large amount of deionized water rinsings then, and drying obtains the substrate of surperficial positively charged.
In the 4th step, the substrate with above-mentioned surperficial positively charged is immersed in 30min in the Graphene solution then, uses a large amount of deionized water rinsings then, and drying obtains surperficial electronegative substrate.
The 5th step, repeat above-mentioned the 3rd step and with the 4th step repeatedly.
Embodiment 2
The first step is with 10mg graphene oxide suspended dispersed ultra-sonic dispersion 30min in the 20mL ultrapure water, with the Na of 5wt%
2CO
3Solution is regulated the graphene oxide pH value of solution to 9-10, adds sodium borohydride solution then, reacts 1h down at 80 ℃.Centrifuge washing is dispersed in again behind sonic oscillation and obtains the prereduction graphene oxide in the water for several times.Under condition of ice bath (0-5 ℃), the ice HCl solution mixing with 460mg Sulphanilic Acid and 0.66g1M adds an amount of frozen water and makes it to dissolve fully, slowly drips 15% NaNO then
2Solution.The aryl diazonium salts for preparing is added drop-wise in the prereduction graphene oxide solution of the first step preparation ice bath reaction 2h.Centrifuge washing is dispersed in the water behind sonic oscillation for several times again.To wherein adding Hydrazine Hydrate 80,100 ℃ are reacted 24h down then.Behind the centrifuge washing several, be dispersed in the water, regulating the pH value is 8, can obtain the surface and be with sulfonic Graphene dispersion liquid.
Second step is with second step of executing in the example 1.
The 3rd step was immersed in polyaniline water dispersion liquid 40min with the quartz substrate after modifying, and used a large amount of deionized water rinsings then, and drying obtains the substrate of surperficial positively charged.
In the 4th step, the substrate that will appeal surperficial positively charged then is immersed in 20min in the Graphene solution, uses a large amount of deionized water rinsings then, and drying obtains surperficial electronegative substrate.
The 5th step, repeat above-mentioned the 3rd step and with the 4th step repeatedly.
Claims (6)
1. one kind prepares the method for graphene/polyaniline laminated film based on layer-by-layer, it is characterized in that by the following steps preparation and gets:
(1), the Graphene and the polyaniline dispersion liquid of configuration finite concentration, certain pH value.
(2), the substrate after will handling is immersed in 5～40min in the polyaniline solutions, uses a large amount of deionized water rinsings then, drying, thus accomplish the preparation of a deposition cycle coating;
(3), the substrate of step (1) is immersed in 5～40min in the Graphene dispersion liquid again, use a large amount of deionized water rinsings then, drying obtains the substrate of surperficial positively charged;
(4), repeat above-mentioned step (2) and (3), obtain the graphene/polyaniline laminated film.
2. according to claim 1ly a kind ofly prepare the method for graphene/polyaniline laminated film, it is characterized in that in the step (1) that used Graphene has negative charge through surface-treated in the configuration Graphene dispersion liquid based on layer-by-layer.
3. according to claim 1ly a kind ofly prepare the method for graphene/polyaniline laminated film, it is characterized in that in the step (2) that polyaniline has positive charge through doping surfaces in the polyaniline dispersion liquid based on layer-by-layer.
4. according to claim 1ly a kind ofly prepare the method for graphene/polyaniline laminated film based on layer-by-layer, the concentration that it is characterized in that Graphene dispersion liquid and polyaniline dispersion liquid is 0.01～100mg/mL.
5. according to claim 1ly a kind ofly prepare the method for graphene/polyaniline laminated film based on layer-by-layer, the pH value that it is characterized in that the Graphene dispersion liquid is 5～14, and the pH value of polyaniline dispersion liquid is 0～5.
6. according to claim 1ly a kind ofly prepare the method for graphene/polyaniline laminated film, it is characterized in that substrate is opticglass, quartz, silicon single crystal, metal, Calcium Fluoride (Fluorspan) or plastics based on layer-by-layer.
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Application publication date: 20121121 |