CN105461948A - Preparation method of conductive macromolecule non-covalent functionalized graphene modified electrokinetic energy conversion polymer material - Google Patents
Preparation method of conductive macromolecule non-covalent functionalized graphene modified electrokinetic energy conversion polymer material Download PDFInfo
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Abstract
The invention discloses a preparation method of a conductive macromolecule non-covalent functionalized graphene modified electrokinetic energy conversion polymer material. according to the method, conductive macromolecules are non-covalent functionalized onto the surface of nano-graphene; and then, the conductive macromolecule non-covalent functionalized graphene nano-material undergoes ultrasonic-assisted dispersion into an electrokinetic energy conversion polymer solution so as to finally obtain a conductive macromolecule non-covalent functionalized graphene/electrokinetic energy conversion polymer composite material. The electro-stimulate response intelligent polymer composite material obtained by the method has high dielectric constant and high electrodeformation value. When content of poly(3,4-ethylenedioxythiophene): polystyrolsulfon acid non-covalent functionalized graphene nanofiller is 3%, dielectric constant of the modified polyurethane dielectric elastomer intelligent material reaches up to 350 at room temperature and at the frequency of 1000 Hz, dielectric loss is 0.20, and loss modulus is 200 MPa. Under the action of a 32.2 MV/m electric field, electrodeformation value in the thickness direction reaches 162%. Performance of the material provided by the invention is far more excellent than performance of a regular nano-ceramic or nano-conductive filler modified intelligent polymer composite material.
Description
Technical field
The present invention relates to stimuli responsive intelligent macromolecule field of compound material, be specifically related to the method for conducting polymer non-covalent modification Graphene modification electric energy conversion polymer materials.
Background technology
Electric energy conversion polymer materials is the novel flexible intelligent material that a class can produce significantly size or change in shape under electric field excitation, there is electric energy-mechanic energy conversion characteristic, become the research object that the front line science such as flexible mechanical and soft material science and technical development field are shown great attention in recent years gradually, at driving mechanism performer, audio frequency and sonac, biomedical sensor, electromechanical transducer and energy collecting device, robot, microelectromechanical-systems and artificial-muscle etc. are multi-field has a wide range of applications.Compared with the functional materials such as electroactive pottery, shape memory alloy, electric energy conversion polymkeric substance has that distortion is large, electomechanical response performance is high, it is rapid, low in energy consumption to respond, quality is light, fracture toughness property is high, manufacturing process is simple and can be made into numerous good characteristics such as different shape.But this kind of intelligent macromolecule material with data-collection function has lower specific inductivity, therefore usually need higher excitation electrical field could produce high electroluminescent deformation, this greatly limits its application.The specific inductivity of pure polymkeric substance is generally lower and Improvement is limited, adopts Nano filling to carry out the function modified important method becoming the high dielectric of preparation and high electroluminescent deformation intelligent macromolecule matrix material to it in recent years.High-k nano ceramics is as barium titanate, Pb-based lanthanumdoped zirconate titanatess etc. are used to prepare high dielectric intelligent macromolecule matrix material (K.S.Lam, Y.Zhou, Y.W.Wong, F.G.Shin.Electrostrictionofleadzirconatetitanate/polyure thanecomposites.JournalofAppliedPhysics2005, 97, 104112.) (Wu Jianfeng, Li Jianqing, Song Aiguo, woods is kept tie, Cong Yuqi, Huang Weisheng. polyurethane elastomer electrostrictive properties. Southeast China University's journal, 2008, 38 (3): 439-443), the advantage of this kind of matrix material has regulatable electrical property, good temperature stability and preparation technology simple, but the prominent question using this type of material to occur obtains ceramic filler amount large (>50%) needed for high dielectric, the existence of flexible polymer substrate middle and high concentration rigidity brittle ceramic filler makes the manufacturing process of material and mechanical property sharply worsen.
This New Two Dimensional nano-carbon material of Graphene just continues to become study hotspot since coming out, and the performance of its excellence is that the high dielectric intelligent macromolecule matrix material of preparation provides excellent opportunity.Theory is oozed according to exceeding, the specific inductivity of the polymer matrix composite that conducting particles is filled can significantly improve when filler content reaches near percolation threshold, and percolation threshold filler content very little (<5%), the graphene nanometer sheet of high conductivity is desirable conductive filler material, but graphene nanometer sheet surfaces hydrophobic state, and there is stronger Van der Waals force between graphene sheet layer and lamella, easy generation is reunited, thus conductive channel is formed in electric energy conversion polymer materials matrix, the dielectric loss of material and out-of-phase modulus is caused sharply to increase, electric breakdown strength reduces, thus limit the application of material.Therefore when preparing Graphene modification electric energy conversion polymer composites, in order to improve dispersiveness, wetting property and the consistency of Graphene in electric energy conversion polymeric matrix, obtain the Electro-stimulate response intelligent macromolecule matrix material of excellent performance, chemically modified must be carried out to Graphene.
Summary of the invention
The problem to be solved in the present invention is to provide the preparation method of a kind of conducting polymer non-covalent modification Graphene modification electric energy conversion polymer materials, and the matrix material obtained according to the method has high-k, low-dielectric loss, low-loss modulus and high electroluminescent deformation value.
The preparation method of a kind of conducting polymer non-covalent modification Graphene modification electric energy conversion polymer materials disclosed by the invention, comprises the following steps:
1) method of evaporation induced self-assembly or the method for in-situ polymerization is adopted to carry out conducting polymer non-covalent modification Graphene.
Described conductive polymers comprises poly-(3,4-ethylene dioxythiophene): the one in polystyrolsulfon acid, polyaniline, polypyrrole, Polythiophene.
Wherein gather (3,4-ethylenedioxy thiophene): polystyrolsulfon acid is dissolvable in water water, commercial goods poly-(3,4-ethylenedioxy thiophene): polystyrolsulfon acid is solid content 1.4% aqueous solution, this aqueous solution is carried out after dilute hydrochloric acid adulterates in right amount, adopt the method for evaporation induced self-assembly to be mixed with in deionized water poly-(3,4-ethylene dioxythiophene) with Graphene according to different mass ratio: polystyrolsulfon acid non-covalent modification Graphene.Specifically, by conductive polymers and graphene dispersion in deionized water, 6 ~ 12h is stirred under ultrasonic wave added, then mixing solutions is poured on the smooth silica glass in bottom surface, be placed in loft drier and carry out evaporation induced self-assembly 12 ~ 48h under 35 ~ 60 DEG C of low temperature, obtain conducting polymer non-covalent modification graphene nano material.
Polyaniline, polypyrrole and Polythiophene are insoluble or be insoluble in water, and the method that must aniline, pyrroles and thiophene monomer be adopted on graphene sheet layer to carry out in-situ polymerization obtains electrically conductive polyaniline, polypyrrole and Polythiophene non-covalent modification graphene nano material.
The method of in-situ polymerization, specifically, by aniline, pyrroles and thiophene monomer respectively according to certain mass ratio and graphene uniform mixing, then ultrasonic disperse 4 ~ 12h at ice-water bath 0 DEG C is placed in, then the dilute hydrochloric acid adding 1M continues ultrasonic disperse 1 ~ 2h, the hydrochloric acid soln initiated polymerization of slow dropping ammonium persulphate, react 10 ~ 24h at keeping 0 DEG C, be separated after reaction and obtain solid and be placed in vacuum drying oven 40 ~ 60 DEG C of drying 12 ~ 48h and namely obtain polyaniline, polypyrrole and Polythiophene non-covalent modification graphene nano material.
2) conducting polymer non-covalent modification graphene nano material ultrasonic wave added is dispersed in electric energy conversion polymers soln, adopts solution film casting method to prepare conducting polymer non-covalent modification Graphene electric energy conversion polymer composites; Specifically, first electric energy is changed polymer materials fully to stir at 50 ~ 80 DEG C, be dissolved in N completely, solution A is formed in dinethylformamide (DMF) solvent, take the non-covalent modification graphene nano functional stuffing with polymer materials certain mass ratio (mass percent is less than 5.0%) in addition respectively, ultrasonic disperse forms B solution in DMF solvent system; Then finely dispersed B solution slowly added in solution A, ultrasonic wave added stirs 4 ~ 8h, obtains mixture, mixture is positioned over refrigerator and cooled degassed process; Finally mixture is poured on smooth silica glass, leave standstill 15 ~ 30min, be placed in vacuum drying oven 60 ~ 80 DEG C of air set 20 ~ 30h, under 50 ~ 75 DEG C of vacuum, 12 ~ 18h is incubated for removing DMF solvent further, 130 DEG C of annealing 3 ~ 5h, take off the electric energy conversion polymer composites namely obtaining modification by the macromolecule membrane on silica glass.
Described electric energy changes that polymkeric substance is urethane dielectric elastomer, silicone dielectric elastomerics, vinylformic acid dielectric elastomer, poly(vinylidene fluoride) and multipolymer thereof any one.
Wherein polyvinylidene fluoride copolymers thing be poly(vinylidene fluoride)-trifluoro-ethylene copolymer, poly(vinylidene fluoride)-trifluoro-ethylene-chlorine fluoride copolymers any one.
The conducting polymer non-covalent modification Graphene electric energy conversion polymer composites utilizing the method to prepare has high-k and high electroluminescent deformation value, wherein gather (3, 4-ethylenedioxy thiophene): when polystyrolsulfon acid non-covalent modification graphene nano filler content is 3%, under modified polyurethane dielectric elastomer intelligent material room temperature and 1000Hz frequency, specific inductivity is up to 350, dielectric loss is 0.20, out-of-phase modulus is 200MPa, under 32.2MV/m electric field action, thickness direction electroluminescent deformation value reaches 162%, performance is far above common nano ceramics or the filler modified intelligent macromolecule matrix material of conductive nano.
Preparation method of the present invention by conducting polymer non-covalent modification on graphene nano lamella, drastically increase dispersiveness, wetting property and the consistency of Graphene in electric energy conversion polymeric matrix, thus make easily to form more micro-capacitance structure in intelligent macromolecule matrices of composite material, and the conductivity utilizing conductive polymers good can play the synergy of conductive polymers and Graphene especially, thus improve the specific inductivity of electric energy conversion polymer materials.Dielectric buffer layer can be served as by the compliant interface of chemically modified between rigidity graphene nano filler and electric energy converting high molecular weight, effectively can reduce dielectric loss and the out-of-phase modulus of electric energy conversion polymer composites, thus strengthen high-voltage electric field disruptive strength, obtain the Electro-stimulate response intelligent macromolecule matrix material of excellent electroluminescent deformation performance and comprehensive electromechanical performance, the method is simple to operate simultaneously, with low cost, there is important science and using value.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of PEDOT:PSS-RGO prepared by embodiment 1;
Fig. 2 is the transmission electron microscope picture of PEDOT:PSS-RGO prepared by embodiment 1;
Fig. 3 is the surface atom force microscope figure of PEDOT:PSS-RGOPU prepared by embodiment 7;
Fig. 4 is the profile scanning Electronic Speculum figure of PEDOT:PSS-RGOPU prepared by embodiment 7;
Fig. 5 is the specific inductivity of the PEDOT:PSS-RGOPU (contrast RGOPU and PU) that under room temperature prepared by embodiment 7 and the dielectric loss change curve with frequency;
Fig. 6 is the change curve of the storage modulus of PEDOT:PSS-RGOPU (contrast RGOPU and PU) prepared by embodiment 7;
Fig. 7 is the out-of-phase modulus variation with temperature curve of PEDOT:PSS-RGOPU (contrast RGOPU and PU) prepared by embodiment 7;
Fig. 8 is that PEDOT:PSS-RGOPU material prepared by embodiment 7 carries out the flexible micro-move device unit pictorial diagram of electric field induced strain test;
Fig. 9 is the change curve of electroluminescent deformation value with strength of electric field of PEDOT:PSS-RGOPU (contrast RGOPU and PU) prepared by embodiment 7.
Embodiment
Below in conjunction with accompanying drawing, to simulation tsunami of the present invention cause atmospheric gravity waves and be described in detail in the method for ionospheric coupling.
Material source illustrates: poly-(3, 4-ethylenedioxy thiophene): polystyrolsulfon acid (1.4% aqueous solution) is purchased from Adamas company of Switzerland, aniline is purchased from Shanghai traditional Chinese medicines Reagent Company, pyrroles and thiophene purchased from American AlfaAesar company, Graphene makes (reference: Park, Sungjin by oneself by this laboratory, An, Jinho, Potts, JeffreyR., Velamakanni, Aruna, Murali, Shanthi, Ruoff, RodneyS.Hydrazine-reductionofgraphite-andgrapheneoxide.C arbon2011, 49, 3019-3023.), urethane dielectric elastomer (EstaneTPU58887) purchased from American Lubrizol company, vinylformic acid dielectric elastomer (VHB4910) purchased from American 3M company, silicon rubber dielectric elastomer (DC3481) purchased from American DowCorning company, poly(vinylidene fluoride) purchased from American AlfaAesar company, poly(vinylidene fluoride)-trifluoro-ethylene copolymer and poly(vinylidene fluoride)-trifluoro-ethylene-chlorine fluoride copolymers are purchased from Japanese KUREHA company, ammonium persulphate, hydrochloric acid, N, dinethylformamide is purchased from Shanghai traditional Chinese medicines Reagent Company.
The code name of synthetic product illustrates: PEDOT:PSS represents poly-(3, 4-ethylenedioxy thiophene): polystyrolsulfon acid, PANI represents polyaniline, PPY represents polypyrrole, PTH represents Polythiophene, RGO represents Graphene, PU represents urethane dielectric elastomer, AC represents vinylformic acid dielectric elastomer, SI represents silicon rubber dielectric elastomer, PVDF represents poly(vinylidene fluoride), P (VDF-TrFE) represents poly(vinylidene fluoride)-trifluoro-ethylene copolymer, P (VDF-TrFE-CFE) represents poly(vinylidene fluoride)-trifluoro-ethylene-chlorine fluoride copolymers, DMF represents N, dinethylformamide, represent nano-filler modified electric energy conversion polymkeric substance.
The preparation of example 1:PEDOT:PSS-RGO (1)
10mL deionized water is added in the small beaker of 25mL, then ultrasonic wave added dispersion 6h after adding the Graphene of 50mg, then PEDOT:PSS (the density 1g/mL of 3.5mL is added with needle applicator, solid content 1.4%) solution, after ultrasonic disperse 4h, mixing solutions is poured over diameter 6cm and on the smooth silica glass in bottom surface, be placed in loft drier and carry out evaporation induced self-assembly 24h under 50 DEG C of low temperature, gathered (3,4-ethylene dioxythiophene): polystyrolsulfon acid non-covalent modification Graphene PEDOT:PSS-RGO (1).The scanning electron microscope (SEM) photograph of the PEDOT:PSS-RGO of preparation and transmission electron microscope picture show this nano material and present " sandwich " structure, and conducting polymer thin layer is evenly coated on graphene sheet layer surface.
The preparation of example 2:PEDOT:PSS-RGO (2)
10mL deionized water is added in the small beaker of 25mL, then ultrasonic wave added dispersion 6h after adding the Graphene of 50mg, then the PEDOT:PSS(density 1g/mL of 3.5mL is added with needle applicator, solid content 1.4%) solution, after ultrasonic disperse 4h, mixing solutions is poured on the smooth silica glass in bottom surface, be placed in loft drier and carry out evaporation induced self-assembly 24h under 50 DEG C of low temperature, gathered (3,4-ethylene dioxythiophene): polystyrolsulfon acid non-covalent modification Graphene PEDOT:PSS-RGO (2).
The preparation of example 3:PEDOT:PSS-RGO (3)
10mL deionized water is added in the small beaker of 25mL, then ultrasonic wave added dispersion 6h after adding the Graphene of 50mg, then PEDOT:PSS (the density 1g/mL of 0.7mL is added with needle applicator, solid content 1.4%) solution, after ultrasonic disperse 4h, mixing solutions is poured on the smooth silica glass in bottom surface, be placed in loft drier and carry out evaporation induced self-assembly 24h under 50 DEG C of low temperature, gathered (3,4-ethylene dioxythiophene): polystyrolsulfon acid non-covalent modification Graphene PEDOT:PSS-RGO (3).
The preparation of example 4:PANI-RGO
100mg Graphene and the mixing of 0.1mL aniline is added in 400mL beaker, then ultrasonic disperse 4h at ice-water bath 0 DEG C is placed in, then add 100mL dilute hydrochloric acid (1M) and continue ultrasonic disperse 2h, the hydrochloric acid soln (0.05M) of slow dropping ammonium persulphate causes aniline monomer polymerization, react 12h at keeping 0 DEG C, after being naturally warmed up to room temperature reaction 10h, separation obtains solid and is placed in the graphene nano material PANI-RGO that namely vacuum drying oven 50 DEG C of dry 20h obtain polyaniline non-covalent modification.Regulate the consumption of aniline can obtain the PANI-RGO of different conducting polymer mass ratio.
The preparation of example 5:PPY-RGO
100mg Graphene and 0.2mL pyrroles's mixing is added in 400mL beaker, then ultrasonic disperse 4h at ice-water bath 0 DEG C is placed in, then add 100mL dilute hydrochloric acid (1M) and continue ultrasonic disperse 2h, the hydrochloric acid soln (0.05M) of slow dropping ammonium persulphate causes pyrrole monomer polymerization, react 12h at keeping 0 DEG C, after being naturally warmed up to room temperature reaction 10h, separation obtains solid and is placed in the graphene nano material PPY-RGO that namely vacuum drying oven 50 DEG C of dry 20h obtain polypyrrole non-covalent modification.Regulate the consumption of pyrroles can obtain the PPY-RGO of different conducting polymer mass ratio.
The preparation of example 6:PTH-RGO
100mg Graphene and the mixing of 0.3mL thiophene is added in 400mL beaker, then ultrasonic disperse 4h at ice-water bath 0 DEG C is placed in, then add 100mL dilute hydrochloric acid (1M) and continue ultrasonic disperse 2h, the hydrochloric acid soln (0.05M) of slow dropping ammonium persulphate causes thiophene monomer polymerization, react 12h at keeping 0 DEG C, after being naturally warmed up to room temperature reaction 10h, separation obtains solid and is placed in the graphene nano material PTH-RGO that namely vacuum drying oven 50 DEG C of dry 20h obtain Polythiophene non-covalent modification.Regulate the consumption of thiophene can obtain the PTH-RGO of different conducting polymer mass ratio.
The preparation of example 7:PEDOT:PSS-RGOPU
500mgPU is fully stirred at 75 DEG C, be dissolved in completely in 25mLDMF solvent and form solution A, take the PEDOT:PSS-RGO nano functional filler of PU mass percent 3.0% in addition, ultrasonic disperse forms B solution in DMF solvent, then finely dispersed B solution is slowly added in solution A, ultrasonic wave added stirs 6h, mixture is positioned over refrigerator and cooled degassed process, finally mixture is poured on smooth silica glass, leave standstill 30min, be placed in air dry oven 70 DEG C of air set 24h, silica glass is placed in vacuum drying oven under 60 DEG C of vacuum, is incubated 12h for removing DMF solvent further, 130 DEG C of annealing 3h, finally the macromolecule membrane on silica glass is taken off electric energy conversion polymer composites PEDOT:PSS-RGO (3%) PU namely obtaining modification.Surface atom force microscope figure and the profile scanning Electronic Speculum figure Presentation Function functionalized graphene of PEDOT:PSS-RGOPU obtain disperseing very equably in polyurethane matrix.Under PEDOT:PSS-RGO (3%) PU room temperature and 1000Hz frequency, specific inductivity is 350, and dielectric loss is 0.20, and out-of-phase modulus is 200MPa, and under 32.2MV/m electric field action, thickness direction electroluminescent deformation value is 162%.
The preparation of example 8:PANI-RGOPU
500mgPU is fully stirred at 75 DEG C, be dissolved in completely in 25mLDMF solvent and form solution A, take the PANI-RGO nano functional filler of PU mass percent 2.5% in addition, ultrasonic disperse forms B solution in DMF solvent, then finely dispersed B solution is slowly added in solution A, ultrasonic wave added stirs 6h, mixture is positioned over refrigerator and cooled degassed process, finally mixture is poured on smooth silica glass, leave standstill 30min, be placed in air dry oven 70 DEG C of air set 24h, silica glass is placed in vacuum drying oven under 60 DEG C of vacuum, is incubated 12h for removing DMF solvent further, 130 DEG C of annealing 3h, finally the macromolecule membrane on silica glass is taken off electric energy conversion polymer composites PANI-RGO (2.5%) PU namely obtaining modification.Under PANI-RGO (2.5%) PU room temperature and 1000Hz frequency, specific inductivity is 172, and dielectric loss is 0.06, and out-of-phase modulus is 261MPa, and under 37.0MV/m electric field action, thickness direction electroluminescent deformation value is 55%.
The preparation of example 9:PPY-RGOPU
500mgPU is fully stirred at 75 DEG C, be dissolved in completely in 25mLDMF solvent and form solution A, take the PPY-RGO nano functional filler of PU mass percent 2.0% in addition, ultrasonic disperse forms B solution in DMF solvent, then finely dispersed B solution is slowly added in solution A, ultrasonic wave added stirs 6h, mixture is positioned over refrigerator and cooled degassed process, finally mixture is poured on smooth silica glass, leave standstill 30min, be placed in air dry oven 70 DEG C of air set 24h, silica glass is placed in vacuum drying oven under 60 DEG C of vacuum, is incubated 12h for removing DMF solvent further, 130 DEG C of annealing 3h, finally the macromolecule membrane on silica glass is taken off electric energy conversion polymer composites PPY-RGO (2%) PU namely obtaining modification.Under PPY-RGO (2%) PU room temperature and 1000Hz frequency, specific inductivity is 193, and dielectric loss is 0.04, and out-of-phase modulus is 151MPa, and under 37.8MV/m electric field action, thickness direction electroluminescent deformation value is 61%.
The preparation of example 10:PTH-RGOPU
500mgPU is fully stirred at 75 DEG C, be dissolved in completely in 25mLDMF solvent and form solution A, take the PTH-RGO nano functional filler of PU mass percent 1.5% in addition, ultrasonic disperse forms B solution in DMF solvent, then finely dispersed B solution is slowly added in solution A, ultrasonic wave added stirs 6h, mixture is positioned over refrigerator and cooled degassed process, finally mixture is poured on smooth silica glass, leave standstill 30min, be placed in air dry oven 70 DEG C of air set 24h, silica glass is placed in vacuum drying oven under 60 DEG C of vacuum, is incubated 12h for removing DMF solvent further, 130 DEG C of annealing 3h, finally the macromolecule membrane on silica glass is taken off electric energy conversion polymer composites PTH-RGO (1.5%) PU namely obtaining modification.Under PTH-RGO (1.5%) PU room temperature and 1000Hz frequency, specific inductivity is 110, and dielectric loss is 0.03, and out-of-phase modulus is 143MPa, and under 38.2MV/m electric field action, thickness direction electroluminescent deformation value is 47%.
The preparation of example 11:PEDOT:PSS-RGOAC, PEDOT:PSS-RGOSI, PEDOT:PSS-RGOPVDF, PEDOT:PSS-RGOP (VDF-TrFE) and PEDOT:PSS-RGOP (VDF-TrFE-CFE)
400mgAC or SI or PVDF or P (VDF-TrFE) or P (VDF-TrFE-CFE) is fully stirred at 75 DEG C, be dissolved in completely in 25mLDMF solvent and form solution A, take the PEDOT:PSS-RGO nano functional filler of PU mass percent 2.0% in addition, ultrasonic disperse forms B solution in DMF solvent, then finely dispersed B solution is slowly added in solution A, ultrasonic wave added stirs 6h, mixture is positioned over refrigerator and cooled degassed process, finally mixture is poured on smooth silica glass, leave standstill 30min, be placed in air dry oven 70 DEG C of air set 24h, silica glass is placed in vacuum drying oven under 60 DEG C of vacuum, is incubated 12h for removing DMF solvent further, 130 DEG C of annealing 3h, finally the macromolecule membrane on silica glass is taken off electric energy conversion polymer composites PEDOT:PSS-RGO (2%) AC or PEDOT:PSS-RGO (2%) SI or PEDOT:PSS-RGO (2%) PVDF or PEDOT:PSS-RGO (2%) P (VDF-TrFE) or PEDOT:PSS-RGO (2%) P (VDF-TrFE-CFE) that namely obtain modification.Regulate the consumption of PEDOT:PSS-RGO can obtain the modification electric energy conversion polymer composites of different PEDOT:PSS-RGO functionalization graphene mass ratio.
The preparation of example 12:PANI-RGOAC, PANI-RGOSI, PANI-RGOPVDF, PANI-RGOP (VDF-TrFE) and PANI-RGOP (VDF-TrFE-CFE)
600mgAC or SI or PVDF or P (VDF-TrFE) or P (VDF-TrFE-CFE) is fully stirred at 75 DEG C, be dissolved in completely in 40mLDMF solvent and form solution A, take the PANI-RGO nano functional filler of PU mass percent 1.0% in addition, ultrasonic disperse forms B solution in DMF solvent, then finely dispersed B solution is slowly added in solution A, ultrasonic wave added stirs 6h, mixture is positioned over refrigerator and cooled degassed process, finally mixture is poured on smooth silica glass, leave standstill 30min, be placed in air dry oven 70 DEG C of air set 24h, silica glass is placed in vacuum drying oven under 60 DEG C of vacuum, is incubated 12h for removing DMF solvent further, 130 DEG C of annealing 3h, finally the macromolecule membrane on silica glass is taken off electric energy conversion polymer composites PANI-RGO (1%) AC or PANI-RGO (1%) SI or PANI-RGO (1%) PVDF or PANI-RGO (1%) P (VDF-TrFE) or PANI-RGO (1%) P (VDF-TrFE-CFE) that namely obtain modification.Regulate the consumption of PANI-RGO can obtain the modification electric energy conversion polymer composites of different PANI-RGO functionalization graphene mass ratio.
The preparation of example 13:PPY-RGOAC, PPY-RGOSI, PPY-RGOPVDF, PPY-RGOP (VDF-TrFE) and PPY-RGOP (VDF-TrFE-CFE)
800mgAC or SI or PVDF or P (VDF-TrFE) or P (VDF-TrFE-CFE) is fully stirred at 75 DEG C, be dissolved in completely in 50mLDMF solvent and form solution A, take the PPY-RGO nano functional filler of PU mass percent 0.5% in addition, ultrasonic disperse forms B solution in DMF solvent, then finely dispersed B solution is slowly added in solution A, ultrasonic wave added stirs 6h, mixture is positioned over refrigerator and cooled degassed process, finally mixture is poured on smooth silica glass, leave standstill 30min, be placed in air dry oven 70 DEG C of air set 24h, silica glass is placed in vacuum drying oven under 60 DEG C of vacuum, is incubated 12h for removing DMF solvent further, 130 DEG C of annealing 3h, finally the macromolecule membrane on silica glass is taken off electric energy conversion polymer composites PPY-RGO (0.5%) AC or PPY-RGO (0.5%) SI or PPY-RGO (0.5%) PVDF or PPY-RGO (0.5%) P (VDF-TrFE) or PPY-RGO (0.5%) P (VDF-TrFE-CFE) that namely obtain modification.Regulate the consumption of PPY-RGO can obtain the modification electric energy conversion polymer composites of different PPY-RGO functionalization graphene mass ratio.
The preparation of example 14:PTH-RGOAC, PTH-RGOSI, PTH-RGOPVDF, PTH-RGOP (VDF-TrFE) and PTH-RGOP (VDF-TrFE-CFE)
1000mgAC or SI or PVDF or P (VDF-TrFE) or P (VDF-TrFE-CFE) is fully stirred at 75 DEG C, be dissolved in completely in 80mLDMF solvent and form solution A, take the PTH-RGO nano functional filler of PU mass percent 0.25% in addition, ultrasonic disperse forms B solution in DMF solvent, then finely dispersed B solution is slowly added in solution A, ultrasonic wave added stirs 6h, mixture is positioned over refrigerator and cooled degassed process, finally mixture is poured on smooth silica glass, leave standstill 30min, be placed in air dry oven 70 DEG C of air set 24h, silica glass is placed in vacuum drying oven under 60 DEG C of vacuum, is incubated 12h for removing DMF solvent further, 130 DEG C of annealing 3h, finally the macromolecule membrane on silica glass is taken off electric energy conversion polymer composites PTH-RGO (0.25%) AC or PTH-RGO (0.25%) SI or PTH-RGO (0.25%) PVDF or PTH-RGO (0.25%) P (VDF-TrFE) or PTH-RGO (0.25%) P (VDF-TrFE-CFE) that namely obtain modification.Regulate the consumption of PTH-RGO can obtain the modification electric energy conversion polymer composites of different PTH-RGO functionalization graphene mass ratio.
The above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.All any amendments done within the spirit and principles in the present invention, equivalent to replace and improvement etc., such as solid state reaction condition, reactant species, reactant ratio, calcination condition etc., within the protection domain that all should be included in the claims in the present invention.
Claims (7)
1. a preparation method for conducting polymer non-covalent modification Graphene modification electric energy conversion polymer materials, is characterized in that, comprise the following steps:
1) method of evaporation induced self-assembly or the method for in-situ polymerization is adopted to carry out conducting polymer non-covalent modification Graphene;
2) conducting polymer non-covalent modification graphene nano material ultrasonic wave added is dispersed in electric energy conversion polymers soln, adopts solution film casting method to prepare conducting polymer non-covalent modification Graphene electric energy conversion polymer composites.
2. the preparation method of electric energy conversion polymer materials according to claim 1, it is characterized in that, described conductive polymers comprises poly-(3,4-ethylene dioxythiophene): the one in polystyrolsulfon acid, polyaniline, polypyrrole, Polythiophene.
3. the preparation method of electric energy conversion polymer materials according to claim 2, it is characterized in that, by described poly-(3,4-ethylenedioxy thiophene): polystyrolsulfon acid carries out after dilute hydrochloric acid adulterates in right amount, the method preparation of evaporation induced self-assembly is adopted to gather (3,4-ethylene dioxythiophene) with Graphene according to different mass ratio: polystyrolsulfon acid non-covalent modification Graphene; The method of evaporation induced self-assembly: by conductive polymers and graphene dispersion in deionized water, 6 ~ 12h is stirred under ultrasonic wave added, then mixing solutions is poured into diameter 6 ~ 15cm and on the smooth silica glass in bottom surface, be placed in loft drier and carry out evaporation induced self-assembly 12 ~ 48h under 35 ~ 60 DEG C of low temperature, obtain conducting polymer non-covalent modification graphene nano material.
4. the preparation method of electric energy conversion polymer materials according to claim 2, it is characterized in that, the method that polyaniline, polypyrrole and Polythiophene adopt aniline, pyrroles and thiophene monomer to carry out in-situ polymerization on graphene sheet layer obtains electrically conductive polyaniline, polypyrrole and Polythiophene non-covalent modification graphene nano material; The method of in-situ polymerization: aniline, pyrroles and thiophene monomer are mixed with graphene uniform respectively, then ultrasonic disperse 4 ~ 12h at ice-water bath 0 DEG C is placed in, then the dilute hydrochloric acid adding 1M continues ultrasonic disperse 1 ~ 2h, the hydrochloric acid soln initiated polymerization of slow dropping ammonium persulphate, react 10 ~ 24h at keeping 0 DEG C, be separated after reaction and obtain solid and be placed in vacuum drying oven 40 ~ 60 DEG C of drying 12 ~ 48h and namely obtain polyaniline, polypyrrole and Polythiophene non-covalent modification graphene nano material.
5. the preparation method of electric energy conversion polymer materials according to claim 1, it is characterized in that, described step 2) detailed process is: first electric energy changed polymer materials and fully stirs at 50 ~ 80 DEG C, be dissolved in N completely, solution A is formed in dinethylformamide (DMF) solvent, take the non-covalent modification graphene nano functional stuffing being less than 5.0% with polymer materials mass percent in addition respectively, ultrasonic disperse forms B solution in DMF solvent system; Then finely dispersed B solution slowly added in solution A, ultrasonic wave added stirs 4 ~ 8h, obtains mixture, mixture is positioned over refrigerator and cooled degassed process; Finally mixture is poured on smooth silica glass, leave standstill 15 ~ 30min, be placed in vacuum drying oven 60 ~ 80 DEG C of air set 20 ~ 30h, under 50 ~ 75 DEG C of vacuum, 12 ~ 18h is incubated for removing DMF solvent further, 130 DEG C of annealing 3 ~ 5h, take off the electric energy conversion polymer composites namely obtaining modification by the macromolecule membrane on silica glass.
6. the preparation method of the electric energy conversion polymer materials according to any one of claim 1 to 5, it is characterized in that, described electric energy changes that polymkeric substance is urethane dielectric elastomer, silicone dielectric elastomerics, vinylformic acid dielectric elastomer, poly(vinylidene fluoride) and multipolymer thereof any one.
7. the preparation method of electric energy conversion polymer materials according to claim 6, it is characterized in that, wherein polyvinylidene fluoride copolymers thing be poly(vinylidene fluoride)-trifluoro-ethylene copolymer, poly(vinylidene fluoride)-trifluoro-ethylene-chlorine fluoride copolymers any one.
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