CN105623136B - A kind of composite conducting polymer material and preparation method thereof - Google Patents
A kind of composite conducting polymer material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of composite conducting polymer materials, by the conducting nanowires of one-dimentional structure, graphene and spherical polymer the matrix composition of two-dimensional structure, combine the advantage of one-dimensional electric nano-material and two-dimensional graphene, by two-dimensional graphene with after polymer matrix bluk recombination again with excellent electrical high length-diameter ratio one-dimensional electric nano wire carry out it is compound, so as to improve the dispersing uniformity of conductive filler in a polymer matrix, increase the touch opportunity between conductive filler in polymer composites, utilize one-dimensional electric nano wire and the synergistic effect of two-dimensional graphene, construct efficient conductive path network, improve the electric conductivity of polymer composites.In addition, the present invention also provides a kind of preparation methods of composite conducting polymer material.
Description
Technical field
The present invention relates to conducing composite material technical field more particularly to a kind of composite conducting polymer material and its preparations
Method.
Background technology
Polymer base conductive composite material is because of its lightweight, easy processing molding, durable, inexpensive and can adjust in a wide range of
The features such as electricity and mechanical property of material, in electromagnetic shielding material, antistatic material, electronic tag, electrode of solar battery
There is significant application value in the fields of grade.Polymer base conductive composite material is usually made of conductive filler and polymeric matrix.It is common
Conductive filler have metallic conductive fillers (predominantly gold, silver, copper, nickel etc., shape can be graininess, spherical, linear etc.) and carbon
It is conductive filler (carbon black, carbon nanotube, graphene etc.).The sheets of conductive filler of two-dimensional structure according to conductive seepage theory
It is more advantageous to obtaining low seepage flow threshold than the conductive fillers such as conventional graininess, spherical with the nano wire conductive filler of one-dimentional structure
Value and high conductivity.
In the conductive filler of two-dimensional structure, graphene is because of its excellent electrical property, hot property and huge specific surface area
The features such as have received widespread attention.How graphene effectively evenly to be disperseed in a polymer matrix, to avoid graphene phase
Performance is caused drastically to decline due to strong Van der Waals force is reunited between mutually, be to prepare conductive composite wood by conductive filler of graphene
One of critical issue of material.
In order to realize effective dispersion of graphene, 102964713 A of patent CN are disperseed with n,N-Dimethylformamide solvent
With chloromethyl ether rnonodisperse polystyrene, function is prepared for by the blending of the two, suction filtration, washing, drying and other steps for graphene oxide
Graphite alkene core-shell nano hybrid material.Although this method realizes graphene in the polymer homodisperse, but use
A large amount of toxic solvents.In order to avoid the use of toxic solvent, 104261403 A of patent CN are with polystyrene moulding and oxidation stone
Electrostatic interaction between black alkene forms uniform water dispersion liquid.104650521 A of patent CN are with cation polystyrene and graphite oxide
Alkene is compound, can inhibit the autohemagglutination of graphene, and Selective graphene is induced to be distributed in polymer particle surface, forms perfect stone
Black alkene three-dimensional network skeleton, prepared composite material exhibits go out extremely low Chongqing of leading and ooze value and higher conductivity.Patent CN
103554702 A are prepared for a kind of network-like graphite of graphene with graphene coated polystyrene through cast or pressing mold
Alkene polymer composite.
The nano-material of one-dimentional structure is because with high length-diameter ratio characteristic, seepage flow threshold can be reduced using it as conductive filler
Value improves conductivity.Patent CN1873838 A using nano silver wire and silver powder as compounded mix, using acrylic resin as polymer
Matrix is prepared for the polymer composite conducting material of high conductivity.104974500 A of patent CN disclose one kind and are received containing metal
Polymer base conductive composite material of rice noodles and graphene oxide and preparation method thereof, passes through the polymer matrix in metal nanometer line
The non-conductive graphene oxide of a small amount of sheet is added in composite material, on the one hand prevents the reunion of metal nanometer line, the opposing party
Face can prevent the sinking of metal nanometer line, therefore the dispersion of metal nanometer line is more uniform, so as to be improved electric conductivity.
But this method is only applicable to water-soluble polymeric matrix, has larger limitation, simultaneous oxidation graphene only plays surely
Determine dispersant effect, do not have electric conductivity.In order to combine two dimension and the advantage of one-dimensional electric filler, patent CN
104992781A is with graphene, nano silver wire and poly- (3,4- ethylenedioxy thiophenes)：Poly styrene sulfonate is prepared for for raw material
A kind of graphene-based tri compound transparent conductive film improves the photoelectric properties of graphene-based transparent conductive film, but the material
Expect the composite material for conductive film rather than ontology conduction.
Invention content
In view of this, in order to overcome the problems, such as prior art the defects of and, the present invention provides a kind of conducting polymer composite wood
Material.
A kind of composite conducting polymer material, by the conducting nanowires of one-dimentional structure, the graphene of two-dimensional structure and spherical shape
Polymeric matrix forms, and each component quality proportioning is as follows：
5~40 parts of the conducting nanowires of one-dimentional structure
0.5~5 part of the graphene of two-dimensional structure
55~90 parts of spherical polymer matrix.
In some embodiments, the conducting nanowires are nano silver wire, copper nano-wire, nanowires of gold, nickel nano wire, aluminium
One or more of nano wire, Fe nanowire, single-walled carbon nanotube and multi-walled carbon nanotube.
In some embodiments, the electrical-conductive nanometer line length is 5~500 μm, 30~300nm of diameter.
In some embodiments, the spherical polymer matrix be spherical polystyrene type, polymethacrylate,
Polyacrylate, cinnamic acrylic ester analog copolymer, acrylic acid-methacrylic acid lipin polymer, polyacrylamide,
One or more of polyethylene, phenolic resin, polysiloxanes, phenyl silicone.
In some embodiments, a diameter of 200nm~10 μm of the spherical polymer.
In addition, the present invention also provides a kind of preparation method of composite conducting polymer material, include the following steps：
Step S10：Prepare the polymer/graphene composite material of graphene coated polymer
The aqueous dispersions of graphene oxide with the aqueous dispersions of spherical polymer are mixed, graphene oxide is made uniformly to coat
On spherical polymer surface, the composite material of graphene oxide coated polymer is obtained；
Then in-situ chemical reduction is carried out to the composite material of the graphene oxide coated polymer, obtains reduction-oxidation
The composite material of graphene coated polymer；
By washing, after removing unreacted impurity, it is dispersed in deionized water again, obtains graphene coated polymer
Polymer/graphene composite material；
Step S20：Prepare polymer/graphene/conducting nanowires mixture of multidimensional hybrid structure
The aqueous dispersions of the conducting nanowires are added to the polymer/graphene composite wood of step (1) preparation
In the aqueous dispersions of material, it is uniformly mixed, obtains polymer/graphene/conducting nanowires mixed dispersion liquid of multidimensional hybrid structure；
Removal aqueous medium is filtered, then polymer/graphene/conducting nanowires through being dried to obtain multidimensional hybrid structure mix
Object；
Step S30：Prepare the polymerization based conductive composite material of multidimensional hybrid structure
Polymer/graphene/conducting nanowires mixture compression molding of multidimensional hybrid structure prepared by step (2),
Obtain the polymerization based conductive composite material of multidimensional hybrid structure, it is each in the composite conducting polymer material of the multidimensional hybrid structure
The quality proportioning of component is as follows：
5~40 parts of the conducting nanowires of one-dimentional structure
0.5~5 part of the graphene of two-dimensional structure
55~90 parts of spherical polymer matrix.
In some embodiments, in step S10, the polymer/graphene composite material of graphene coated polymer is prepared,
Specifically include following step：
The aqueous dispersions of graphene oxide with the aqueous dispersions of spherical polymer are mixed, use cationic spherical polymer
Or graphene oxide is made to be evenly coated at spherical polymer surface to 1~6 by adjusting pH value of solution, obtain graphene oxide cladding
The composite material of polymer.
In some embodiments, in step S10, graphene oxide in-situ reducing method is electronation, and reducing agent is water
Close one kind in hydrazine, Dimethylhydrazine, hydroiodic acid, sodium borohydride, potassium borohydride, vitamin C, concentrated ammonia liquor.
In some embodiments, in step S30, the compression molding is for cold pressing or heating and mould pressing, cold pressing condition：Temperature
For room temperature, pressure 1-30MPa, time 10min~3h；Pressurized conditions are：Temperature (Tg+10)~(Tg+50) DEG C, Tg are polymerization
Object glass transition temperature, pressure 1-30MPa, time 2min~2h.
Relative to the prior art, composite conducting polymer material provided by the invention, by the conducting nanowires of one-dimentional structure,
Graphene and spherical polymer the matrix composition of two-dimensional structure, combine the excellent of one-dimensional electric nano-material and two-dimensional graphene
Gesture, by after two-dimensional graphene and polymer matrix bluk recombination again with the high length-diameter ratio one-dimensional electric nano wire with excellent electrical
It carries out compound, so as to improve the dispersing uniformity of conductive filler in a polymer matrix, increases in polymer composites
Touch opportunity between conductive filler using one-dimensional electric nano wire and the synergistic effect of two-dimensional graphene, constructs efficient
Conductive path network improves the electric conductivity of polymer composites.
In addition, the present invention also provides the preparation method of composite conducting polymer material, gathered by preparing graphene coated
The polymer/graphene composite material of object is closed, then prepares polymer/graphene/conducting nanowires mixing of multidimensional hybrid structure
The polymerization based conductive composite material of multidimensional hybrid structure is finally prepared in object, this preparation method is simple for process, recombination process without
Poisonous and harmful solvent need to be used, environmental protection, the composite material quality of preparation is high, good conductivity.
Simultaneously as it is uniformly dispersed in spherical polymer matrix using the graphene oxide of two-dimensional structure and gone back in situ
Original forms the conductive path of networking, the advantageous electric conductivity for improving polymer composites；The conducting nanowires of one-dimentional structure with
Redox graphene is uniformly dispersed and is in close contact, the synergistic effect of the two promote polymer composites electric conductivity into one
Step improves.
Description of the drawings
The polymer base conductive composite material of Fig. 1 multidimensional hybrid structures and its preparation process schematic diagram.
Fig. 2 is polymer/graphene/conducting nanowires mixture SEM figures of multidimensional hybrid structure prepared by embodiment 1.
Fig. 3 is the part of polymer/graphene/conducting nanowires mixture of multidimensional hybrid structure prepared by embodiment 1
Amplify SEM figures.
Fig. 4 is the section SEM figures of the polymer-matrix electric conduction material of multidimensional hybrid structure prepared by embodiment 1.
Specific embodiment
For the ease of understanding the present invention, the present invention is described more fully below with reference to relevant drawings.In attached drawing
Give the better embodiment of the present invention.It these are only the preferred embodiment of the present invention, not thereby limit the special of the present invention
Sharp range, every equivalent structure or equivalent flow shift made using description of the invention and accompanying drawing content directly or
It connects and is used in other related technical areas, be included within the scope of the present invention.
Unless otherwise defined, all of technologies and scientific terms used here by the article is with belonging to technical field of the invention
The normally understood meaning of technical staff is identical.Term used in the description of the invention herein is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein " and/or " including one or more
The arbitrary and all combination of relevant Listed Items.
Composite conducting polymer material provided by the invention, by the conducting nanowires of one-dimentional structure, the graphite of two-dimensional structure
Alkene and spherical polymer matrix composition, each component quality proportioning are as follows：
5~40 parts of the conducting nanowires of one-dimentional structure
0.5~5 part of the graphene of two-dimensional structure
55~90 parts of spherical polymer matrix.
Preferably, the conducting nanowires for nano silver wire, copper nano-wire, nanowires of gold, nickel nano wire, aluminium nano wire,
One or more of Fe nanowire, single-walled carbon nanotube and multi-walled carbon nanotube.
Preferably, the electrical-conductive nanometer line length is 5~500 μm, 30~300nm of diameter.
Preferably, the spherical polymer matrix is spherical polystyrene type, polymethacrylate, polyacrylic acid
Esters, cinnamic acrylic ester analog copolymer, acrylic acid-methacrylic acid lipin polymer, polyacrylamide, polyethylene, phenol
One or more of urea formaldehyde, polysiloxanes, phenyl silicone.
Preferably, a diameter of 200nm~10 μm of the spherical polymer.
It is appreciated that composite conducting polymer material provided by the invention, is tied by the conducting nanowires of one-dimentional structure, two dimension
Graphene and spherical polymer the matrix composition of structure, combine the advantage of one-dimensional electric nano-material and two-dimensional graphene, lead to
Two-dimensional graphene is crossed with being carried out again with the high length-diameter ratio one-dimensional electric nano wire with excellent electrical after polymer matrix bluk recombination
It is compound, so as to improve the dispersing uniformity of conductive filler in a polymer matrix, increase conductive in polymer composites
Touch opportunity between filler using one-dimensional electric nano wire and the synergistic effect of two-dimensional graphene, constructs efficient conduction
Passage way network improves the electric conductivity of polymer composites.
Referring to Fig. 1, the polymer-matrix electric conduction of the preparation method for composite conducting polymer material provided by the invention is answered
Condensation material and its preparation process schematic diagram, include the following steps：
Step S10：Prepare the polymer/graphene composite material of graphene coated polymer
The aqueous dispersions of graphene oxide with the aqueous dispersions of spherical polymer are mixed, graphene oxide is made uniformly to coat
On spherical polymer surface, the composite material of graphene oxide coated polymer is obtained；
Then in-situ chemical reduction is carried out to the composite material of the graphene oxide coated polymer, obtains reduction-oxidation
The composite material of graphene coated polymer；
By washing, after removing unreacted impurity, it is dispersed in deionized water again, obtains graphene coated polymer
Polymer/graphene composite material；
Step S20：Prepare polymer/graphene/conducting nanowires mixture of multidimensional hybrid structure
The aqueous dispersions of the conducting nanowires are added to the polymer/graphene composite wood of step (1) preparation
In the aqueous dispersions of material, it is uniformly mixed, obtains polymer/graphene/conducting nanowires mixed dispersion liquid of multidimensional hybrid structure；
Removal aqueous medium is filtered, then polymer/graphene/conducting nanowires through being dried to obtain multidimensional hybrid structure mix
Object；
Step S30：Prepare the polymerization based conductive composite material of multidimensional hybrid structure
Polymer/graphene/conducting nanowires mixture compression molding of multidimensional hybrid structure prepared by step (2),
Obtain the polymerization based conductive composite material of multidimensional hybrid structure.
It is appreciated that the above-mentioned preparation method of the present invention is since the graphene oxide using two-dimensional structure is in spherical polymer base
Simultaneously in-situ reducing is uniformly dispersed in body, forms the conductive path of networking, the advantageous electric conductivity for improving polymer composites；One
The conducting nanowires of dimension structure are uniformly dispersed and are in close contact with redox graphene, and the synergistic effect of the two promotes polymer
Conductivity of composite material further improves.
Embodiment 1：
The graphene oxide aqueous dispersions of 10mL 5mg/mL (1 mass parts) are taken, are added to 89mL 5wt% (89 mass parts)
Grain size be about 440nm polystyrene spheres moisture dissipate, magnetic agitation is uniform, and hydrochloric acid solution is slowly added dropwise, by mixed solution
PH is adjusted to 2, stirs lower mixing 30min and obtains the spherical poly styrene composite material mixed solution of graphene oxide cladding；It will be above-mentioned
Mixed solution is placed in 80 DEG C of water-bath, is added in the hydrazine hydrate of 5ml85%, is terminated after reacting 3h under magnetic agitation, aoxidized
Reduced graphene coats the mixed solution of poly styrene composite material.This mixed solution is filtered, washing multipass removal unreacted
It after impurity, is dispersed to again in 100mL deionized waters, then is charged with the nano silver wire water of 10mL 5wt% (10 mass parts)
Dispersion liquid is dispersed with stirring the polystyrene/graphene/nano silver wire mixing dispersion solution for uniformly, obtaining multidimensional hybrid structure.It takes out
It filters off except aqueous medium, is put into 60 DEG C of baking ovens dry, dried powder is put into mold, 180 DEG C, suppress under 15MPa
10min obtains the polymer base conductive composite material of multidimensional hybrid structure.The polymerization of multidimensional hybrid structure prepared by the embodiment
The nano silver wire of one-dimentional structure and the mass ratio of the graphene of two-dimensional structure and polymeric matrix are in object based conductive composite material
10:1:89, conductivity is about 250S/m.
Please refer to Fig. 2, Fig. 3 and Fig. 4, respectively the polymer/graphene of multidimensional hybrid structure prepared by embodiment 1/lead
Thermoelectric nanowires mixture SEM schemes, the partial enlargement SEM of polymer/graphene/conducting nanowires mixture of multidimensional hybrid structure
The section SEM figures of the polymer-matrix electric conduction material of figure and multidimensional hybrid structure.
Embodiment 2：
The graphene oxide aqueous dispersions of 30mL 5mg/mL (3 mass parts) are taken, are added to 70mL 5wt% (70 mass parts)
Grain size be about 2.2 μm poly (methyl methacrylate) micro-sphere moisture dissipate, magnetic agitation is uniform, and hydrochloric acid solution is slowly added dropwise,
Mixed solution pH is adjusted to 3, lower mixing 30min is stirred and obtains the spherical polymethyl methacrylate composite wood of graphene oxide cladding
Expect mixed solution；Above-mentioned mixed solution is placed in 100 DEG C of water-bath, the hydroiodic acid of addition 5ml 45%, it is anti-under magnetic agitation
Terminate after answering 10h, obtain the mixed solution of redox graphene coated composite material of polymethyl methacrylate.This is mixed
Solution filters, after washing multipass removal unreacted impurity, is dispersed to again in 100mL deionized waters, then be charged with 27mL
The copper nano-wire aqueous dispersions of 5wt% (27 mass parts) are dispersed with stirring uniformly, obtain the polymethylacrylic acid of multidimensional hybrid structure
Methyl esters/graphene/copper nano-wire mixing dispersion solution.Removal aqueous medium is filtered, is put into drying in 40 DEG C of vacuum drying oven, it will be dry
Powder after dry is put into mold, under room temperature, 30MPa suppress 30min obtain multidimensional hybrid structure polymer-matrix electric conduction it is compound
Material.The nano silver wire and two of one-dimentional structure in the polymer base conductive composite material of multidimensional hybrid structure prepared by the embodiment
The mass ratio of graphene and polymeric matrix for tieing up structure is 27:3:70, conductivity is about 1080S/m.
Embodiment described above only expresses the several embodiments of the present invention, and description is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (6)
1. a kind of preparation method of composite conducting polymer material, which is characterized in that include the following steps：
Step S10：Prepare the polymer/graphene composite material of graphene coated polymer
The aqueous dispersions of graphene oxide with the aqueous dispersions of spherical polymer are mixed, graphene oxide is made to be evenly coated at ball
Shape polymer surfaces obtain the composite material of graphene oxide coated polymer；
Then in-situ chemical reduction is carried out to the composite material of the graphene oxide coated polymer, obtains reduction-oxidation graphite
The composite material of alkene coated polymer；
It by washing, after removing unreacted impurity, is dispersed in deionized water again, obtains the poly- of graphene coated polymer
Close object/graphene composite material；
Step S20：Prepare polymer/graphene/conducting nanowires mixture of multidimensional hybrid structure
The aqueous dispersions of the conducting nanowires are added to the polymer/graphene composite material of step (1) preparation
In aqueous dispersions, it is uniformly mixed, obtains polymer/graphene/conducting nanowires mixed dispersion liquid of multidimensional hybrid structure；
Filter removal aqueous medium, then polymer/graphene/conducting nanowires mixture through being dried to obtain multidimensional hybrid structure；
Step S30：Prepare the polymerization based conductive composite material of multidimensional hybrid structure
Polymer/graphene/conducting nanowires mixture compression molding of multidimensional hybrid structure prepared by step (2), obtains
The polymerization based conductive composite material of multidimensional hybrid structure, each component in the composite conducting polymer material of the multidimensional hybrid structure
Quality proportioning it is as follows：
5~40 parts of the conducting nanowires of one-dimentional structure
0.5~5 part of the graphene of two-dimensional structure
55~90 parts of spherical polymer matrix；
In step S10, the polymer/graphene composite material of graphene coated polymer is prepared, specifically includes following step：
The aqueous dispersions of graphene oxide with the aqueous dispersions of spherical polymer are mixed, using cationic spherical polymer or are led to
Overregulating pH value of solution makes graphene oxide be evenly coated at spherical polymer surface to 1~6, obtains graphene oxide cladding polymerization
The composite material of object；
In step S30, the compression molding is for cold pressing or heating and mould pressing, cold pressing condition：Temperature is room temperature, pressure 1-
30MPa, time 10min~3h；Pressurized conditions are：Temperature (Tg+10)~(Tg+50) DEG C, Tg are polymer glass transition temperature
Degree, pressure 1-30MPa, time 2min~2h.
2. the preparation method of composite conducting polymer material as described in claim 1, which is characterized in that the conducting nanowires
For nano silver wire, copper nano-wire, nanowires of gold, nickel nano wire, aluminium nano wire, Fe nanowire, single-walled carbon nanotube and multi wall carbon
One or more of nanotube.
3. the preparation method of composite conducting polymer material as claimed in claim 2, which is characterized in that the conducting nanowires
Length is 5~500 μm, 30~300nm of diameter.
4. the preparation method of composite conducting polymer material as described in claim 1, which is characterized in that the spherical polymer
Matrix is spherical polystyrene type, polymethacrylate, polyacrylate, cinnamic acrylic ester analog copolymer,
Acrylic acid-methacrylic acid lipin polymer, polyacrylamide, polyethylene, phenolic resin, polysiloxanes, phenyl silicone
One or more of.
5. the preparation method of composite conducting polymer material as claimed in claim 4, which is characterized in that the spherical polymer
A diameter of 200nm~10 μm.
6. the preparation method of composite conducting polymer material as described in claim 1, which is characterized in that in step S10, oxidation
Graphene in-situ reducing method be electronation, reducing agent for hydrazine hydrate, Dimethylhydrazine, hydroiodic acid, sodium borohydride, potassium borohydride,
One kind in vitamin C, concentrated ammonia liquor.
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