CN105623136A - Polymer conductive composite and preparation method thereof - Google Patents
Polymer conductive composite and preparation method thereof Download PDFInfo
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Abstract
The invention provides a polymer conductive composite. The polymer conductive composite is composed of conductive nano-wires of one-dimensional structures, graphene of a two-dimensional structure and a spherical polymer matrix. The advantages of the one-dimensional conductive nano-wire materials and the two-dimensional graphene are combined, the two-dimensional graphene and the polymer matrix are compounded and then compounded with the one-dimensional conductive nano-wires with high length-diameter ratios and excellent electrical performance, and therefore dispersion uniformity of conductive filler in the polymer matrix is improved, and the contact chance between the conductive filler in the polymer composite is increased; through the synergistic effect of the one-dimensional conductive nano-wires and the two-dimensional graphene, an efficient conductive path network is established, and conductivity of the polymer composite is improved. The invention further provides a preparation method of the polymer conductive composite.
Description
Technical field
The present invention relates to conducing composite material technical field, particularly relate to a kind of composite conducting polymer material and its preparation method.
Background technology
Polymer base conductive composite material is because of its lightweight, easily machine-shaping, durable, low cost and can regulate the features such as the electricity of material and mechanical property on a large scale, has significant application value in fields such as electromagnetic shielding material, antistatic material, electronic tag, electrode of solar battery. Polymer base conductive composite material is made up of conductive filler material and polymeric matrix usually. Conventional conductive filler material has metallic conduction filler (being mainly gold and silver, copper, nickel etc., shape can be particulate state, spherical, wire etc.) and carbon conductive filler (carbon black, carbon nanotube, Graphene etc.). The nano wire conductive filler material of sheets of conductive filler and one-dimentional structure according to the conduction known two-dirnentional structure of seepage theory more is conducive to obtaining low seepage flow threshold value and high specific conductivity than conventional particulate state, the conductive filler material such as spherical.
In the conductive filler material of two-dirnentional structure, Graphene is paid close attention to widely because the features such as the electrical property of its excellence, thermal characteristics and huge specific surface area receive. How Graphene is effectively evenly dispersed in polymeric matrix, avoids Graphene each other because strong Van der Waals force is reunited and cause performance sharply to decline, be take Graphene as one of conductive filler material key issue preparing conducing composite material.
In order to realize effective dispersion of Graphene, patent CN102964713A is with N, dinethylformamide solvent dispersion graphene oxide, disperses polystyrene with chlorine first ether, by the two blended, take out filter, washing, drying and other steps prepared functionalization graphene core-shell nano hybrid material. Although the method achieves Graphene even dispersion in the polymer, but employs a large amount of noxious solvent. In order to avoid the use of noxious solvent, patent CN104261403A forms the loose liquid of uniform water with the electrostatic interaction between polystyrene moulding and graphene oxide. Patent CN104650521A is with cation polystyrene and graphene oxide compound, the certainly poly-of Graphene can be suppressed, and induce Selective graphene to be distributed in polymer beads sub-surface, forming perfect Graphene three-dimensional network skeleton, prepared matrix material shows extremely low Chongqing of leading and oozes value and higher electric conductivity. Patent CN103554702A is with graphene coated polystyrene, and has prepared the network-like Graphene polymer composite of a kind of Graphene through cast or pressing mold.
The nano-material of one-dimentional structure, because having high length-diameter ratio characteristic, can reduce seepage flow threshold value, it is to increase specific conductivity using it as conductive filler material. Patent CN1873838A for polymeric matrix, has prepared the polymkeric substance composite conducting material of high conductivity by compounded mix of nano silver wire and silver powder, taking acrylic resin. Patent CN104974500A discloses a kind of polymer base conductive composite material and its preparation method that contain metal nanometer line and graphene oxide, by adding the not electric conductive oxidation Graphene of a small amount of sheet in the polymer matrix composite of metal nanometer line, prevent the reunion of metal nanometer line on the one hand, the sinking of metal nanometer line can be stoped on the other hand, therefore the dispersion of metal nanometer line is more even, thus electroconductibility is improved. But the method is only applicable to water-soluble polymeric matrix, having bigger limitation, simultaneous oxidation Graphene only plays stable dispersant effect, does not have electroconductibility. In order to combine the advantage of two dimension with one-dimensional electric filler, patent CN104992781A is with Graphene, nano silver wire and poly-(3,4-enedioxy thiophene): poly styrene sulfonate is that a kind of graphene-based tri compound transparent conductive film prepared by raw material, improve the photoelectric properties of graphene-based transparent conductive film, but this material is conductive film, but not the matrix material of body conduction.
Summary of the invention
In view of this, in order to overcome defect and the problem of prior art, the present invention provides a kind of composite conducting polymer material.
A kind of composite conducting polymer material, is made up of the Graphene of the conducting nanowires of one-dimentional structure, two-dirnentional structure and spherical polymer matrix, and each constituent mass proportioning is as follows:
The conducting nanowires of one-dimentional structure 5��40 parts
The Graphene of two-dirnentional structure 0.5��5 part
Spherical polymer matrix 55��90 parts.
In certain embodiments, described conducting nanowires is one or more in nano silver wire, copper nano-wire, nanowires of gold, nickel nano wire, aluminium nano wire, Fe nanowire, Single Walled Carbon Nanotube and multi-walled carbon nano-tubes.
In certain embodiments, described conducting nanowires length is 5��500 ��m, diameter 30��300nm.
In certain embodiments, described spherical polymer matrix is one or more in spherical polystyrene type, polymethacrylate, polyacrylate(s), cinnamic acrylic ester analog copolymer, vinylformic acid-methyl acrylic ester multipolymer, polyacrylamide, polyethylene, resol, polysiloxane, phenyl silicone.
In certain embodiments, described spherical polymer diameter is 200nm��10 ��m.
In addition, present invention also offers the preparation method of a kind of composite conducting polymer material, comprise the steps:
Step S10: the polymer/graphene composite material preparing graphene coated polymkeric substance
The aqueous dispersions of graphene oxide is mixed with the aqueous dispersions of spherical polymer, makes graphene oxide evenly be coated on spherical polymer surface, obtain the matrix material of graphene oxide coated polymer;
Then the matrix material of described graphene oxide coated polymer is carried out in-situ chemical reduction, obtain the matrix material of redox graphene coated polymer;
By washing, after removing unreacted impurity, again it is dispersed in deionized water, obtains the polymer/graphene composite material of graphene coated polymkeric substance;
Step S20: the polymer/graphene/conducting nanowires mixture of preparation multidimensional hybrid structure
The aqueous dispersions of described conducting nanowires is joined in the aqueous dispersions of described polymer/graphene composite material prepared by step (1), mix, obtain the polymer/graphene/conducting nanowires mixed dispersion liquid of multidimensional hybrid structure;
Take out elimination except water medium, then drying obtains the polymer/graphene/conducting nanowires mixture of multidimensional hybrid structure;
Step S30: the polyradical conducing composite material of preparation multidimensional hybrid structure
The polymer/graphene of multidimensional hybrid structure prepared by step (2)/conducting nanowires mixture compression molding, obtaining the polyradical conducing composite material of multidimensional hybrid structure, in the composite conducting polymer material of described multidimensional hybrid structure, the quality proportioning of each component is as follows:
The conducting nanowires of one-dimentional structure 5��40 parts
The Graphene of two-dirnentional structure 0.5��5 part
Spherical polymer matrix 55��90 parts.
In certain embodiments, in step S10, prepare the polymer/graphene composite material of graphene coated polymkeric substance, specifically comprise the steps:
The aqueous dispersions of graphene oxide is mixed with the aqueous dispersions of spherical polymer, use positively charged ion spherical polymer or by regulating pH value of solution to 1��6 to make graphene oxide evenly be coated on spherical polymer surface, obtain the matrix material of graphene oxide coated polymer.
In certain embodiments, in step S10, graphene oxide in-situ reducing method is chemical reduction, and reductive agent is the one in hydrazine hydrate, dimethylhydrazine, hydroiodic acid HI, sodium borohydride, POTASSIUM BOROHYDRIDE, vitamins C, strong aqua.
In certain embodiments, in step S30, described compression molding is for colding pressing or heating and mould pressing, and the condition of colding pressing is: temperature is room temperature, and pressure is 1-30MPa, time 10min��3h; Pressurized conditions is: temperature (Tg+10)��(Tg+50) DEG C, Tg are glass transition temperature of polymer, pressure 1-30MPa, time 2min��2h.
Relative to prior art, composite conducting polymer material provided by the invention, by the conducting nanowires of one-dimentional structure, the Graphene of two-dirnentional structure and spherical polymer matrix composition, combine the advantage of one-dimensional electric nano-material and two-dimensional graphene, by carrying out compound with the high length-diameter ratio one-dimensional electric nano wire with excellent electrical again after two-dimensional graphene and polymer-based carbon volume recombination, thus improve the dispersing uniformity of conductive filler material in polymeric matrix, add the touch opportunity between conductive filler material in polymer composites, utilize the synergy of one-dimensional electric nano wire and two-dimensional graphene, construct efficient conductive path network, improve the electroconductibility of polymer composites.
In addition, present invention also offers the preparation method of composite conducting polymer material, by preparing the polymer/graphene composite material of graphene coated polymkeric substance, preparing the polymer/graphene/conducting nanowires mixture of multidimensional hybrid structure again, finally prepare the polyradical conducing composite material of multidimensional hybrid structure, this preparation method technique is simple, recombination process is without the need to using poisonous and harmful solvent, environmental protection, the matrix material quality height of preparation, good conductivity.
Meanwhile, owing to adopting the graphene oxide of two-dirnentional structure evenly to disperse and in-situ reducing in spherical polymer matrix, the conductive path of networking is formed, the favourable electroconductibility improving polymer composites; The conducting nanowires of one-dimentional structure and redox graphene evenly disperse and are in close contact, and the synergy of the two impels the further raising of polymer composites electroconductibility.
Accompanying drawing explanation
The polymer base conductive composite material of Fig. 1 multidimensional hybrid structure and preparation process schematic diagram thereof.
Polymer/graphene/conducting nanowires mixture SEM that Fig. 2 is multidimensional hybrid structure prepared by embodiment 1 schemes.
The partial enlargement SEM that Fig. 3 is the polymer/graphene/conducting nanowires mixture of multidimensional hybrid structure prepared by embodiment 1 schemes.
The section SEM that Fig. 4 is the polymer-matrix electric conduction material of multidimensional hybrid structure prepared by embodiment 1 schemes.
Embodiment
For the ease of understanding the present invention, below with reference to relevant drawings, the present invention is described more fully. Accompanying drawing gives the better embodiment of the present invention. These are only the preferred embodiments of the present invention; not thereby the patent scope of the present invention is limited; every utilize specification sheets of the present invention and accompanying drawing content to do equivalent structure or equivalence flow process conversion; or directly or indirectly it is used in other relevant technical fields, all it is included in the scope of patent protection of the present invention with reason.
Unless otherwise defined, all technology used herein are identical with the implication that the those skilled in the art belonging to the present invention understand usually with scientific terminology. The term used in the description of the invention herein is the object in order to describe concrete enforcement mode, is not intended to be restriction the present invention. Term as used herein " and/or " comprise arbitrary and all combinations of one or more relevant Listed Items.
Composite conducting polymer material provided by the invention, is made up of the Graphene of the conducting nanowires of one-dimentional structure, two-dirnentional structure and spherical polymer matrix, and each constituent mass proportioning is as follows:
The conducting nanowires of one-dimentional structure 5��40 parts
The Graphene of two-dirnentional structure 0.5��5 part
Spherical polymer matrix 55��90 parts.
Preferably, described conducting nanowires is one or more in nano silver wire, copper nano-wire, nanowires of gold, nickel nano wire, aluminium nano wire, Fe nanowire, Single Walled Carbon Nanotube and multi-walled carbon nano-tubes.
Preferably, described conducting nanowires length is 5��500 ��m, diameter 30��300nm.
Preferably, described spherical polymer matrix is one or more in spherical polystyrene type, polymethacrylate, polyacrylate(s), cinnamic acrylic ester analog copolymer, vinylformic acid-methyl acrylic ester multipolymer, polyacrylamide, polyethylene, resol, polysiloxane, phenyl silicone.
Preferably, described spherical polymer diameter is 200nm��10 ��m.
It is appreciated that, composite conducting polymer material provided by the invention, by the conducting nanowires of one-dimentional structure, the Graphene of two-dirnentional structure and spherical polymer matrix composition, combine the advantage of one-dimensional electric nano-material and two-dimensional graphene, by carrying out compound with the high length-diameter ratio one-dimensional electric nano wire with excellent electrical again after two-dimensional graphene and polymer-based carbon volume recombination, thus improve the dispersing uniformity of conductive filler material in polymeric matrix, add the touch opportunity between conductive filler material in polymer composites, utilize the synergy of one-dimensional electric nano wire and two-dimensional graphene, construct efficient conductive path network, improve the electroconductibility of polymer composites.
Refer to Fig. 1, it is the polymer base conductive composite material of preparation method and the preparation process schematic diagram thereof of composite conducting polymer material provided by the invention, comprises the steps:
Step S10: the polymer/graphene composite material preparing graphene coated polymkeric substance
The aqueous dispersions of graphene oxide is mixed with the aqueous dispersions of spherical polymer, makes graphene oxide evenly be coated on spherical polymer surface, obtain the matrix material of graphene oxide coated polymer;
Then the matrix material of described graphene oxide coated polymer is carried out in-situ chemical reduction, obtain the matrix material of redox graphene coated polymer;
By washing, after removing unreacted impurity, again it is dispersed in deionized water, obtains the polymer/graphene composite material of graphene coated polymkeric substance;
Step S20: the polymer/graphene/conducting nanowires mixture of preparation multidimensional hybrid structure
The aqueous dispersions of described conducting nanowires is joined in the aqueous dispersions of described polymer/graphene composite material prepared by step (1), mix, obtain the polymer/graphene/conducting nanowires mixed dispersion liquid of multidimensional hybrid structure;
Take out elimination except water medium, then drying obtains the polymer/graphene/conducting nanowires mixture of multidimensional hybrid structure;
Step S30: the polyradical conducing composite material of preparation multidimensional hybrid structure
The polymer/graphene of multidimensional hybrid structure step (2) prepared/conducting nanowires mixture compression molding, obtains the polyradical conducing composite material of multidimensional hybrid structure.
It can be appreciated that the above-mentioned preparation method of the present invention is owing to adopting the graphene oxide of two-dirnentional structure evenly to disperse and in-situ reducing in spherical polymer matrix, form the conductive path of networking, the favourable electroconductibility improving polymer composites; The conducting nanowires of one-dimentional structure and redox graphene evenly disperse and are in close contact, and the synergy of the two impels the further raising of polymer composites electroconductibility.
Embodiment 1:
Get the graphene oxide aqueous dispersions of 10mL5mg/mL (1 mass parts), the particle diameter joining 89mL5wt% (89 mass parts) is about in the polystyrene spheres water-dispersion of 440nm, magnetic agitation is even, slowly drip and add hydrochloric acid soln, mixing solutions pH is adjusted to 2, stirs lower mixing 30min and obtain the coated spherical poly styrene composite material mixing solutions of graphene oxide; The water-bath that above-mentioned mixing solutions is placed in 80 DEG C, adds the hydrazine hydrate of 5ml85%, terminates, obtain the mixing solutions of redox graphene coated poly styrene composite material under magnetic agitation after reacting 3h. This mixing solutions is taken out filter, wash many all over removing after unreacted impurity, again it is dispersed in 100mL deionized water, again toward the nano silver wire aqueous dispersions wherein adding 10mL5wt% (10 mass parts), dispersed with stirring is even, obtains the polystyrene/Graphene/nano silver wire blending dispersion solution of multidimensional hybrid structure. Take out elimination except water medium, put into 60 DEG C of baking ovens dry, dried powder is put into mould, 180 DEG C, suppress the polymer base conductive composite material that 10min obtains multidimensional hybrid structure under 15MPa. In the polymer base conductive composite material of multidimensional hybrid structure prepared by this embodiment, the mass ratio of the nano silver wire of one-dimentional structure and the Graphene of two-dirnentional structure and polymeric matrix is 10:1:89, and specific conductivity is about 250S/m.
Refer to Fig. 2, Fig. 3 and Fig. 4, polymer/graphene/conducting nanowires mixture the SEM being respectively multidimensional hybrid structure prepared by embodiment 1 schemes, and the section SEM of the partial enlargement SEM figure of the polymer/graphene of multidimensional hybrid structure/conducting nanowires mixture and the polymer-matrix electric conduction material of multidimensional hybrid structure schemes.
Embodiment 2:
Get the graphene oxide aqueous dispersions of 30mL5mg/mL (3 mass parts), the particle diameter joining 70mL5wt% (70 mass parts) is about in the poly (methyl methacrylate) micro-sphere water-dispersion of 2.2 ��m, magnetic agitation is even, slowly drip and add hydrochloric acid soln, mixing solutions pH is adjusted to 3, stirs lower mixing 30min and obtain the coated spherical composite material of polymethyl methacrylate mixing solutions of graphene oxide; The water-bath that above-mentioned mixing solutions is placed in 100 DEG C, adds the hydroiodic acid HI of 5ml45%, terminates, obtain the mixing solutions of redox graphene coated composite material of polymethyl methacrylate under magnetic agitation after reacting 10h. This mixing solutions is taken out filter, wash many all over removing after unreacted impurity, again it is dispersed in 100mL deionized water, again toward the copper nano-wire aqueous dispersions wherein adding 27mL5wt% (27 mass parts), dispersed with stirring is even, obtains the polymethylmethacrylate/Graphene/copper nano-wire blending dispersion solution of multidimensional hybrid structure. Taking out elimination except water medium, the vacuum drying oven putting into 40 DEG C is dry, dried powder is put into mould, suppresses the polymer base conductive composite material that 30min obtains multidimensional hybrid structure under room temperature, 30MPa. In the polymer base conductive composite material of multidimensional hybrid structure prepared by this embodiment, the mass ratio of the nano silver wire of one-dimentional structure and the Graphene of two-dirnentional structure and polymeric matrix is 27:3:70, and specific conductivity is about 1080S/m.
The above embodiment only have expressed several enforcement modes of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to patent scope of the present invention. , it is also possible to make some distortion and improvement, it should be appreciated that for the person of ordinary skill of the art, without departing from the inventive concept of the premise these all belong to protection scope of the present invention. Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (9)
1. a composite conducting polymer material, it is characterised in that, it is made up of the Graphene of the conducting nanowires of one-dimentional structure, two-dirnentional structure and spherical polymer matrix, each constituent mass proportioning is as follows:
The conducting nanowires of one-dimentional structure 5��40 parts
The Graphene of two-dirnentional structure 0.5��5 part
Spherical polymer matrix 55��90 parts.
2. composite conducting polymer material as claimed in claim 1, it is characterized in that, described conducting nanowires is one or more in nano silver wire, copper nano-wire, nanowires of gold, nickel nano wire, aluminium nano wire, Fe nanowire, Single Walled Carbon Nanotube and multi-walled carbon nano-tubes.
3. composite conducting polymer material as claimed in claim 2, it is characterised in that, described conducting nanowires length is 5��500 ��m, diameter 30��300nm.
4. composite conducting polymer material as claimed in claim 1, it is characterized in that, described spherical polymer matrix is one or more in spherical polystyrene type, polymethacrylate, polyacrylate(s), cinnamic acrylic ester analog copolymer, vinylformic acid-methyl acrylic ester multipolymer, polyacrylamide, polyethylene, resol, polysiloxane, phenyl silicone.
5. composite conducting polymer material as claimed in claim 4, it is characterised in that, described spherical polymer diameter is 200nm��10 ��m.
6. the preparation method of a composite conducting polymer material as claimed in claim 1, it is characterised in that, comprise the steps:
Step S10: the polymer/graphene composite material preparing graphene coated polymkeric substance
The aqueous dispersions of graphene oxide is mixed with the aqueous dispersions of spherical polymer, makes graphene oxide evenly be coated on spherical polymer surface, obtain the matrix material of graphene oxide coated polymer;
Then the matrix material of described graphene oxide coated polymer is carried out in-situ chemical reduction, obtain the matrix material of redox graphene coated polymer;
By washing, after removing unreacted impurity, again it is dispersed in deionized water, obtains the polymer/graphene composite material of graphene coated polymkeric substance;
Step S20: the polymer/graphene/conducting nanowires mixture of preparation multidimensional hybrid structure
The aqueous dispersions of described conducting nanowires is joined in the aqueous dispersions of described polymer/graphene composite material prepared by step (1), mix, obtain the polymer/graphene/conducting nanowires mixed dispersion liquid of multidimensional hybrid structure;
Take out elimination except water medium, then drying obtains the polymer/graphene/conducting nanowires mixture of multidimensional hybrid structure;
Step S30: the polyradical conducing composite material of preparation multidimensional hybrid structure
The polymer/graphene of multidimensional hybrid structure prepared by step (2)/conducting nanowires mixture compression molding, obtaining the polyradical conducing composite material of multidimensional hybrid structure, in the composite conducting polymer material of described multidimensional hybrid structure, the quality proportioning of each component is as follows:
The conducting nanowires of one-dimentional structure 5��40 parts
The Graphene of two-dirnentional structure 0.5��5 part
Spherical polymer matrix 55��90 parts.
7. the preparation method of composite conducting polymer material as claimed in claim 6, it is characterised in that, in step S10, prepare the polymer/graphene composite material of graphene coated polymkeric substance, specifically comprise the steps:
The aqueous dispersions of graphene oxide is mixed with the aqueous dispersions of spherical polymer, use positively charged ion spherical polymer or by regulating pH value of solution to 1��6 to make graphene oxide evenly be coated on spherical polymer surface, obtain the matrix material of graphene oxide coated polymer.
8. the preparation method of composite conducting polymer material as claimed in claim 6, it is characterized in that, in step S10, graphene oxide in-situ reducing method is chemical reduction, and reductive agent is the one in hydrazine hydrate, dimethylhydrazine, hydroiodic acid HI, sodium borohydride, POTASSIUM BOROHYDRIDE, vitamins C, strong aqua.
9. the preparation method of composite conducting polymer material as claimed in claim 6, it is characterised in that, in step S30, described compression molding is for colding pressing or heating and mould pressing, and the condition of colding pressing is: temperature is room temperature, and pressure is 1-30MPa, time 10min��3h; Pressurized conditions is: temperature (Tg+10)��(Tg+50) DEG C, Tg are glass transition temperature of polymer, pressure 1-30MPa, time 2min��2h.
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