CN104231653A - Chemical bond riveted graphene laminated composite metamaterial, as well as preparation method and device of composite metamaterial - Google Patents
Chemical bond riveted graphene laminated composite metamaterial, as well as preparation method and device of composite metamaterial Download PDFInfo
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- CN104231653A CN104231653A CN201410354272.1A CN201410354272A CN104231653A CN 104231653 A CN104231653 A CN 104231653A CN 201410354272 A CN201410354272 A CN 201410354272A CN 104231653 A CN104231653 A CN 104231653A
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Abstract
The invention provides a chemical bond riveted graphene laminated composite metamaterial, as well as a preparation method and device of the composite metamaterial. The metamaterial mainly comprises a polymer material and graphene, wherein the graphene is uniformly distributed in the polymer material matrix; polymer layers on two sides of the graphene layer are crosslinked, and partial cross bonds penetrate a graphene micro-layer and perform chemical crosslinking with the polymer layer on the other side of the graphene layer; and chemical bonds are riveted with the graphene layer to form the composite metamaterial. According to the composite metamaterial, the graphene or graphene oxide, flow-state polymer resin and auxiliaries are subjected to nano-scale alternate lamination by utilizing the effect of a laminator, the graphene is highly oriented along the flowing direction, and a polymer micro-layer mixed with a crosslinking agent and a crosslink promoter is interlaminated, and then polymers on two sides of the graphene layer carry out a crosslinking reaction by means of heating and pressurizing or high-energy ray radiation. The preparation method and the device are used for producing the organic inorganic composite metamaterial with simple process, little energy consumption, wide raw material source and low cost.
Description
Technical field
The invention belongs to organic/inorganic composite material and production technical field thereof.Relate generally to and adopt lamination device to prepare polymer chemistry key riveted Graphene organo-mineral complexing Meta Materials and preparation method thereof and device.
Background technology
Graphene is as a kind of novel Two-dimensional Inorganic nano material, because of the nanostructure that it is exclusive, there is high physical strength, outstanding conductive performance, abundant source and workability, the series of advantages such as with low cost, be at present known the thinnest be the hardest nano material also, it is almost completely transparent, only absorb the light of 2.3%, thermal conductivity is up to 5300W/mK, higher than carbon nanotube and diamond, under normal temperature, its electronic mobility is again than CNT (carbon nano-tube) or silicon wafer height, and resistivity than copper or silver lower, for the material that resistivity is minimum in the world at present.Research shows, adds the mechanical property that a small amount of Graphene can strengthen polymkeric substance effectively in the polymer.The Young's modulus of polymkeric substance is multiplied along with the increase of Graphene content usually, and obtained matrix material has great using value in Defence business, military project and automobile industry, such as, prepare high-performance rubber tire, light vehicle shell etc.
In recent years, along with graphene oxide prepares the consummation of Graphene technique, be able to preparation in macroscopic quantity with the graphene oxide that cheap graphite-made obtains.But Graphene is typical two dimensional crystal, there is anisotropy, in the intensity perpendicular to lamella direction much smaller than the intensity in graphene sheet layer direction, and also there is very large difference in electroconductibility in both direction and thermal conductivity.Further, at present there is Graphene in polymeric matrix, arrange the series of problems such as unordered, irregular structure in existing graphene composite material obtained by method, and it is lower that performance improves degree, is far from reaching desired index.
Chinese patent (patent publication No.: CN102675883A) refer to a kind of surface modified graphite alkene polymer base pressure drag matrix material and preparation method thereof, piezoresistance sensitivity degree has been prepared high by solution blended process, surface modified graphite alkene/silicon rubber pressure drag matrix material that pressure drag is reproducible, but it is freer graphene dispersion to be made in a polymer solution to distribute between graphene sheet layer, in a jumble, destroy the regular texture of Graphene, the excellent properties of two-dimensional directional can not be fully used, and the production cycle is long, the discontinuous production efficiency that causes of production process is low.
Summary of the invention
The object of the invention is to propose a kind of polymer chemistry key riveted Graphene lamination compound Meta Materials and preparation method thereof and device.Utilize the effect of lamination device, Graphene or graphene oxide and flowable state macromolecule resin and auxiliary agent is made to carry out the alternately laminated of nanoscale, Graphene is height-oriented and be mixed with the polymer microbedding of linking agent and crosslinking accelerator at Intercalation reaction along flow direction, afterwards by heating and pressurizing or high-energy ray irradiation, make the polymer generation crosslinking reaction of graphene layer both sides, macromolecule layer itself is cross-linked and has partial cross-linked key to penetrate Graphene microbedding (being particularly with pertusate graphene oxide etc.) and opposite side macromolecule layer generation chemically crosslinked, thus obtain polymer chemistry key riveted Graphene organo-mineral complexing Meta Materials.There is Graphene in polymeric matrix, arrange the series of problems such as unordered, irregular structure in the graphene composite material namely overcome obtained by prior art, performance is improved.
The chemical bond riveted Graphene lamination compound Meta Materials that the present invention proposes, it is characterized in that, the macromolecule layer of graphene layer both sides itself is cross-linked and has partial cross-linked key to penetrate Graphene microbedding (being particularly with pertusate graphene oxide etc.) and opposite side macromolecule layer generation chemically crosslinked.
Chemical bond riveted Graphene lamination compound Meta Materials of the present invention, in preparation process, in advance to Graphene or graphene oxide process, obtain solution or the suspension of Graphene or graphene oxide, or Graphene or graphene oxide and macromolecule resin Homogeneous phase mixing obtain mixture, the differential method is adopted to carry out layering to Nano grade to graphene/graphene oxide layer, Graphene or graphene oxide and flowable state macromolecule resin and auxiliary agent carry out the alternately laminated of nanoscale, make Graphene height-oriented and be mixed with the polymer microbedding of linking agent and crosslinking accelerator at Intercalation reaction along flow direction, afterwards by heating and pressurizing or high-energy ray irradiation, polymer generation crosslinking reaction can fix graphene/graphene oxide layer, prepare have superpower, super tough, the organo-mineral complexing Meta Materials of the specific performances such as anisotropic conductive heat conduction.
Preparing chemical bond riveted Graphene lamination compound Meta Materials of the present invention the adopted method that achieves the above object is: the first step, using graphene/graphene oxide solution or suspension system and macromolecule resin and auxiliary agent as raw material, and raw material is used two or multiple stage forcing machine co-extrusion (base material kind quantity determines specifically to use the number of units of forcing machine needed for composite system), outlet of extruder is connected with junction station entrance, and multilayer dose converges through junction station; Second step, the raw material after converging enters multiple lamination device and carries out the processing of sufficient lamination and orientation, and the thickness of graphene/graphene oxide layer and adjacent high-molecular resin layer is close to single-layer graphene thickness; 3rd step, Composite Melt after stacked is joined in forming mould, polymer resin layer generation vulcanization reaction or crosslinking reaction that sulfuration or crosslinking reaction condition make graphene/graphene oxide layer both sides is applied in forming mould, and make partial cross-linked key penetrate Graphene mesh or its damaged hole and opposite side polymer resin layer generation chemical bond to be cross-linked, to realize the riveted of graphene/graphene oxide sheet interlayer.The present invention is the preparation method of the organo-mineral complexing Meta Materials that a kind of technique is simple, energy consumption is little, raw material sources are extensive, cost is low.
The another kind of preparation method that chemical bond riveted Graphene lamination compound Meta Materials of the present invention adopts is: be deployed into the high workability raw material of Graphene and macromolecule resin (as silicon rubber, urethane, nylon etc.) and polymerization starter, linking agent, promotor etc. processing raw material of mixing respectively, then the raw material type required for reaction, uses separate unit, two or multiple stage ram pump to stacked device feed respectively.Mold cavity is entered in the filling of stacked device high speed flow orientation, carry out the polymerization of macromolecular chemistry key riveted graphene sheet layer or crosslinked chemical reaction in a mold, obtain the molded, shaped articles of described polymer chemistry key riveted Graphene organo-mineral complexing Meta Materials.
The invention provides a kind of equipment preparing polymer chemistry key riveted Graphene lamination compound Meta Materials, described equipment comprises raw material premixing cell, mixes overlapping unit and vulcanization crosslinking unit, and its Raw premixing cell comprises three forcing machines or injector plasticizing apparatus: A forcing machine, B forcing machine and C forcing machine; Mix overlapping unit to be formed by junction station and multiple lamination device serial connection; Vulcanization crosslinking unit is vulcanizing press, injector or other moulding-forming equipment.Graphene/graphene oxide solvent system extruded by A forcing machine, B forcing machine extruding macromolecular resin and vulcanizing agent system, C forcing machine extruding macromolecular resin and adjuvant system, the graphene/graphene oxide solvent system that A forcing machine is extruded enters junction station A runner, the macromolecule resin that B forcing machine is extruded and a small amount of vulcanization system enter junction station B runner, the macromolecule resin that C forcing machine is extruded and adjuvant system enter junction station C runner, finally merge into one composite three-layer material to enter multiple lamination device and carry out abundant lamination, when the thickness of graphene layer and adjacent high-molecular resin layer is close to single-layer graphene thickness, the polymer resin layer generation crosslinking reaction of graphene layer both sides, cross-link bond penetrates mesh or its damaged hole riveted joint, realize the riveted of graphene film interlayer, end product enter the further vulcanization crosslinking of vulcanizing press prepare have superpower, super tough, the organo-mineral complexing Meta Materials of the specific performances such as anisotropic conductive heat conduction.
Chemical bond riveted Graphene of the present invention stacked compound Meta Materials preparation facilities, described junction station has three buswaies, material from A forcing machine enters junction station A channel, material from B forcing machine enters junction station channel B, material from C forcing machine enters junction station C-channel, the sectional area of three buswaies can regulate, simultaneously three feed extruder screw speeds can speed governing, so just can change the material rate of graphene/graphene oxide layer and two polymer resin layers in lamination compound Meta Materials.
Chemical bond riveted Graphene organo-mineral complexing Meta Materials preparation facilities of the present invention, described lamination device be n layer macromolecule melt that junction station is extruded in the width direction average mark be slit into m decile, 90-degree rotation when each decile melt continues flow forward in lamination compound producer and broadening m doubly, conflux into the rhythmo structure of n × m layer at exit end with adjacent melts layer mutually; If the lamination compound producer that series connection k is same, then n × m can be obtained
kthe layer composite material of layer.Wherein n, m and k are integers, m and k is not less than 2, n and is not less than 1.
The invention has the beneficial effects as follows:
1. a kind of polymer-based cross-link bond riveted Graphene lamination compound Meta Materials of the present invention, macromolecule layer is adopted to be cross-linked the riveted realizing graphene film interlayer, the two-dimensional graphene lamella arrangements making distribution more mixed and disorderly is more regular, there is hard and soft replacing and the microscopic pattern of network interpenetrating, increase substantially stripping strength and the toughness of two-dimensional graphene sheet interlayer, thus obtain the Meta Materials of the organic-inorganic nano lamination compound with specific performances such as superpower, super tough, anisotropic conductive heat conduction.
2, a kind of polymer chemistry key riveted Graphene lamination compound Meta Materials preparation method of the present invention and device, adopt the control of the lamination device matrix material number of plies convenient, after different raw material layerings, overlapping cross linking conditions can relatively goodly be grasped again, can adopt the plasticizing blending means of each self application before converging, chemical bond riveted Graphene lamination compound Meta Materials preparation method of the present invention and device have the advantage that technique is simple, energy consumption is little, raw material sources are extensive, cost is low.
Accompanying drawing explanation
Fig. 1 is chemical bond riveted Graphene lamination compound Meta Materials schematic diagram of the present invention.
Fig. 2 is with hole graphene oxide sheet layer microcosmic schematic diagram in chemical bond riveted Graphene lamination compound Meta Materials of the present invention.
Fig. 3 is the schematic diagram of chemical bond riveted Graphene lamination compound Meta Materials preparation facilities of the present invention.
Fig. 4 is chemical bond riveted Graphene lamination compound Meta Materials preparation facilities runner schematic diagram of the present invention.
In figure: 1. macromolecule resin and on a small quantity vulcanizing agent or other adjuvant system layer, 2. graphene/graphene oxide system layer, 3. graphene oxide hole, 4.A forcing machine, 5.B forcing machine, 6. junction station, 7. lamination device, 8. head, 9.C forcing machine, 10. junction station A runner, 11. junction station B runners, 12. lamination device runners, 13. junction station C runners.
Embodiment
Now by reference to the accompanying drawings patent of the present invention is described in detail as follows:
It is chemical bond riveted Graphene lamination compound Meta Materials schematic diagram of the present invention shown in Fig. 1, macromolecule resin and on a small quantity vulcanizing agent or other adjuvant system layer 1 define riveted construction with graphene/graphene oxide system layer 2, and graphene oxide hole 3 is passages of chemical bond riveted.Fig. 2 show further band hole graphene oxide sheet layer microtexture.
Chemical bond riveted Graphene lamination compound Meta Materials preparation method of the present invention, with the graphene/graphene oxide solution of high density (>1mg.ml-1) or suspension system, processing characteristics is excellent and be easy to crosslinked macromolecule resin and adopt the good vulcanizing agent of curability and promotor as raw material, in raw material premixing cell part, the graphene/graphene oxide solvent system that A forcing machine 4 is extruded enters junction station A runner 10, the macromolecule resin that B forcing machine 5 is extruded and a small amount of vulcanization system enter junction station B runner 11, the macromolecule resin that C forcing machine 9 is extruded and adjuvant system enter junction station C runner 13.
After three forcing machine co-extrusions, material enters the overlapping unit of mixing, as shown in Figure 3.The composite three-layer material being about 0.1mm through junction station 6 one strand thickness directly enters lamination device 7.After entering lamination device 7, composite three-layer material in the width direction average mark is slit into 4 deciles, half-twist when each decile melt continues flow forward in lamination device 7 and broadening 4 times, lamination device runner 12 is illustrated as shown in Figure 4, mutually confluxes into the rhythmo structure of 12 layers at exit end with adjacent melts layer.The lamination device 7 that this experiment adopts series connection 8 same, then can obtain 3 × (4
8the layer composite material of)=196608 layer.Can obtain now thickness in monolayer as calculated and be about 0.51nm, close to the thickness of single-layer graphene lamella (0.34nm), three layers of material enters head 8 after multiple lamination device 7 or other mould obtains required shape.
To the flaky composite material of gained after lamination device is fully overlapping, the vulcanization curve test carrying out being correlated with is to determine optimum curing time and cure conditions.Vulcanizing press Optimal Temperature, pressure and time are set, layer composite material is cross-linked.Time crosslinked, the cross-link bond between polymkeric substance can penetrate mesh or its damaged graphene oxide hole 3, realizes the riveted of graphene film interlayer.Graphene inlay polymer has toughening effect, can sum up the preparation method of the organic-inorganic nano lamination compound Meta Materials that a kind of technique is simple, energy consumption is little, raw material sources are extensive, cost is low through said process.
In above process, if graphene/graphene oxide solution or suspension system are not suitable for extruding, the mode injected continuously can be adopted, graphene/graphene oxide solution or suspension system are injected into junction station A runner 10, then enter after converging with unclassified stores and mix overlapping unit, the shearing preventing graphene/graphene oxide solution or suspension system from standing screw rod occurs broken.
The above is concrete instrument and supplies situation of the present invention, coordinates each figure to be explained.But the present invention is not limited to above-described concrete instrument and supplies process, any based on above-mentioned said for relevant device amendment or replacement, any based on the above-mentioned said local directed complete set for related process, as long as within the scope of realm of spirit of the present invention, all belong to the present invention.
Claims (9)
1. chemical bond riveted Graphene lamination compound Meta Materials, it is characterized in that: primarily of macromolecular material and Graphene composition, graphene uniform is distributed in macromolecular material matrix, the macromolecule layer of graphene layer both sides itself is cross-linked and has partial cross-linked key or penetrate Graphene microbedding and opposite side macromolecule layer generation chemically crosslinked, and chemical bond riveted graphene layer forms compound Meta Materials.
2. chemical bond riveted Graphene lamination compound Meta Materials according to claim 1, is characterized in that: Graphene is the pertusate graphene oxide of band.
3. chemical bond riveted Graphene lamination compound Meta Materials according to claim 1, is characterized in that: macromolecular material is the plastics that vulcanized rubber maybe can produce cross-link bond.
4. the preparation method of chemical bond riveted Graphene lamination compound Meta Materials according to claim 1, it is characterized in that: the first step, using graphene/graphene oxide solution or suspension system and macromolecule resin and auxiliary agent as raw material, and raw material is used two or multiple stage forcing machine co-extrusion, outlet of extruder is connected with junction station entrance, and multilayer dose converges through junction station; Second step, the raw material after converging enters multiple lamination device and carries out the processing of sufficient lamination and orientation, and the thickness of graphene/graphene oxide layer and adjacent high-molecular resin layer is close to single-layer graphene thickness; 3rd step, Composite Melt after stacked is joined in forming mould, polymer resin layer generation vulcanization reaction or crosslinking reaction that sulfuration or crosslinking reaction condition make graphene/graphene oxide layer both sides is applied in forming mould, and make partial cross-linked key penetrate Graphene mesh or its damaged hole and opposite side polymer resin layer generation chemical bond to be cross-linked, to realize the riveted of graphene/graphene oxide sheet interlayer.
5. the preparation method of chemical bond riveted Graphene lamination compound Meta Materials according to claim 4, A forcing machine is replaced with ram pump, adopt the mode injected continuously that graphene/graphene oxide solution or suspension system are injected into junction station A runner, and then enter after converging with unclassified stores and mix overlapping unit.
6. adopt the preparation facilities of the preparation method of chemical bond riveted Graphene lamination compound Meta Materials according to claim 4, it is characterized in that: mainly comprise raw material premixing cell, mix overlapping unit and vulcanization crosslinking unit, its Raw premixing cell comprises three forcing machines: A forcing machine, B forcing machine and C forcing machine; Mix overlapping unit to be formed by junction station and multiple lamination device serial connection; Vulcanization crosslinking unit is the forming mould of vulcanizing press, injector or other moulding-forming equipment; A forcing machine extrudes graphene/graphene oxide solution or suspension system, B forcing machine extruding macromolecular resin and vulcanizing agent system, C forcing machine extruding macromolecular resin and adjuvant system, the graphene/graphene oxide solvent system that A forcing machine is extruded enters junction station A runner, the macromolecule resin that B forcing machine is extruded and a small amount of vulcanization system enter junction station B runner, the macromolecule resin that C forcing machine is extruded and adjuvant system enter junction station C runner, finally merge into one composite three-layer material and enter multiple lamination device and carry out abundant lamination; The thickness of graphene layer and adjacent high-molecular resin layer is close to single-layer graphene thickness, and the further vulcanization crosslinking of forming mould that Composite Melt enters vulcanizing press prepares organo-mineral complexing Meta Materials goods.
7. the preparation facilities of chemical bond riveted Graphene lamination compound Meta Materials according to claim 6, it is characterized in that: described lamination device be n layer macromolecule melt that junction station is extruded in the width direction average mark be slit into m decile, 90-degree rotation when each decile melt continues flow forward in lamination compound producer and broadening m doubly, conflux into the rhythmo structure of n × m layer at exit end with adjacent melts layer mutually; If the lamination compound producer that series connection k is same, then n × m can be obtained
kthe layer composite material of layer.
8. the preparation facilities of chemical bond riveted Graphene lamination compound Meta Materials according to claim 6, is characterized in that: three the replaceable one-tenth of forcing machine, three ram pumps.
9. the preparation facilities of chemical bond riveted Graphene lamination compound Meta Materials according to claim 6, is characterized in that: three the replaceable one-tenth of forcing machine, three injector plasticizing apparatus, vulcanization crosslinking unit is the forming mould of injector.
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Application publication date: 20141224 |