CN102786756A - Three-dimensional continuous graphene network composite material and its preparation method - Google Patents
Three-dimensional continuous graphene network composite material and its preparation method Download PDFInfo
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Abstract
The invention belongs to the nanocomposite material field, and relates to a preparation method of a novel three-dimensional graphene network composite material. The method comprises the following steps: obtaining a three-dimensional continuous graphene skeleton composite structure by adopting a metal template having a three-dimensional continuous pore structure as a catalyst, by growing the graphene through utilizing a chemical vapor deposition method until the graphene sklayer number is 1-20, and by adopting an etching liquid to remove the metal template; and compositing the graphene composite structure with a high polymer material to obtain the three-dimensional graphene network composite material. The three-dimensional graphene network composite material has the advantages of simple technology, easily controlled processes, excellent conductivity, and low preparation cost, and is suitable for the fields of solar cells, energy storage cells and conductive composite materials.
Description
Technical field
The invention belongs to field of nanometer material technology, relate to the network combined preparation methods of a kind of three-dimensional continuous graphite alkene, the network combined material of said three-dimensional continuous graphite alkene is mainly used in solar cell, energy-storage battery, heat radiation, anti-electrostatic field.
Background technology
Cellular lattice structure of the bidimensional that Graphene is made up of the carbon six-ring (2D) cycle, it is the elementary cell that makes up other dimension carbon-based material (soccerballene of 0D, the carbon nanotube of 1D and the graphite of 3D).The unique crystalline structure of Graphene makes it have excellent properties, like high heat conductance, high mechanical strength, peculiar electrical properties and optical property.Fields such as therefore, Graphene emission on the scene, electrode materials, composite functional material have broad application prospects.
Macromolecular material generally has advantages such as easy moulding, but is generally insulating material, thereby has limited its application in many aspects.For making it become conductor or semi-conductor, can adopt the method for adding conductive filler material.Use the conductive additive of Graphene, because the high electronic mobility and excellent electrical properties of Graphene only needs to add can reach the conduction requirement on a small quantity as macromolecular material.In addition, if will prepare micron or the nano-graphene three-dimensional framework not only can further improve the conduction property of matrix material as filler, and can also give the characteristic of the many uniquenesses of matrix material.As: because the skeleton structure of Graphene has the super strength high molecule mechaanical property of materials.In addition, the Graphene skeleton can improve the heat conductivility of matrix material, is applied to semi-conductor industry as good heat sink material.Simultaneously, the compound fields such as lithium cell and ultracapacitor that are applied to as electrode materials of Graphene skeleton and conducting polymer composite.
Attempted at present Graphene three-dimensional framework and macromolecular material compound [Zongping Chen, Wencai Ren, Libo Gao; Bilu Liu, Songfeng Pei, Hui-Ming Cheng; Nature Materials, 2011, DOI:10.1038/NMAT3001]; But the used Graphene number of plies is uncontrollable, particularly the three-dimensional framework of minority layer graphene.In addition, used three-dimensional framework adopts organic solvent to remove in the propping material process, and three-dimensional framework is difficult to intact reservation, and complicated process of preparation can't be organic compound with macromolecular material, and this will have a strong impact on the over-all properties of three-dimensional Graphene skeleton matrix material.
Summary of the invention
In order to improve the composite conducting material conductivity and to simplify technology; The present invention proposes the network combined preparation methods of a kind of three-dimensional continuous graphite alkene; Metal form with the continuous pore structure of three-dimensional is a catalyzer, utilizes the chemical Vapor deposition process magnanimity to prepare three-dimensional continuous graphite alkene skeleton; This Graphene skeleton and high score material are organically combined the three-dimensional Graphene network structure matrix material of preparation.The present invention need not to remove the skeleton supporter, can obtain the Graphene three-dimensional network matrix material that the number of plies is controlled, skeleton is complete, and this composite material preparation process is simple; Process is easy to control; Conductivity is excellent, and preparation cost is low, is suitable for solar cell, energy-storage battery, heat radiation, anti-electrostatic field.
One aspect of the present invention provides a kind of three-dimensional continuous graphite alkene network combined preparation methods, and it is characterized in that: the network combined material of said Graphene is made up of Graphene and macromolecular material, and said method comprises:
(1) metal form with the continuous pore structure of three-dimensional is a catalyzer, puts into chemical vapor deposition reaction chamber, is heated to temperature of reaction 400-1000 ℃; After constant temperature 0-60 minute; Import carbon source, hydrogen and protection gas, gas flow is 1-1000sccm, reaction times 1-60 minute; Reaction finishes postcooling to room temperature, and preferably controlling rate of temperature fall is 10-300 ℃/minute;
Is (2) the Graphene three-dimensional net structure that step (1) is obtained put into solution (what solution?) in, deposit framework material from the teeth outwards;
(3) after baking and curing, put into etching liquid, remove the metal form catalyzer;
(4) use deionized water wash, obtain three-dimensional successive Graphene skeleton composite structure;
(5) place macromolecular solution to soak three-dimensional Graphene skeleton composite structure and disperseed 1-48 hour, and under air, nitrogen, argon gas or hydrogen-argon-mixed atmosphere, solidified, solidification value is 100-400 ℃, and be 10-200 minute set time.
In one embodiment of the present invention; Said macromolecular material is selected from pvdf, Vinylpyrrolidone polymer, polyoxyethylene glycol, Z 150PH, polymethylmethacrylate, Vilaterm, SE, Vestolen PP 7052, tetrafluoroethylene, resol, polyamide resin and rubber resin, and the massfraction of Graphene in macromolecular material is 0.1%-10%.
In one embodiment of the present invention, the three-dimensional metal form of pore structure continuously that adopts in the step (1) is commercially available foam iron, foam copper, foam cobalt, nickel foam and foam ruthenium, and area density is 100-3000g/m
2, hole count is 10-300, thickness is 0.5-50mm.
In one embodiment of the present invention, the carbon source that chemical vapour deposition is adopted in the step (1) comprises: gaseous carbon source, liquid carbon source and solid-state carbon source; Said protection gas bag is drawn together: nitrogen, argon gas, helium and their gas mixture.Said gaseous carbon source is selected from methane, ethene, acetylene, ethane, propane and their gas mixture; Said liquid carbon source is selected from methyl alcohol, ethanol, propyl alcohol and their mixing liquid; And said solid-state carbon source is selected from pvdf, Vinylpyrrolidone polymer, polyoxyethylene glycol, Z 150PH, polymethylmethacrylate, YSR 3286.
In one embodiment of the present invention, etching liquid described in the step (3) is hydrochloric acid, sulfuric acid, nitric acid, iron trichloride and their mixing solutions, and etching temperature is 30-80 ℃, and etching time is 20-800 minute.
In the present invention, the Graphene three-dimensional net structure aperture that step (1) obtains is 50-600 μ m, and the Graphene number of plies is 1-20.
In one embodiment of the present invention; Sedimentary framework material is identical with macromolecular material in the matrix material in the step (2); Be selected from pvdf, Vinylpyrrolidone polymer, polyoxyethylene glycol, Z 150PH, Vilaterm, SE, Vestolen PP 7052, tetrafluoroethylene, polymethylmethacrylate, resol, polyamide resin and rubber resin.
The present invention also provides the three-dimensional continuous graphite alkene that makes according to preparation method according to the invention network combined material, and the network combined material of said three-dimensional continuous graphite alkene as conduction, heat conduction and/or heat radiation matrix material in solar cell, energy-storage battery, heat radiation, anti-electrostatic Application for Field.
The network combined preparation methods of three-dimensional continuous graphite alkene according to the invention need not to remove the skeleton supporter; Can obtain the Graphene three-dimensional network matrix material that the number of plies is controlled, skeleton is complete, this composite material preparation process is simple, and process is easy to control; Conductivity is excellent; Facility investment is few, can scale operation, have broad application prospects in solar cell, energy-storage battery, heat radiation, anti-electrostatic field.
Description of drawings
Fig. 1: be the stereoscan photograph of three-dimensional Graphene skeleton composite structure;
Fig. 2: be the stereoscan photograph of the three-dimensional Graphene skeleton that caves in;
Fig. 3: be Raman (Raman) spectrum of three-dimensional Graphene skeleton;
Fig. 4: the curve that changes with Graphene (GF) composition for the specific conductivity of Graphene/composite material of polymethyl methacrylate.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is elaborated, but protection domain of the present invention is not limited thereto.
Embodiment 1
(1) adopt commercially available foam copper (available from novel material company of Changsha power unit) metal form in the chemical vapour deposition reactor furnace of packing into, to feed 100sccm hydrogen and 100sccm argon gas as catalyzer; Begin to be heated to 800 ℃ after 60 minutes; Constant temperature feeds 80sccm methane after 30 minutes, in 30 minutes reaction times, reaction stops through methane after finishing; Close electric furnace, naturally cool to room temperature;
(2) product that step (1) is obtained takes out the back 100 ℃ of oven dry 3 hours in the aqueous solution of 4wt% Z 150PH, make its surface deposition layer of polyethylene alcohol, puts into 100ml 1M hydrochloric acid and 1M FeCl
3Stirred 4 hours in the solution, remove metallic copper, obtain three-dimensional Graphene/Z 150PH skeleton composite structure, stereoscan photograph is as shown in Figure 1.As remove the Z 150PH supporter, and the Graphene skeleton partly caves in, and is difficult to intact reservation, and as shown in Figure 2, the gained Graphene is 1-3 atomic shell (like Fig. 3).
(3) the three-dimensional Graphene of 3wt%/Z 150PH skeleton structure is put into polyvinyl alcohol water solution, vacuum filtration solidified 5 hours at 120 ℃, the Graphene/polyvinyl alcohol composite material of acquisition, and its specific conductivity is as shown in Figure 4.
The preparation method is basically with embodiment 1, and difference is: in the step (1), adopting the nickel foam through ethanol, acetone and Virahol ultrasonic cleaning is catalyzer; It is immersed the N of YSR 3286, in N two-dimethyl formamide solution, obtain nickel foam/YSR 3286 composite structure; Through 100sccm hydrogen, 100sccm nitrogen, 30 minutes reaction times; Raman spectrum is as shown in Figure 2, and the Graphene number of plies is 3-10; In the step (2),, adopt the concentrated hydrochloric acid nickel that defoams at nickel foam surface deposition one deck pvdf; In the step (5), 2wt% Graphene three-dimensional framework and pvdf is compound, and solidification value is 60 ℃, and be 10 hours set time, and gained Graphene/polyvinylidene fluoride composite material specific conductivity is 15.3S/cm.
Claims (10)
1. network combined preparation methods of three-dimensional continuous graphite alkene, it is characterized in that: the network combined material of said Graphene is made up of Graphene and macromolecular material, and said method comprises:
(1) metal form with the continuous pore structure of three-dimensional is a catalyzer; Put into chemical vapor deposition reaction chamber, be heated to temperature of reaction 400-1000 ℃, after constant temperature 0-60 minute; Import carbon source, hydrogen and protection gas; Gas flow is 1-1000sccm, and reaction times 1-60 minute, reaction finished postcooling to room temperature;
(2) the Graphene three-dimensional net structure that step (1) is obtained is put into the solution of macromolecular material, deposits the high-molecular bone frame material from the teeth outwards;
(3) after baking and curing, put into etching liquid, remove the metal form catalyzer;
(4) use deionized water wash, obtain three-dimensional successive Graphene skeleton composite structure;
(5) placing macromolecule material solution to soak three-dimensional Graphene skeleton composite structure disperseed 1-48 hour; Under air, nitrogen, argon gas or hydrogen-argon-mixed atmosphere, solidify; Solidification value is 100-400 ℃; Be 10-200 minute set time, obtains the network combined material of three-dimensional continuous graphite alkene thus.
2. preparation method according to claim 1; It is characterized in that; Said macromolecular material is selected from pvdf, Vinylpyrrolidone polymer, polyoxyethylene glycol, Z 150PH, polymethylmethacrylate, Vilaterm, SE, Vestolen PP 7052, tetrafluoroethylene, resol, polyamide resin and rubber resin, and the massfraction of Graphene in macromolecular material is 0.1%-10%.
3. preparation method according to claim 1 is characterized in that: in the step (1), the three-dimensional metal form of pore structure continuously of employing is foam iron, foam copper, foam cobalt, nickel foam and foam ruthenium, and area density is 100-3000g/m
2, hole count is 10-300, thickness is 0.5-50mm.
4. preparation method according to claim 1 is characterized in that: in the step (1), the carbon source that chemical vapour deposition is adopted comprises: gaseous carbon source, liquid carbon source and solid-state carbon source; Said protection gas bag is drawn together: nitrogen, argon gas, helium and their gas mixture.
5. preparation method according to claim 4 is characterized in that: said gaseous carbon source is selected from methane, ethene, acetylene, ethane, propane and their gas mixture; Said liquid carbon source is selected from methyl alcohol, ethanol, propyl alcohol and their mixing liquid; And said solid-state carbon source is selected from pvdf, Vinylpyrrolidone polymer, polyoxyethylene glycol, Z 150PH, polymethylmethacrylate, YSR 3286.
6. preparation method according to claim 1 is characterized in that: in the step (3), said etching liquid is hydrochloric acid, sulfuric acid, nitric acid, iron trichloride and their mixing solutions, and etching temperature is 30-80 ℃, and etching time is 20-800 minute.
7. preparation method according to claim 1 is characterized in that: the Graphene three-dimensional net structure aperture that step (1) obtains is 50-600 μ m, and the Graphene number of plies is 1-20.
8. preparation method according to claim 1; It is characterized in that: sedimentary framework material is identical with macromolecular material in the matrix material in the step (2); Be selected from pvdf, Vinylpyrrolidone polymer, polyoxyethylene glycol, Z 150PH, Vilaterm, SE, Vestolen PP 7052, tetrafluoroethylene, polymethylmethacrylate, resol, polyamide resin and rubber resin.
9. the network combined material of three-dimensional continuous graphite alkene that makes according to each said preparation method of claim 1-8.
The network combined material of the said three-dimensional continuous graphite alkene of claim 9 as conduction, heat conduction and/or heat radiation matrix material in solar cell, energy-storage battery, heat radiation, anti-electrostatic Application for Field.
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