CN106129353A - A kind of lithium battery graphene complex and preparation method thereof - Google Patents

A kind of lithium battery graphene complex and preparation method thereof Download PDF

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Publication number
CN106129353A
CN106129353A CN201610518542.7A CN201610518542A CN106129353A CN 106129353 A CN106129353 A CN 106129353A CN 201610518542 A CN201610518542 A CN 201610518542A CN 106129353 A CN106129353 A CN 106129353A
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lithium battery
graphite
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graphene
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党斌
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Suzhou Kemiao New Material Co Ltd
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    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
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    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
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    • H01G11/32—Carbon-based
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
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Abstract

This application discloses a kind of lithium battery graphene complex and preparation method thereof, raw material is trimethylolpropane polyoxyethylene polyoxypropylene ether, mesophase pitch, aromatic naphtha, graphite, sodium carboxymethyl cellulose, paraffin, perchloric acid, cobalt carbonate, titanium dioxide and methanol；Technique is simple, mild condition, has good electric conductivity, electrochemical lithium storage content is big, energy density is high, good cycle；Low in raw material price, operation is simple；Can be not only used for fuel cell oxygen reduction reaction non-precious metal catalyst, it may also be used for ultracapacitor, lithium ion battery homenergic field of storage and the field such as Industrial Catalysis, environmental treatment；Do not rely on large-scale instrument and equipment, the large-scale production of high-quality graphene and complex thereof can be realized.

Description

A kind of lithium battery graphene complex and preparation method thereof
Technical field
The application belongs to the preparation field of grapheme material, particularly relates to a kind of lithium battery graphene complex and system thereof Preparation Method.
Background technology
It addition, Graphene is almost fully transparent, only absorb the light of 2.3%.On the other hand, it is the finest and close, even Minimum gas atom (helium atom) also cannot penetrate.These features make it be highly suitable as the former of transparent electron product Material, such as transparent touch display screen, luminous plaque and solar panel.
As the thinnest, a kind of novel nano-material that maximum intensity, electrical and thermal conductivity performance are the strongest that have now been found that, Graphene Being referred to as " dark fund ", be " king of new material ", scientist even foretells that Graphene " will thoroughly change 21 century ".Very likely lift Play a subversiveness new technique new industrial revolution have swept the globe.
Actually Graphene is inherently present in nature, is simply difficult to separate single layer structure.Graphene is folded from level to level Getting up is exactly mesophase pitch, and the mesophase pitch of thick 1 millimeter comprises about 3,000,000 layer graphenes.Pencil is drawn on paper gently Crossing, which floor the most only layer graphene the vestige stayed it is possible to be.
Graphene is in 2004 in the lab, at that time, and two scientist An Delie of Univ Manchester UK Jim and the Ke Siteyanuowo love that disappears finds that they can obtain the thinnest mesophase by a kind of very simple method Colophonium thin slice.They separate mesophase pitch sheet from highly directional pyrolysis mesophase pitch, are then bonded on the two sides of thin slice On a kind of special adhesive tape, tear adhesive tape, just mesophase pitch sheet can be divided into two.The most so operate, then thin slice More and more thinner, finally, they have obtained the thin slice being only made up of one layer of carbon atom, here it is Graphene.After this, prepare graphite The new method of alkene emerged in an endless stream, through the development of 5 years, it has been found that, Graphene is brought into the field of industrialized production for time Within sight.Therefore, in subsequently three years, An Deliegaimu and Constantine's Nuo Woxiao love are at monolayer and double-layer graphite Being found that the quantum hall effect under integer quantum Hall effect and normal temperature condition in alkene system respectively, the most therefore they obtain 2010 annual Nobel Prizes in physics.
Before finding Graphene, most of physicisies are thought, thermodynamics fluctuation does not allow any two dimensional crystal having Exist at a temperature of limit.So, its discovery has shaken condensed matter physics academia immediately.Although theoretical and experiment circle is all thought Perfect two-dimensional structure cannot at non-absolute zero stable existence, but single-layer graphene is prepared out in an experiment.
Graphene has perfect two dimensional crystal structure, and its lattice is the hexagon surrounded by six carbon atom, thickness It it is an atomic layer.Between carbon atom bonded by σ, combination is sp2 hydridization, and it is the most excellent that these σ keys impart Graphene Different mechanical property and structural rigidity.The iron and steel that the hardness ratio of Graphene is best is strong 100 times, diamond to be exceeded.At stone In ink alkene, each carbon atom has the p electronics of a non-bonding, and these p electronics can move freely in crystal, and motion speed The 1/300 of the degree up to light velocity, imparts the electric conductivity that Graphene is good.Graphene is the transparent conductive material of a new generation, can Jian Guang district, the transmitance of four layer graphenes is suitable with traditional ito thin film, and at other wave band, the transmitance of four layer graphenes is remote Far above ito thin film.
The scientific circles that occur in of Graphene have evoked huge great waves.It has been found that Graphene has unusual leading Electrical property, beyond intensity and the fabulous light transmission of iron and steel decades of times, its appearance is expected to cause at hyundai electronics sciemtifec and technical sphere One takes turns revolution.In Graphene, electronics can extremely efficiently migrate, and traditional quasiconductor and conductor, such as silicon and copper are remote Graphene is not had to show well.Due to electronics and the collision of atom, the form of traditional quasiconductor and conductor heat releases one A little energy, within 2013, general computer chip wastes the electric energy of 72%-81% by this way, and Graphene is the most different, its electricity Sub-energy will not be depleted, and this makes it be provided with the good characteristic being not of the common run.
China also has the advantage of uniqueness in Graphene research, from a manufacturing perspective, as Graphene raw materials for production Mesophase pitch, enriches in China's energy storage, cheap.It addition, it is to hinder Graphene big that mass production and large scale produce The main factor that scale is commercial.And the up-to-date achievement in research of China the most successfully breaks through this two hang-up, manufacturing cost from 3 yuan/gram are down to by 5000 yuan/gram, solve a volume production difficult problem for this material.Chemical vapour deposition technique is utilized successfully to be manufactured that state The single-layer graphene of interior first 15 inches, and successfully graphene transparent electrode is applied on electric resistance touch screen, prepare 7 Inch Graphene touch screen.
The research worker of Chongqing Institute of Green and Intelligent Technology of the Chinese Academy of Sciences is showing the superpower printing opacity of single-layer graphene product Property and flexibility.
Graphene industrial technology innovation strategic alliances of China lead Bei Terui, Zheng Tai group, the hexa-atomic element in Changzhou, BOCO's collection Hispanic Graphene meeting has been participated in the representative of Tuan Dengsijia listed company, and signs with Italy, delegation of Sweden respectively Degree of depth strategic cooperation agreement, for " the Graphene whole world is merged, and China integrates ", the first shot was fired for strategy.Additionally, the whole world at the beginning of 3 months First batch of 30,000 volume production Graphene mobile phones are issued in Chongqing, open the New Times of Graphene commercial application.Graphene is selected in The planning of " 13 " new material makes a decision the most substantially, it is contemplated that within 2015, will become China's Graphene industry and break out the first year, along with society Can urbanization, technicalization, the development of hommization, design a kind of be difficult to be destroyed, productivity is high and the lithium battery that is produced on a large scale With graphene complex and preparation method thereof, with low cost, to meet the market demand, it is very important.
Summary of the invention
Solve the technical problem that:
The application is low for existing graphene complex productivity, easily by strong oxidizer destruction and high in cost of production technical problem, it is provided that A kind of lithium battery graphene complex and preparation method thereof.
Technical scheme:
A kind of lithium battery graphene complex, the raw materials by weight portion proportioning of described lithium battery graphene complex is such as Under: 100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, mesophase pitch 5-15 part, aromatic naphtha 4-8 part, graphite 2-6 Part, sodium carboxymethyl cellulose 1-3 part, paraffin 4-6 part, perchloric acid 8-12 part, cobalt carbonate 3-5 part, titanium dioxide 3-5 part, methanol 6-10 part.
As a preferred technical solution of the present invention: the raw materials by weight portion of described lithium battery graphene complex Proportioning is as follows: 100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, mesophase pitch 5 parts, aromatic naphtha 4 parts, 2 parts of graphite, Sodium carboxymethyl cellulose 1 part, 4 parts of paraffin, 8 parts of perchloric acid, cobalt carbonate 3 parts, titanium dioxide 3 parts, methanol 6 parts.
As a preferred technical solution of the present invention: the raw materials by weight portion of described lithium battery graphene complex Proportioning is as follows: 100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, mesophase pitch 15 parts, aromatic naphtha 8 parts, graphite 6 Part, sodium carboxymethyl cellulose 3 parts, 6 parts of paraffin, 12 parts of perchloric acid, cobalt carbonate 5 parts, titanium dioxide 5 parts, methanol 10 parts.
As a preferred technical solution of the present invention: the raw materials by weight portion of described lithium battery graphene complex Proportioning is as follows: 100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, mesophase pitch 10 parts, aromatic naphtha 6 parts, graphite 4 Part, sodium carboxymethyl cellulose 2 parts, 5 parts of paraffin, 10 parts of perchloric acid, cobalt carbonate 4 parts, titanium dioxide 4 parts, methanol 8 parts.
The preparation method of a kind of described lithium battery graphene complex, comprises the steps:
The first step: proportioning by weight weighs trimethylolpropane polyoxyethylene polyoxypropylene ether, mesophase pitch, aromatic hydrocarbons Oil, graphite, sodium carboxymethyl cellulose, paraffin, perchloric acid, cobalt carbonate, titanium dioxide and methanol；
Second step: at room temperature, by raw material in grinding machine for grinding 30-50 minute so that it is mix homogeneously；
3rd step: the raw material of mix homogeneously is placed in ceramic crucible with cover, then ceramic crucible with cover is put into tube furnace In high pure nitrogen protect under be first heated to 400-500 DEG C, insulation reaction 1-3 hour, be then further heated to 900- 1000 DEG C, insulation reaction 2-4 hour, prepared lithium battery graphene complex.
Beneficial effect:
A kind of lithium battery graphene complex of the present invention and preparation method thereof uses above technical scheme and prior art Compare, have following technical effect that 1, technique is simple, mild condition, have good electric conductivity, electrochemical lithium storage content big, Energy density is high, good cycle；2, low in raw material price, operation is simple；3, can be not only used for fuel cell oxygen also Former reaction non-precious metal catalyst, it may also be used for ultracapacitor, lithium ion battery homenergic field of storage and Industrial Catalysis, The fields such as environmental treatment；4, do not rely on large-scale instrument and equipment, the extensive life of high-quality graphene and complex thereof can be realized Produce, can be with the widespread production not division of history into periods for current material.
Detailed description of the invention
Embodiment 1:
Proportioning by weight weighs 100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, mesophase pitch 5 parts, aromatic hydrocarbons Oil 4 parts, 2 parts of graphite, sodium carboxymethyl cellulose 1 part, 4 parts of paraffin, 8 parts of perchloric acid, cobalt carbonate 3 parts, titanium dioxide 3 parts, methanol 6 Part.
At room temperature, by raw material grinding machine for grinding 30 minutes so that it is mix homogeneously.
The raw material of mix homogeneously is placed in ceramic crucible with cover, then ceramic crucible with cover is put in tube furnace It is first heated to 400 DEG C under high pure nitrogen protection, insulation reaction 1 hour, then it is further heated to 900 DEG C, insulation reaction 2 is little Time, prepared lithium battery graphene complex.
Technique is simple, mild condition, has good electric conductivity, electrochemical lithium storage content is big, energy density is high, cyclicity Can be good；Low in raw material price, operation is simple；Can be not only used for fuel cell oxygen reduction reaction non-precious metal catalyst, Can be additionally used in ultracapacitor, lithium ion battery homenergic field of storage and the field such as Industrial Catalysis, environmental treatment；It is independent of In large-scale instrument and equipment, the large-scale production of high-quality graphene and complex thereof can be realized.
Embodiment 2:
Proportioning by weight weighs 100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, mesophase pitch 15 parts, aromatic hydrocarbons Oil 8 parts, 6 parts of graphite, sodium carboxymethyl cellulose 3 parts, 6 parts of paraffin, 12 parts of perchloric acid, cobalt carbonate 5 parts, titanium dioxide 5 parts, methanol 10 parts.
At room temperature, by raw material grinding machine for grinding 50 minutes so that it is mix homogeneously.
The raw material of mix homogeneously is placed in ceramic crucible with cover, then ceramic crucible with cover is put in tube furnace It is first heated to 500 DEG C under high pure nitrogen protection, insulation reaction 3 hours, then it is further heated to 1000 DEG C, insulation reaction 4 Hour, prepared lithium battery graphene complex.
Technique is simple, mild condition, has good electric conductivity, electrochemical lithium storage content is big, energy density is high, cyclicity Can be good；Low in raw material price, operation is simple；Can be not only used for fuel cell oxygen reduction reaction non-precious metal catalyst, Can be additionally used in ultracapacitor, lithium ion battery homenergic field of storage and the field such as Industrial Catalysis, environmental treatment；It is independent of In large-scale instrument and equipment, the large-scale production of high-quality graphene and complex thereof can be realized.
Embodiment 3:
Proportioning by weight weighs 100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, mesophase pitch 10 parts, aromatic hydrocarbons Oil 6 parts, 4 parts of graphite, sodium carboxymethyl cellulose 2 parts, 5 parts of paraffin, 10 parts of perchloric acid, cobalt carbonate 4 parts, titanium dioxide 4 parts, methanol 8 parts.
At room temperature, by raw material grinding machine for grinding 40 minutes so that it is mix homogeneously.
The raw material of mix homogeneously is placed in ceramic crucible with cover, then ceramic crucible with cover is put in tube furnace It is first heated to 450 DEG C under high pure nitrogen protection, insulation reaction 2 hours, then it is further heated to 950 DEG C, insulation reaction 3 is little Time, prepared lithium battery graphene complex.
Technique is simple, mild condition, has good electric conductivity, electrochemical lithium storage content is big, energy density is high, cyclicity Can be good；Low in raw material price, operation is simple；Can be not only used for fuel cell oxygen reduction reaction non-precious metal catalyst, Can be additionally used in ultracapacitor, lithium ion battery homenergic field of storage and the field such as Industrial Catalysis, environmental treatment；It is independent of In large-scale instrument and equipment, the large-scale production of high-quality graphene and complex thereof can be realized.
All components in above example all can be commercially available.
Above-described embodiment is only intended to be illustrated present disclosure rather than limit, therefore with the present invention's Any change in implication that claims are suitable and scope, is all considered as being included within the scope of the claims.

Claims (5)

1. a lithium battery graphene complex, it is characterised in that the raw material of described lithium battery graphene complex is by weight Amount number proportioning is as follows: 100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, mesophase pitch 5-15 part, aromatic naphtha 4-8 Part, graphite 2-6 part, sodium carboxymethyl cellulose 1-3 part, paraffin 4-6 part, perchloric acid 8-12 part, cobalt carbonate 3-5 part, titanium dioxide 3-5 part, methanol 6-10 part.
A kind of lithium battery graphene complex the most according to claim 1, it is characterised in that: described lithium battery graphite The raw materials by weight portion proportioning of alkene complex is as follows: 100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, and mesophase drips Blue or green 5 parts, aromatic naphtha 4 parts, 2 parts of graphite, sodium carboxymethyl cellulose 1 part, 4 parts of paraffin, 8 parts of perchloric acid, cobalt carbonate 3 parts, titanium dioxide Titanium 3 parts, methanol 6 parts.
A kind of lithium battery graphene complex the most according to claim 1, it is characterised in that: described lithium battery graphite The raw materials by weight portion proportioning of alkene complex is as follows: 100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, and mesophase drips Blue or green 15 parts, aromatic naphtha 8 parts, 6 parts of graphite, sodium carboxymethyl cellulose 3 parts, 6 parts of paraffin, 12 parts of perchloric acid, cobalt carbonate 5 parts, dioxy Change titanium 5 parts, methanol 10 parts.
A kind of lithium battery graphene complex the most according to claim 1, it is characterised in that: described lithium battery graphite The raw materials by weight portion proportioning of alkene complex is as follows: 100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, and mesophase drips Blue or green 10 parts, aromatic naphtha 6 parts, 4 parts of graphite, sodium carboxymethyl cellulose 2 parts, 5 parts of paraffin, 10 parts of perchloric acid, cobalt carbonate 4 parts, dioxy Change titanium 4 parts, methanol 8 parts.
5. the preparation method of lithium battery graphene complex described in a claim 1, it is characterised in that include walking as follows Rapid:
The first step: proportioning by weight weighs trimethylolpropane polyoxyethylene polyoxypropylene ether, mesophase pitch, aromatic hydrocarbons Oil, graphite, sodium carboxymethyl cellulose, paraffin, perchloric acid, cobalt carbonate, titanium dioxide and methanol；
Second step: at room temperature, by raw material in grinding machine for grinding 30-50 minute so that it is mix homogeneously；
3rd step: the raw material of mix homogeneously is placed in ceramic crucible with cover, then ceramic crucible with cover is put into tube furnace In high pure nitrogen protect under be first heated to 400-500 DEG C, insulation reaction 1-3 hour, be then further heated to 900- 1000 DEG C, insulation reaction 2-4 hour, prepared lithium battery graphene complex.
CN201610518542.7A 2016-07-05 2016-07-05 A kind of lithium battery graphene complex and preparation method thereof Pending CN106129353A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106783218A (en) * 2016-12-29 2017-05-31 南京悠谷知识产权服务有限公司 A kind of battery graphene complex material and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101857221A (en) * 2010-05-21 2010-10-13 哈尔滨工业大学 Method for preparing graphene compounds and graphene oxide compounds with high efficiency
CN104134806A (en) * 2014-07-01 2014-11-05 南京航空航天大学 Method for preparing nitrogen-doped graphene/metal complex from bottom to top, product thereof and application of product
CN104192834A (en) * 2014-08-27 2014-12-10 中国科学院电工研究所 Preparation method of graphene and graphene composition for supercapacitor
CN104310383A (en) * 2014-09-29 2015-01-28 中国科学院理化技术研究所 Graphene nanosheet and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101857221A (en) * 2010-05-21 2010-10-13 哈尔滨工业大学 Method for preparing graphene compounds and graphene oxide compounds with high efficiency
CN104134806A (en) * 2014-07-01 2014-11-05 南京航空航天大学 Method for preparing nitrogen-doped graphene/metal complex from bottom to top, product thereof and application of product
CN104192834A (en) * 2014-08-27 2014-12-10 中国科学院电工研究所 Preparation method of graphene and graphene composition for supercapacitor
CN104310383A (en) * 2014-09-29 2015-01-28 中国科学院理化技术研究所 Graphene nanosheet and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106783218A (en) * 2016-12-29 2017-05-31 南京悠谷知识产权服务有限公司 A kind of battery graphene complex material and preparation method thereof

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