CN105439128A - Preparation method for porous graphene lithium ion battery positive electrode material - Google Patents
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- CN105439128A CN105439128A CN201510759703.7A CN201510759703A CN105439128A CN 105439128 A CN105439128 A CN 105439128A CN 201510759703 A CN201510759703 A CN 201510759703A CN 105439128 A CN105439128 A CN 105439128A
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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
- 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
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- 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
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a preparation method for a porous graphene lithium ion battery positive electrode material. The method comprises the following steps of: 1) preparing graphite oxide with a modified Hummer method; 2) preparing porous graphene by self-assembly with a hydrothermal/solvothermal method; and 3) performing high-temperature reduction/doping treatment on the porous graphene obtained in the step 2), and pressing the porous graphene to form a film. A forming material serves as a positive electrode material to be directly applied to a lithium ion battery, so that the discharge specific capacity can reach 175mAh/g, and high cycle stability and excellent rate performance are achieved; and the preparation method is low in cost and suitable for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of nanometer energy storage material, be specifically related to a kind of preparation method of porous graphene anode material for lithium-ion batteries.
Background technology
Lithium ion battery has the features such as specific energy is high, memory-less effect, long circulation life, has been widely used in the field such as mobile equipment, electric automobile energy.The performance of the electrode materials of lithium ion battery directly determines the Key Performance Indicator such as specific energy, cycle life of lithium ion battery.At present, developed the multiple negative material such as Si, Sn and mesoporous carbon, their capacity can reach 1000 ~ 2000mAh/g, even higher.But, in positive electrode material, research mostly comparatively is Li-Co-O, Li-Ni-O, Li-Mn-O, Li-Fe-O and ternary material, although the development all obtained to a certain degree and practical application, but actual specific capacity is usually less than 160mAh/g, cyclical stability and high rate performance are all poor, in addition, these positive electrode materials need extra conductive agent, binding agent and metal collector (Al paper tinsel) usually, thus reduce the specific storage of battery at double.Therefore, the height ratio capacity positive electrode material of development of new is particularly important to the over-all properties promoting lithium ion battery.
The bidimensional cycle honeycomb lattice structure that Graphene is made up of carbon six-ring, has excellent heat conductance, physical strength and electrical properties, and in addition, graphene-structured can carry out flexible modulation, such as surface grafting oxygen-containing functional group, introduces defective bit.The Graphene of partial oxidation has huge specific surface area, its surface functional group can with lithium ion generation chemical reaction, can be used as positive electrode material and be applied to lithium ion battery.At present, the research of graphene anode material is in the starting stage, and its specific storage is lower, and the graphene powder developed also needs to add binding agent, conductive agent and collector as positive electrode material usually.
After introducing oxygen-containing functional group in Graphene, its specific surface area significantly increases, and is beneficial to electrochemical lithium storage, but also causes the significantly reduction of electrical properties simultaneously, the lifting of restriction high rate performance.Therefore, how regulating and controlling the defective bit of Graphene, type functional group, specific surface area and electric property is the key obtaining High-performance graphene positive electrode material.
Summary of the invention
The object of this invention is to provide a kind of preparation method of porous graphene anode material for lithium-ion batteries, effectively can regulate and control the conduction of Graphene, oxygen-containing functional group and specific surface area, obtain high connductivity, the self-supporting of bigger serface, Flexible graphene positive electrode material, the method cost is low, is applicable to large-scale commercial production.
To achieve these goals, the present invention is by the following technical solutions:
A preparation method for porous graphene anode material for lithium-ion batteries, said method comprising the steps of:
1) the Hummer legal system of modifying is for graphite oxide;
2) porous graphene is prepared in the hot method self-assembly of hydrothermal/solvent:
(a) configuration graphene oxide solution: by powerful for the graphite oxide solution of dispersion ultrasonic 10min ~ 10h;
B step (a) gained solution is carried out hydro-thermal or solvent thermal reaction by () at 80 ~ 240 DEG C, the reaction times is 30min ~ 48h;
C organic solvent in step (b) gained reaction solution is replaced as deionized water by (), then lyophilize obtains described porous graphene;
3) high temperature reduction/doping treatment step 2) gained porous graphene, then be pressed into film.
First optimal technical scheme of the preparation method of described porous graphene anode material for lithium-ion batteries, step 1) the Hummer method of described modification comprises the steps:
A 0.2 ~ 10g natural flake graphite and 0.2 ~ 10g SODIUMNITRATE add in the reaction vessel at 0 DEG C by ();
B () slowly adds 20 ~ 200ml vitriol oil under stirring in the described reaction vessel of step (a), more slowly add 2 ~ 50g potassium permanganate, stirs 20 ~ 120min in 0 DEG C of lower magnetic force;
C () slowly adds the deionized water of 20 ~ 300ml react 2h at 25 DEG C ~ 45 DEG C after, then at 70-95 DEG C, to react after 5 ~ 60min Temperature fall to 30-40 DEG C;
D () adds hydrogen peroxide solution 2 ~ 100ml and the deionized water 50 ~ 1000ml of 30% in step (c) gained solution, stir 10min and namely obtain graphite oxide solution;
E () close to neutral, dries 30min ~ 24h by graphite oxide solution described in washed with de-ionized water at 30 ~ 120 DEG C.
Second optimal technical scheme of the preparation method of described porous graphene anode material for lithium-ion batteries, step 2) described in the solvent of graphene oxide solution be the combination of one or more in deionized water, ethanol, acetone, acetic acid, ammoniacal liquor and N-Methyl pyrrolidone.
3rd optimal technical scheme of the preparation method of described porous graphene anode material for lithium-ion batteries, step 2) described in the concentration of graphene oxide solution be 0.2 ~ 20mg/ml.
4th optimal technical scheme of the preparation method of described porous graphene anode material for lithium-ion batteries, step 3) described in the temperature of hydro-thermal or solvent thermal reaction be 120 ~ 200 DEG C, the time is 10 ~ 24h.
5th optimal technical scheme of the preparation method of described porous graphene anode material for lithium-ion batteries, the temperature of described hydro-thermal or solvent thermal reaction is 180 DEG C, and the time is 12h.
6th optimal technical scheme of the preparation method of described porous graphene anode material for lithium-ion batteries, step 3) described in the atmosphere of reduction/doping treatment be one or more gas mixture of hydrogen, argon gas and ammonia.
7th optimal technical scheme of the preparation method of described porous graphene anode material for lithium-ion batteries, step 3) described in the temperature of reduction/doping treatment be 300 ~ 1000 DEG C, the time is 10min ~ 10h.
8th optimal technical scheme of the preparation method of described porous graphene anode material for lithium-ion batteries, the temperature of described reduction/doping treatment is 800 DEG C, and the time is 6h.
The porous graphene prepared of described method is for the preparation of the application of anode material for lithium-ion batteries aspect.
With immediate prior art ratio, the present invention has following beneficial effect:
1) the present invention prepare novel flexible, self supporting structure the character such as porous graphene positive electrode material has high electroconductibility, high specific surface area, oxygen-containing functional group is adjustable;
2) porous graphene material of the present invention directly can be applied to lithium ion battery as positive electrode material, does not need extra conductive agent, binding agent and collector, and its specific storage can reach 175mAh/g;
3) preparation method's technique of the present invention is simple, and process is easy to control, and do not need under vacuum, facility investment is few, can be applicable to scale operation.
Accompanying drawing explanation
Fig. 1: positive electrode material is respectively the cyclical stability of the lithium ion battery of the Graphene of embodiment 1 and the graphene oxide of comparative example 1;
Fig. 2: the photo of porous graphene material;
Fig. 3: the scanning electron microscope (SEM) photograph of porous graphene material;
Fig. 4: the transmission electron microscope picture of porous graphene material.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in detail, but scope is not limited thereto.
Embodiment 1
Adopt the Hummer legal system of modifying for graphite oxide: to weigh 2g natural flake graphite, 2g SODIUMNITRATE joins in reaction vessel, the temperature of reaction vessel remains on 0 DEG C, then in reaction vessel, the 96ml vitriol oil is slowly added, continuous reaction stirred, then 12g potassium permanganate is slowly added wherein, to guarantee that heat can leave in time, and holding temperature is 0 DEG C, react under magnetic stirring after 90 minutes, again temperature was elevated to 35 DEG C of reactions after two hours, then the deionized water of 80ml is slowly added wherein, and temperature is elevated to 90-95 DEG C, react after 15 minutes, naturally 30-40 DEG C is reduced the temperature to, add the deionized water of 10ml hydrogen peroxide solution (30%) and 200ml more wherein, react and can obtain graphite oxide solution after 10 minutes.
Graphite oxide solution is dried 12 hours in 80 DEG C, takes a certain amount of graphite oxide, ultrasonic stripping 5 hours, obtain 1.0mg/ml graphene oxide solution.Transfer in reactor by above-mentioned solution, carry out hydro-thermal reaction, temperature of reaction is 180 DEG C, 12 hours reaction times; Lyophilize obtains described porous graphene (Fig. 2 and Fig. 3), and Graphene is few Rotating fields, as shown in Figure 4.Under ammonia atmosphere, porous graphene is carried out pyroprocessing, treatment temp is 800 DEG C, and the reaction times is 2 hours, and in Graphene, oxygen level is about 15.8% (mass ratio), and nitrogen content is 9.6% (mass ratio), and its specific surface area is 990m
2/ g.The porous graphene processed is pressed into certain thickness flexibility, self-supporting Graphene porous membrane.
Using the film of preparation directly as positive electrode material, comparison electrode is lithium sheet, and assembling lithium ion battery, under 1.5V ~ 4.5V scope, carry out electrochemical property test, specific storage is lower, is greater than 150mAh/g (as shown in Figure 1).
Found by contrast, the porous graphene of assembling, by further reducing and doping treatment, oxygen level reduces, and specific surface area significantly promotes, and the positive electrode material specific storage of final lithium ion battery is far above graphene oxide composite material.
Embodiment 2
Other preparation condition is constant, the atmosphere of the pyroprocessing in embodiment 1 is become the gas mixture of hydrogen and argon gas, and the reaction times is 4 hours, and in Graphene, oxygen level is about 25.8% (mass ratio), and its specific surface area is 450m
2/ g.Graphene porous membrane directly it can be used as positive electrode material, and specific storage is 95mAh/g.
Embodiment 3
Other preparation condition is constant, and the atmosphere of the pyroprocessing in embodiment 1 is become argon gas, and the reaction times is 1.5 hours, and in Graphene, oxygen level is about 28.8% (mass ratio), and its specific surface area is 550m
2/ g.Graphene porous membrane directly it can be used as positive electrode material, and specific storage is 115mAh/g.
Embodiment 4
Other preparation condition is constant, the atmosphere of the pyroprocessing in embodiment 1 is become ammonia, and the reaction times is 6 hours, and in Graphene, oxygen level is about 12.8% (mass ratio), nitrogen content is 11.5% (mass ratio), and its specific surface area is 1050m
2/ g.Graphene porous membrane directly it can be used as positive electrode material, and specific storage is 175mAh/g.
Embodiment 5
Other preparation condition is constant, and the atmosphere of the pyroprocessing in embodiment 1 is become argon gas, and the reaction times is 8 hours, and in Graphene, oxygen level is about 20.2% (mass ratio), and its specific surface area is 480m
2/ g.Graphene porous membrane directly it can be used as positive electrode material, and specific storage is 87mAh/g.
Comparative example 1
Adopt and obtain graphite oxide solution with same procedure described in embodiment 1.The graphite oxide solution deionized water of gained is gone cleaning, until the pH value of graphite oxide solution after cleaning is close to neutrality, then directly carry out lyophilize, obtain porous oxidation Graphene, oxygen level is 45% (mass ratio), and specific surface area is 268m
2/ g.Be pressed into the graphene oxide composite material of flexibility, self-supporting by press, directly it can be used as positive electrode material, comparison electrode is lithium sheet, assembling lithium ion battery, under 1.5V ~ 4.5V scope, carry out electrochemical property test, specific storage is lower, is less than 50mAh/g (as shown in Figure 1).
Above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; those of ordinary skill in the field are to be understood that; can modify to the specific embodiment of the present invention with reference to above-described embodiment or equivalent to replace, these do not depart from any amendment of spirit and scope of the invention or equivalently to replace within the claims that all awaits the reply in application.
Claims (10)
1. a preparation method for porous graphene anode material for lithium-ion batteries, is characterized in that, said method comprising the steps of:
1) the Hummer legal system of modifying is for graphite oxide;
2) porous graphene is prepared in the hot method self-assembly of hydrothermal/solvent:
(a) configuration graphene oxide solution: by powerful for the graphite oxide solution of dispersion ultrasonic 10min ~ 10h;
B step (a) gained solution is carried out hydro-thermal or solvent thermal reaction 30min ~ 48h by () at 80 ~ 240 DEG C;
C () is with after the organic solvent in deionized water displacement step (b) gained reaction solution, then lyophilize obtains described porous graphene;
3) high temperature reduction/doping treatment step 2) gained porous graphene, then be pressed into film.
2. the preparation method of porous graphene anode material for lithium-ion batteries according to claim 1, is characterized in that, step 1) the Hummer method of described modification comprises the steps:
A 0.2 ~ 10g natural flake graphite and 0.2 ~ 10g SODIUMNITRATE add in the reaction vessel at 0 DEG C by ();
B () slowly adds 20 ~ 200ml vitriol oil under stirring in the described reaction vessel of step (a), more slowly add 2 ~ 50g potassium permanganate, stirs 20 ~ 120min in 0 DEG C of lower magnetic force;
C () slowly adds the deionized water of 20 ~ 300ml react 2h at 25 DEG C ~ 45 DEG C after, then at 70-95 DEG C, to react after 5 ~ 60min Temperature fall to 30-40 DEG C;
D () adds hydrogen peroxide solution 2 ~ 100ml and the deionized water 50 ~ 1000ml of 30% in step (c) gained solution, stir 10min and namely obtain graphite oxide solution;
E () close to neutral, dries 30min ~ 24h by graphite oxide solution described in washed with de-ionized water at 30 ~ 120 DEG C.
3. the preparation method of porous graphene anode material for lithium-ion batteries according to claim 1, it is characterized in that, step 2) described in the solvent of graphene oxide solution be the combination of one or more in deionized water, ethanol, acetone, acetic acid, ammoniacal liquor and N-Methyl pyrrolidone.
4. the preparation method of porous graphene anode material for lithium-ion batteries according to claim 1, is characterized in that, step 2) described in the concentration of graphene oxide solution be 0.2 ~ 20mg/ml.
5. the preparation method of porous graphene anode material for lithium-ion batteries according to claim 1, is characterized in that, step 3) described in the temperature of hydro-thermal or solvent thermal reaction be 120 ~ 200 DEG C, the time is 10 ~ 24h.
6. the preparation method of porous graphene anode material for lithium-ion batteries according to claim 5, is characterized in that, the temperature of described hydro-thermal or solvent thermal reaction is 180 DEG C, and the time is 12h.
7. the preparation method of porous graphene anode material for lithium-ion batteries according to claim 1, is characterized in that, step 3) described in the atmosphere of reduction/doping treatment be one or more gas mixture of hydrogen, argon gas and ammonia.
8. the preparation method of porous graphene anode material for lithium-ion batteries according to claim 1, is characterized in that, step 3) described in the temperature of reduction/doping treatment be 300 ~ 1000 DEG C, the time is 10min ~ 10h.
9. the preparation method of porous graphene anode material for lithium-ion batteries according to claim 8, is characterized in that, the temperature of described reduction/doping treatment is 800 DEG C, and the time is 6h.
10. according to claim 1 the porous graphene prepared of method for the preparation of the application of anode material for lithium-ion batteries.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105762360A (en) * | 2016-04-01 | 2016-07-13 | 上海交通大学 | Graphene-silicon-coated composite negative electrode material and preparing method and application thereof |
| CN106082177A (en) * | 2016-05-27 | 2016-11-09 | 中国科学院山西煤炭化学研究所 | The preparation method of a kind of Carbon Materials hydrogenation catalyst and application |
| CN106542522A (en) * | 2017-01-16 | 2017-03-29 | 哈尔滨工业大学 | The method that template prepares three-dimensional grapheme |
| CN106784835A (en) * | 2017-02-23 | 2017-05-31 | 南阳师范学院 | A kind of preparation method of carbon negative electrode material of lithium ion cell |
| CN106784654A (en) * | 2016-11-28 | 2017-05-31 | 荆门市格林美新材料有限公司 | A kind of preparation method of graphene coated cobalt acid lithium material |
| CN106938845A (en) * | 2017-03-10 | 2017-07-11 | 华南理工大学 | A kind of graphite oxide positive electrode and preparation method for lithium ion battery, the preparation method of lithium ion cell positive |
| CN108155378A (en) * | 2017-12-13 | 2018-06-12 | 南京红太阳新能源有限公司 | A kind of preparation based on graphene high energy lithium ion cell negative material |
| CN108390063A (en) * | 2018-01-19 | 2018-08-10 | 同济大学 | Graphene prepares the method and electrode of flexible self-supporting electrode as conductive adhesive |
| CN108633241A (en) * | 2017-03-23 | 2018-10-09 | 洛阳尖端技术研究院 | A kind of suction wave cellular material and preparation method thereof |
| CN108892123A (en) * | 2018-06-08 | 2018-11-27 | 深圳新恒业电池科技有限公司 | A kind of preparation method of porous graphene |
| CN109036877A (en) * | 2018-07-10 | 2018-12-18 | 扬州大学 | Porous type graphene/transient metal chalcogenide compound film preparation method |
| CN109935789A (en) * | 2017-12-15 | 2019-06-25 | 中国科学院大连化学物理研究所 | A kind of lithium ion battery negative material and preparation and application |
| CN110504411A (en) * | 2019-08-30 | 2019-11-26 | 清远佳致新材料研究院有限公司 | Preparation method, lithium ion cell positive, lithium ion battery and the electric device of lithium ion cell positive |
| CN112537767A (en) * | 2019-09-23 | 2021-03-23 | 中国科学院上海硅酸盐研究所苏州研究院 | High-elasticity three-dimensional graphene macroscopic body and preparation method thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105762360A (en) * | 2016-04-01 | 2016-07-13 | 上海交通大学 | Graphene-silicon-coated composite negative electrode material and preparing method and application thereof |
| CN106082177A (en) * | 2016-05-27 | 2016-11-09 | 中国科学院山西煤炭化学研究所 | The preparation method of a kind of Carbon Materials hydrogenation catalyst and application |
| CN106784654A (en) * | 2016-11-28 | 2017-05-31 | 荆门市格林美新材料有限公司 | A kind of preparation method of graphene coated cobalt acid lithium material |
| CN106542522A (en) * | 2017-01-16 | 2017-03-29 | 哈尔滨工业大学 | The method that template prepares three-dimensional grapheme |
| CN106784835A (en) * | 2017-02-23 | 2017-05-31 | 南阳师范学院 | A kind of preparation method of carbon negative electrode material of lithium ion cell |
| CN106938845A (en) * | 2017-03-10 | 2017-07-11 | 华南理工大学 | A kind of graphite oxide positive electrode and preparation method for lithium ion battery, the preparation method of lithium ion cell positive |
| CN108633241A (en) * | 2017-03-23 | 2018-10-09 | 洛阳尖端技术研究院 | A kind of suction wave cellular material and preparation method thereof |
| CN108155378A (en) * | 2017-12-13 | 2018-06-12 | 南京红太阳新能源有限公司 | A kind of preparation based on graphene high energy lithium ion cell negative material |
| CN109935789A (en) * | 2017-12-15 | 2019-06-25 | 中国科学院大连化学物理研究所 | A kind of lithium ion battery negative material and preparation and application |
| CN108390063A (en) * | 2018-01-19 | 2018-08-10 | 同济大学 | Graphene prepares the method and electrode of flexible self-supporting electrode as conductive adhesive |
| CN108892123A (en) * | 2018-06-08 | 2018-11-27 | 深圳新恒业电池科技有限公司 | A kind of preparation method of porous graphene |
| CN109036877A (en) * | 2018-07-10 | 2018-12-18 | 扬州大学 | Porous type graphene/transient metal chalcogenide compound film preparation method |
| CN110504411A (en) * | 2019-08-30 | 2019-11-26 | 清远佳致新材料研究院有限公司 | Preparation method, lithium ion cell positive, lithium ion battery and the electric device of lithium ion cell positive |
| CN112537767A (en) * | 2019-09-23 | 2021-03-23 | 中国科学院上海硅酸盐研究所苏州研究院 | High-elasticity three-dimensional graphene macroscopic body and preparation method thereof |
| CN112537767B (en) * | 2019-09-23 | 2023-09-08 | 中国科学院上海硅酸盐研究所苏州研究院 | High-elasticity three-dimensional graphene macroscopic body and preparation method thereof |
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