CN102956872B - Preparation method and application of compound electrode slice - Google Patents
Preparation method and application of compound electrode slice Download PDFInfo
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- CN102956872B CN102956872B CN201110251092.7A CN201110251092A CN102956872B CN 102956872 B CN102956872 B CN 102956872B CN 201110251092 A CN201110251092 A CN 201110251092A CN 102956872 B CN102956872 B CN 102956872B
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Abstract
The invention is suitable for the field of electrode preparation, and provides a preparation method and application of a compound electrode slice. The preparation method of the compound electrode slice comprises the following steps of: preparing a first solution, preparing a compound electrode slice precursor, and preparing the compound electrode slice. According to the preparation method of the compound electrode slice, graphene oxide and a carbon nano tube are dissolved in alcohol, and are ultrasonically stirred, so that the specific surface area after graphene is dried is increased; and through an electro-deposition method, the process is simple and the time is short, and the equivalent series resistance (ESR) of the compound electrode slice can be reduced. The preparation method of the compound electrode slice is low in cost and high in production profit, and is very suitable for industrialized production.
Description
Technical field
The invention belongs to electrode preparation field, particularly relate to a kind of combination electrode piece preparation method and application thereof.
Background technology
Strong K sea nurse (Andre K.Geim) of the peace moral of Univ Manchester UK etc. prepared grapheme material in 2004, paid attention to widely because the structure of its uniqueness and photoelectric property receive people.Single-layer graphene is due to its large specific area, and excellent conduction, heat conductivility and low thermal coefficient of expansion and be considered to desirable material, can be used as electrode material in ultracapacitor and lithium ion battery.
But be easy to occur to reunite and stacked because the two-dimensional structure of the monolayer of Graphene to lose in drying in the water process of interlayer, curling or height fold, finally causes the utilance of its specific area greatly to reduce; Meanwhile, the technique that tradition prepares electrode slice is comparatively complicated, and adds certain binding agent, increases the equivalent series resistance of electrode, affects the power density of ultracapacitor.
Summary of the invention
In view of this, the embodiment of the present invention provides a kind of preparation method of compound electric pole piece, solves in prior art to use Graphene to be applied in electrode slice easily to occur to reunite and stacked technical problem, and the application of compound electric pole piece prepared by the method.
The present invention is achieved in that
A kind of combination electrode piece preparation method, comprises the steps:
By weight ratio be 1 ~ 2: 1 graphene oxide and carbon nano-tube be added in alcoholic solvent, ultrasonic process, stir, obtain the first solution;
In this first solution, add metal salt solution, ultrasonic process, obtain the second solution, with this second solution for electrolyte, take metal forming as electrode, carry out electrophoretic process, obtain compound electric pole piece precursor;
By this electrode slice precursor drying process, put into reducing solution, under temperature is 80 DEG C ~ 100 DEG C conditions, react 1 hour ~ 36 hours, by the vacuumize of reacted compound electric pole piece precursor, obtain compound electric pole piece.
Embodiment of the present invention combination electrode piece preparation method, by graphene oxide and carbon nano-tube are dissolved in ethanol, and ultrasonic agitation, graphene oxide is made to be reduced to Graphene by liquid phase chemical reduction again, carbon nano-tube is inserted between graphene sheet layer, Graphene is separated from each other out between layers, avoid Graphene and reunite and lamination, improve the dried specific area of Graphene, play the effect of Graphene and carbon nano-tube performance complement better; By the method for electro-deposition, Graphene and carbon nano-tube is made to be deposited on electrode, complicated coating process can be saved, technique is simple and the time is short, the equivalent series resistance (ESR) of compound electric pole piece can be reduced simultaneously, thus the more effective power density improving the ultracapacitor of this compound electric pole piece of application; Embodiment of the present invention combination electrode piece preparation method, with low cost, productivity effect is high, is very suitable for suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is embodiment of the present invention combination electrode piece preparation method flow chart;
Fig. 2 is the button cell charging and discharging curve of compound electric pole piece prepared by the application embodiment of the present invention one;
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Refer to Fig. 1, Fig. 1 shows embodiment of the present invention combination electrode piece preparation method flow chart, comprises the steps:
Step S01, prepares the first solution
By weight ratio be 1 ~ 2: 1 graphene oxide and carbon nano-tube be added in alcoholic solvent, ultrasonic process, stir, obtain the first solution;
Step S02, prepares compound electric pole piece precursor
In this first solution, add metal salt solution, ultrasonic process, obtain the second solution, with this second solution for electrolyte, take metal forming as electrode, carry out electrophoretic process, obtain compound electric pole piece precursor;
Step S03, prepares compound electric pole piece
By this electrode slice precursor drying process, put into reducing solution, under temperature is 80 DEG C ~ 100 DEG C conditions, react 1 hour ~ 36 hours, by the vacuumize of reacted compound electric pole piece precursor, obtain compound electric pole piece.
Particularly, in step S01, this graphene oxide is standby, specific as follows by the Hummers legal system improved:
Be 50 object crystalline graphite powders by 20g particle diameter, 10g potassium peroxydisulfate and 10g phosphorus pentoxide add in the concentrated sulfuric acid of 80 DEG C and obtain mixed solution, mixed solution is stirred, cool more than 6 hours, filter, by extremely neutral for the pre-oxidation graphite washing obtained, then dry, dried sample is added 0 DEG C, in the concentrated sulfuric acid of 460mL, add 60g potassium permanganate again, the temperature of mixture remains on less than 20 DEG C, then after keeping 2h in the oil bath of 35 DEG C, slowly add 920mL deionized water, after 15min, add 2.8L deionized water (wherein containing 50mL concentration is the hydrogen peroxide of 30%) again, mixture color becomes glassy yellow afterwards, suction filtration while hot, wash with the hydrochloric acid that 5L concentration is 10% again, suction filtration, namely graphite oxide is obtained at 50 DEG C of vacuumize 48h.This graphite oxide, through the ultrasonic process of subsequent step, is peeled off and is formed graphene oxide.
Particularly, this carbon nano-tube does not limit, and be preferably acidifying nanotube, this acidifying carbon nano-tube refers to the carbon nano-tube after peracid treatment, and the acid treatment step of this nanotube is:
Carbon nano-tube is added in acid solution, under 60 DEG C of-90 DEG C of conditions, adds hot reflux 1 hour ~ 3 hours.Filter, washing and drying.This acid is restriction not, such as, and watery hydrochloric acid, dilute sulfuric acid, dust technology etc.; By carbon nano-tube is used acid solution immersion treatment, make carbon nano tube surface functional group (as OH; COOH) quantity increases greatly;
Particularly, this alcoholic solvent does not limit, and the alcohol that can use as solvent, being preferably carbon number is C
1-C
6alcohol, such as, ethanol, propyl alcohol, isopropyl alcohol etc.; The power of this ultrasonic process is 150W ~ 200W, and sonication treatment time is 0.5 hour ~ 2 hours, and this mixing time is 0.5 hour ~ 1 hour, and temperature is 20 DEG C ~ 30 DEG C.By by graphite oxide and carbon nano-tube (carbon nano-tube particularly after acidification) ultrasonic process in alcoholic solvent, stir, carbon nano-tube is well mixed with graphene oxide, form graphene oxide-Carbon Nanotube.That divides between graphene oxide lamella and lamella opens very much, but the functional group of reduction rear surface easily reunites after losing, and better with carbon pipe mixed effect when graphene oxide, adds the reunion that carbon pipe can prevent the Graphene after reducing.
Particularly, in step S02, in this metal salt solution, the concentration of slaine is 0.2mg/ml ~ 0.5mg/ml, and this slaine does not limit, such as Mg (SO
4)
27H
2o, Fe (NO
3)
39H
2o, Zn (NO
3)
26H
2o or Mg (NO
3)
26H
2one in O; The solvent of this metal salt solution is water.Be added to by metal salt solution after in the first solution, sonification power is 150W ~ 200W, and sonication treatment time is 15 minutes ~ 60 minutes, obtains the second solution, is stirred by the second solution;
The metal forming of two 5cm ~ 10cm diameters is added as electrode in this second solution, be placed in electrolyte by its Parallel Symmetric, add the direct current of 40V ~ 80V at the two ends of electrode, two die openings are 0.5cm, electrophoresis 5min ~ 20min, just can obtain compound electric pole piece precursor; This metal forming does not limit, such as, and nickel foil, aluminium foil, Copper Foil etc.
Particularly, in step S03, dry process refers to: the compound electric pole piece precursor obtained by step S02 dries naturally, and then toast 1 hour ~ 3 hours under vacuum, baking temperature is 40 DEG C ~ 50 DEG C; Again the compound electric pole piece precursor after drying process is added in reducing solution, the temperature of the reducing solution containing compound electric pole piece precursor is adjusted to 80 DEG C ~ 100 DEG C, be preferably 100 DEG C, react 1 hour ~ 36 hours; Carrying out liquid-phase reduction process by being put into by compound electric pole piece under said temperature condition, making the graphene oxide in compound electric pole piece be reduced to Graphene, obtaining the electrode slice of graphene-containing-carbon nano-tube;
This reducing solution refers to the solution system using reducing substances as solute, such as, hydrazine hydrate solution, sodium borohydride solution, quinol solution, ethylenediamine solution, hydroiodic acid solution etc., the mass percent of this reducing solution is 50% ~ 85%;
In the liquid-phase reduction treatment step of this step, more than 1 hour reaction time, specifically do not limit, be preferably 1-36 hour, reaction time determines according to the reproducibility of reducing agent, such as, the hydrazine hydrate solution reaction time is 24 hours ~ 36 hours, and the reaction time of sodium borohydride solution is 1 hour ~ 6 hours.
After liquid phase reactor completes, the electrode slice of this graphene-carbon nano tube is carried out vacuumize 5 hours ~ 10 hours, baking temperature is 50 DEG C ~ 80 DEG C, obtains compound electric pole piece.
Embodiment of the present invention combination electrode piece preparation method, by graphene oxide and carbon nano-tube are dissolved in ethanol, and ultrasonic agitation, graphene oxide is made to be reduced to Graphene by liquid phase chemical reduction again, can better carbon nano-tube be inserted between graphene sheet layer, Graphene is separated from each other out between layers, avoid Graphene and reunite and lamination, improve the dried specific area of Graphene, play the effect of Graphene and carbon nano-tube performance complement better; By the method for electro-deposition, Graphene and carbon nano-tube is made to be deposited on electrode, complicated coating process can be saved, technique is simple and the time is short, the equivalent series resistance (ESR) of compound electric pole piece can be reduced simultaneously, thus the more effective power density improving the ultracapacitor of this compound electric pole piece of application.Embodiment of the present invention combination electrode piece preparation method, with low cost, productivity effect is high, is very suitable for suitability for industrialized production.
The embodiment of the present invention provides the application of the compound electric pole piece prepared by above-mentioned combination electrode piece preparation method in battery, capacitor further.
Below in conjunction with specific embodiment, above-mentioned combination electrode piece preparation method is described in detail.
Embodiment one
Embodiment of the present invention combination electrode piece preparation method, comprises the steps:
By improve Hummers legal system for graphite oxide:
20g 50 order graphite powder, 10g potassium peroxydisulfate and 10g phosphorus pentoxide are added in the concentrated sulfuric acid of 80 DEG C, stir, cooling more than 6h, washing is to neutral, dry.Dried sample is added 0 DEG C, in the concentrated sulfuric acid of 460mL, then add 60g potassium permanganate, the temperature of mixture remains on less than 20 DEG C, after then keeping 2h in the oil bath of 35 DEG C, slowly adds 920mL deionized water.After 15min, add 2.8L deionized water (wherein containing 50mL concentration is the hydrogen peroxide of 30%) again, mixture color becomes glassy yellow afterwards, while hot suction filtration, then carries out washing with the hydrochloric acid that 5L concentration is 10%, suction filtration, namely obtain graphite oxide at 50 DEG C of vacuumize 48h.
Prepare the first solution:
Carbon nano-tube graphite oxide and HCl treatment crossed adds in ethanol with the ratio of weight ratio 1: 1, ultrasonic 0.5h, stirs 0.5h, obtain homodisperse graphene oxide, carbon nano-tube solution under temperature is 20 DEG C of conditions;
Prepare compound electric pole piece precursor:
Magnesium nitrate solution (Mg (the NO that concentration is 0.5mg/ml is added in the first solution
3)
26H
2o), ultrasonic 15min, obtain uniform second solution, using the second solution as electrolyte, using the nickel foil of 5cm diameter as electrode, its Parallel Symmetric is placed in electrolyte, the direct current of 40V is added at the two ends of electrode, two die openings are 0.5cm, electrophoresis 5min, obtain compound electric pole piece precursor;
Prepare compound electric pole piece:
After compound electric pole piece is dried naturally, vacuum bakeout 1 hour under 60 DEG C of conditions, then adding mass percent is in the aqueous solution of the hydrazine hydrate of 50%, temperature is adjusted to 100 DEG C, after liquid-phase reduction process 24h, then vacuumize 5h under 60 DEG C of conditions, obtains compound electric pole piece.
Performance Detection:
The pole piece roller mill of gained is carried out roll extrusion, the pole piece card punch of roll-in is broken into the circular pole piece that diameter is 10mm, correct amount.By pole piece in glove box, barrier film and electrolyte are assembled into ultracapacitor according to cell making process, its septation is celgard 2000, electrolyte is the 1-ethyl-3-methylimidazole tetrafluoro boric acid salting liquid of 0.5mol/L, assemble rear leaving standstill and carry out a constant current charge-discharge test in, wherein voltage range is 0-1.85V, and electric current is that 1A/g carries out constant current charge-discharge.
Refer to Fig. 2, the button cell charging and discharging curve of the compound electric pole piece of Fig. 2 display application embodiment of the present invention one preparation, as can be seen from Figure 2, under 1A/g current density, the charging and discharging curve shape that the charging and discharging curve of battery is near the mark, has good charge-discharge performance.
Embodiment two
Embodiment of the present invention combination electrode piece preparation method, comprises the steps:
By improve Hummers legal system for graphite oxide:
20g 50 order graphite powder, 10g potassium peroxydisulfate and 10g phosphorus pentoxide are added in the concentrated sulfuric acid of 80 DEG C, stir, cooling more than 6h, washing is to neutral, dry.Dried sample is added 0 DEG C, in the concentrated sulfuric acid of 460mL, then add 60g potassium permanganate, the temperature of mixture remains on less than 20 DEG C, after then keeping 2h in the oil bath of 35 DEG C, slowly adds 920mL deionized water.After 15min, add 2.8L deionized water (wherein containing 50mL concentration is the hydrogen peroxide of 30%) again, mixture color becomes glassy yellow afterwards, while hot suction filtration, then carries out washing with the hydrochloric acid that 5L concentration is 10%, suction filtration, namely obtain graphite oxide at 50 DEG C of vacuumize 48h.
Prepare the first solution:
Carbon nano-tube graphite oxide and sulfuric acid treatment crossed adds in propyl alcohol with the ratio of weight ratio 1.5: 1, ultrasonic 2h, stirs 0.75h, obtain homodisperse graphene oxide, carbon nano-tube solution under temperature is 20 DEG C of conditions;
Prepare compound electric pole piece precursor:
Adlerika Mg (the SO that concentration is 0.2mg/ml is added in the first solution
4)
27H
2o, ultrasonic 60min, obtain uniform second solution, using the second solution as electrolyte, using the Copper Foil of 10cm diameter as electrode, its Parallel Symmetric is placed in electrolyte, adds the direct current of 80V at the two ends of electrode, two die openings are 0.5cm, electrophoresis 20min, obtain compound electric pole piece precursor;
Prepare compound electric pole piece:
After compound electric pole piece is dried naturally, vacuum bakeout 2 hours under 60 DEG C of conditions, then adding mass percent is in the aqueous solution of the sodium borohydride of 60%, temperature is adjusted to 80 DEG C, after liquid-phase reduction process 6h, then vacuumize 10h under 60 DEG C of conditions, obtains compound electric pole piece.
Embodiment three
Embodiment of the present invention combination electrode piece preparation method, comprises the steps:
By improve Hummers legal system for graphite oxide:
20g 50 order graphite powder, 10g potassium peroxydisulfate and 10g phosphorus pentoxide are added in the concentrated sulfuric acid of 80 DEG C, stir, cooling more than 6h, washing is to neutral, dry.Dried sample is added 0 DEG C, in the concentrated sulfuric acid of 460mL, then add 60g potassium permanganate, the temperature of mixture remains on less than 20 DEG C, after then keeping 2h in the oil bath of 35 DEG C, slowly adds 920mL deionized water.After 15min, add 2.8L deionized water (wherein containing 50mL concentration is the hydrogen peroxide of 30%) again, mixture color becomes glassy yellow afterwards, while hot suction filtration, then carries out washing with the hydrochloric acid that 5L concentration is 10%, suction filtration, namely obtain graphite oxide at 50 DEG C of vacuumize 48h.
Prepare the first solution:
Carbon nano-tube graphite oxide and nitric acid treatment crossed adds in isopropyl alcohol with the ratio of weight ratio 2: 1, ultrasonic 1h, stirs 1h, obtain homodisperse graphene oxide, carbon nano-tube solution under temperature is 30 DEG C of conditions;
Prepare compound electric pole piece precursor:
Iron nitrate solution (Fe (the NO that concentration is 0.2mg/ml is added in the first solution
3)
39H
2o), ultrasonic 45min, obtain uniform second solution, using the second solution as electrolyte, using the aluminium foil of 8cm diameter as electrode, its Parallel Symmetric is placed in electrolyte, the direct current of 60V is added at the two ends of electrode, two die openings are 0.5cm, electrophoresis 15min, obtain compound electric pole piece precursor;
Prepare compound electric pole piece:
After compound electric pole piece is dried naturally, vacuum bakeout 3 hours under 60 DEG C of conditions, then adding mass percent is in the aqueous solution of the ethylenediamine of 75%, temperature is adjusted to 80 DEG C, after liquid-phase reduction process 24h, then vacuumize 6h under 60 DEG C of conditions, obtains compound electric pole piece.
Embodiment four
Embodiment of the present invention combination electrode piece preparation method, comprises the steps:
By improve Hummers legal system for graphite oxide:
20g 50 order graphite powder, 10g potassium peroxydisulfate and 10g phosphorus pentoxide are added in the concentrated sulfuric acid of 80 DEG C, stir, cooling more than 6h, washing is to neutral, dry.Dried sample is added 0 DEG C, in the concentrated sulfuric acid of 460mL, then add 60g potassium permanganate, the temperature of mixture remains on less than 20 DEG C, after then keeping 2h in the oil bath of 35 DEG C, slowly adds 920mL deionized water.After 15min, add 2.8L deionized water (wherein containing 50mL concentration is the hydrogen peroxide of 30%) again, mixture color becomes glassy yellow afterwards, while hot suction filtration, then carries out washing with the hydrochloric acid that 5L concentration is 10%, suction filtration, namely obtain graphite oxide at 50 DEG C of vacuumize 48h.
Prepare the first solution:
Carbon nano-tube graphite oxide and nitric acid treatment crossed adds in isopropyl alcohol with the ratio of weight ratio 2: 1, ultrasonic 2h, stirs 1h, obtain homodisperse graphene oxide, carbon nano-tube solution under temperature is 30 DEG C of conditions;
Prepare compound electric pole piece precursor:
Zinc nitrate solution (Zn (the NO that concentration is 0.5mg/ml is added in the first solution
3)
26H
2o), ultrasonic 60min, obtain uniform second solution, using the second solution as electrolyte, using the nickel foil of 10cm diameter as electrode, its Parallel Symmetric is placed in electrolyte, the direct current of 80V is added at the two ends of electrode, two die openings are 0.5cm, electrophoresis 20min, obtain compound electric pole piece precursor;
Prepare compound electric pole piece:
After compound electric pole piece is dried naturally, vacuum bakeout 3 hours under 60 DEG C of conditions, then adding mass percent is in the aqueous solution of the hydroiodic acid of 85%, temperature is adjusted to 100 DEG C, after liquid-phase reduction process 24h, then vacuumize 12h under 60 DEG C of conditions, obtains compound electric pole piece.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. a combination electrode piece preparation method, comprises the steps:
Be that graphene oxide and the carbon nano-tube of 1 ~ 2:1 is added in alcoholic solvent by weight ratio, ultrasonic process, stirs, obtains the first solution;
In described first solution, add metal salt solution, ultrasonic process, obtain the second solution, with described second solution for electrolyte, take metal forming as electrode, carry out electrophoretic process, obtain compound electric pole piece precursor; Described slaine is Mg (NO
3)
26H
2o, Mg (SO
4)
27H
2o, Fe (NO
3)
39H
2o or Zn (NO
3)
26H
2one in O;
By described electrode slice precursor drying process, put into reducing solution, under temperature is 80 DEG C ~ 100 DEG C conditions, react 1 hour ~ 36 hours, by the vacuumize of reacted compound electric pole piece precursor, obtain compound electric pole piece.
2. combination electrode piece preparation method as claimed in claim 1, it is characterized in that, described carbon nano-tube is through acid-treated carbon nano-tube.
3. combination electrode piece preparation method as claimed in claim 1, it is characterized in that, described alcohol is carbon number is C
1~ C
6alcohol.
4. combination electrode piece preparation method as claimed in claim 1, it is characterized in that, prepare in the step of described first solution, sonication treatment time is 0.5 hour ~ 2 hours, and mixing time is 0.5 hour ~ 1 hour.
5. combination electrode piece preparation method as claimed in claim 3, it is characterized in that, the concentration of described metal salt solution is 0.2mg/ml ~ 0.5mg/ml.
6. combination electrode piece preparation method as claimed in claim 1, it is characterized in that, prepare in the step of described second solution, sonication treatment time is 15 minutes ~ 60 minutes.
7. combination electrode piece preparation method as claimed in claim 1, it is characterized in that, described reducing solution comprises hydrazine hydrate solution, sodium borohydride solution, quinol solution, ethylenediamine solution or hydroiodic acid solution.
8. combination electrode piece preparation method as claimed in claim 1, it is characterized in that, the mass percent of described reducing solution is 50% ~ 85%.
9. the application of compound electric pole piece in battery or capacitor prepared by combination electrode piece preparation method as described in any one of claim 1 ~ 8.
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| CN103346024B (en) * | 2013-06-18 | 2016-10-19 | 常州大学 | The preparation method of high-conductivity flexible graphene membrane electrode |
| CN103439381A (en) * | 2013-09-18 | 2013-12-11 | 桂林理工大学 | Method for detecting trace hydroquinone by using graphene/carbon nano tube modified electrode |
| CN104810426A (en) * | 2014-01-26 | 2015-07-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Self-driven light detector and preparation method thereof |
| CN105420794B (en) * | 2015-11-13 | 2018-01-26 | 上海应用技术学院 | A kind of preparation method of graphene/ferriferrous oxide composite material |
| WO2018032323A1 (en) * | 2016-08-16 | 2018-02-22 | 肖丽芳 | Electrodeposition method for manufacturing positive electrode of lithium-ion capacitor |
| WO2018032317A1 (en) * | 2016-08-16 | 2018-02-22 | 肖丽芳 | Electrodeposition method for manufacturing graphene foam |
| WO2018032320A1 (en) * | 2016-08-16 | 2018-02-22 | 肖丽芳 | Method for manufacturing sulfur composite graphene foam positive electrode |
| CN106848248A (en) * | 2017-03-08 | 2017-06-13 | 哈尔滨工业大学 | The preparation method of graphene-supported hollow carbon sphere composite |
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| CN101210339A (en) * | 2006-12-27 | 2008-07-02 | 上海比亚迪有限公司 | Method for preparing battery electrode |
| CN101734650A (en) * | 2009-12-23 | 2010-06-16 | 沈阳建筑大学 | Method for preparing graphene-carbon nano tube hybrid composite |
| CN101982408A (en) * | 2010-10-20 | 2011-03-02 | 天津大学 | Graphene three-dimensional material as well as preparation method and application thereof |
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| CN101210339A (en) * | 2006-12-27 | 2008-07-02 | 上海比亚迪有限公司 | Method for preparing battery electrode |
| CN101734650A (en) * | 2009-12-23 | 2010-06-16 | 沈阳建筑大学 | Method for preparing graphene-carbon nano tube hybrid composite |
| CN101982408A (en) * | 2010-10-20 | 2011-03-02 | 天津大学 | Graphene three-dimensional material as well as preparation method and application thereof |
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