CN110176332A - A kind of Graphene electrodes material and preparation method thereof - Google Patents
A kind of Graphene electrodes material and preparation method thereof Download PDFInfo
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- CN110176332A CN110176332A CN201910441450.7A CN201910441450A CN110176332A CN 110176332 A CN110176332 A CN 110176332A CN 201910441450 A CN201910441450 A CN 201910441450A CN 110176332 A CN110176332 A CN 110176332A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
The invention discloses a kind of Graphene electrodes materials and preparation method thereof; it is related to carbon nanomaterial preparation technology field; the Graphene electrodes material is prepared by polymethyl methacrylate and graphene film; the preparation method is that copper wire is used as graphene growth carrier at 950-1000 DEG C after annealed processing; using acetylene as carbon source, using hydrogen as protective gas, 3-4h is kept the temperature in 950-1000 DEG C; carbon atom sufficiently deposits on copper wire surface, generates single-layer graphene；PMMA/ graphene/copper wire is prepared, then using polymethyl methacrylate as binder with Fe (NO3)3Solution corrosion copper wire prepares PMMA/ graphene；Copper wire facilitates carbon atom and deposits bonded, generation single-layer graphene on copper atom surface by annealing in preparation method provided by the invention；By using methyl methacrylate, the grapheme material prepared can be shaped and be bonded, installs and takes when preparing electrode convenient for graphene.
Description
Technical field
The present invention relates to carbon nanomaterial preparation technology fields, and in particular to a kind of Graphene electrodes material and its preparation side
Method.
Background technique
Graphene is only made of carbon, forms carbon carbon covalent bond, graphite using sp2 hydridization form between each carbon atom
Alkene planar can be with infinite expanding, and in the scale perpendicular to only one atom of the direction of plane, therefore graphene can be with
It is defined as two-dimension nano materials, with the property that nano material is excellent.Graphene electron mass is close to zero, and it is in track
Movement velocity reach the 1/300 of the light velocity, conduction band and valence-band electrons intersect near fermi level, carrier present outlet
Property dispersion relation, therefore graphene have unique electronic structure and electrical properties, thus conductive film material, battery,
Capacitor, etc. technical fields have very big application potential.Graphene is two-dimensional free state crystal, between carbon carbon covalent bond
Bending angle is big, it is thus possible to which free bend produces fullerene, carbon nanotube and graphite, thus graphene is already received as carbon
Rice investigation of materials is set about a little and hot spot.Graphene production method includes expanded graphite ultrasound stripping method or ball-milling treatment method,
But obtained most of the graphene of both methods is the superimposed body of multi-layer graphene, it is difficult to obtain single layer truly
Graphene, and obtained graphene can not shape.
A kind of preparation method of graphene composite material is disclosed in the Chinese patent of Publication No. CN103373724A, it should
Method includes a resuspending step, a graphene film is added in a solvent, to obtain a graphite suspension, wherein graphene film is
The grapheme material of Multilayer stack；One strip step is become the graphene film removing in graphite suspension using mechanical forces
Multiple single-layer graphene materials, and obtain a graphene suspension；One separating step, by the mono-layer graphite in graphene suspension
Alkene material is separated with the graphene film that small part is not peeled off, and after the graphene film that removal small part is not peeled off, obtains a stone
Black alkene dispersion liquid；And one active material add step, be added an active material into graphene dispersing solution, active material and stone
Single-layer graphene in black alkene dispersion liquid is combined into graphene composite material, and obtains a graphene composite material dispersion liquid.
But this method and solution above-mentioned technical problem not yet in effect.
Summary of the invention
The purpose of the present invention is to provide a kind of Graphene electrodes materials and preparation method thereof, to solve above-mentioned background technique
The problem of middle proposition.
To achieve the above object, the present invention provides a kind of Graphene electrodes material and preparation method thereof, graphene electricity
Pole material is prepared by polymethyl methacrylate and graphene film.
Preferably, above-mentioned preparation method includes the following steps,
It washes, wash and each 8-15min of pickling Step 1: copper wire successively to be passed through to alcohol, it is then dry in high pure nitrogen；It takes
Copper wire after drying is immersed in corrosive liquid, soaking time 45-60s, then takes out copper wire, is stretched copper wire both ends, is made copper wire
Keep straight configuration；By the copper wire elder generation pickling after corrosion, then washes, finally dried in high pure nitrogen again；
Step 2: will be evacuated to inside device close to vacuum, then to hydrogen is passed through inside device it is restored to its internal pressure
Normal pressure；It then keeps being passed through H2, H2Flow is 500-700mL/min, and for constant heating rates sintering to 950-1000 DEG C, maintaining this temperature is 30-
40min makes annealing treatment copper wire；Then to the mixed gas for being passed through acetylene and hydrogen inside device, acetylene flow is
300-400mL/min, hydrogen flowing quantity 150-250mL/min, isothermal holding 3-4h make carbon atom be deposited on copper wire surface, obtain
To graphene film；
Step 2: prepare polymethyl methacrylate/acetone soln that mass fraction is 5%, it will wrap up in that bear graphene thin
The copper wire of film is dipped to polymethyl methacrylate/acetone soln, then it is dry to place it in vacuum by soaking time 5-10min
It keeps temperature to be 75-90 DEG C in dry case to be dried；After acetone volatilizees completely, PMMA/ graphene/copper wire is taken out, by copper wire
One end polishing, the PMMA and graphene that removal hinders copper to contact with corrosive liquid；Then PMMA/ graphene/copper wire is immersed in corruption
It loses in liquid, after copper wire is completely dissolved, picks up PMMA/ graphite composite material, rinsed well with deionized water, dried in the air in high pure nitrogen
It is dry, the column PMMA/ graphene composite material of inner hollow can be obtained.
Preferably, corrosive liquid is Fe (NO that concentration is 1-3mol/L in above-mentioned steps one and step 23)3Solution.
Preferably, alcohol washes operation and use mass fraction for 95% ethyl alcohol in above-mentioned steps one, and pickling operation is using quality
The hydrochloric acid that score is 25%.
Compared with prior art, beneficial effects of the present invention are as follows:
The present invention is using copper wire as carrier, and using acetylene as carbon source, under 950-1000 DEG C, atmosphere of hydrogen, carbon atom is in copper
Silk table face deposits, and generates single-layer graphene；Copper wire is activated at high temperature, helps by annealing, surface copper atom
Bonded, generation graphene is deposited on copper atom surface in carbon atom；By using methyl methacrylate, it can shape and bond
The grapheme material prepared is installed and is taken when preparing electrode convenient for graphene.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment one
It is successively 25% in ethyl alcohol, deionized water and the mass fraction that mass fraction is 95% by the copper wire that diameter is 20um
Hydrochloric acid solution in clean 8min, it is then dry in high pure nitrogen；It is 1mol/L's that copper wire after taking drying, which is immersed in concentration,
Fe(NO3)3In aqueous solution, soaking time 45s, copper wire passes through Fe (NO3)3Corrode in aqueous solution, after taking out copper wire, draws
Copper wire both ends are stretched, copper wire is made to keep straight configuration；The hydrochloric acid solution that mass fraction is 25% is first used to rush on the copper wire after corrosion
It washes, then reuses deionized water flushing, finally dried in high pure nitrogen；Copper wire is placed on quartz slide, it will be quartzy
Slide glass is pushed into quartz ampoule pipe outer end close to the position of thermocouple.Lead to after being evacuated to pressure≤5Pa inside device, then to inside device
Entering hydrogen makes its internal pressure be restored to normal pressure；It then keeps being passed through H2, H2Flow is 500mL/min, constant heating rates sintering to 950 DEG C,
This temperature 30min is maintained, copper wire is made annealing treatment；Then to the mixed gas for being passed through acetylene and hydrogen inside device, second
Alkynes flow is 300mL/min, and hydrogen flowing quantity 150mL/min, isothermal holding 3h make carbon atom be deposited on copper wire surface, obtain
Graphene film；Polymethyl methacrylate/acetone soln that mass fraction is 5% is prepared, bears graphene film for wrapping up in
Copper wire is dipped to polymethyl methacrylate/acetone soln, then soaking time 5min is placed it in vacuum oven and protected
Temperature is held to be dried for 75 DEG C；After acetone volatilizees completely, PMMA/ graphene/copper wire is taken out, copper wire one end is polished, is gone
Except the PMMA and graphene for hindering copper to contact with corrosive liquid；Prepare the Fe (NO that mass fraction is 25%3)3Aqueous solution is as corrosion
Then PMMA/ graphene/copper wire is immersed in corrosive liquid by liquid, after copper wire is completely dissolved, pick up PMMA/ graphite composite wood
Material, is rinsed well with deionized water, is air-dried, can be obtained the column PMMA/ graphene composite material of inner hollow, the composite material
It can be used for battery electrode material.
Embodiment two
It is successively 25% in ethyl alcohol, deionized water and the mass fraction that mass fraction is 95% by the copper wire that diameter is 20um
Hydrochloric acid solution in clean 15min, it is then dry in high pure nitrogen；It is 3mol/L's that copper wire after taking drying, which is immersed in concentration,
Fe(NO3)3In aqueous solution, soaking time 60s, copper wire passes through Fe (NO3)3Corrode in aqueous solution, after taking out copper wire, draws
Copper wire both ends are stretched, copper wire is made to keep straight configuration；The hydrochloric acid solution that mass fraction is 25% is first used to rush on the copper wire after corrosion
It washes, then reuses deionized water flushing, finally dried in high pure nitrogen；Copper wire is placed on quartz slide, it will be quartzy
Slide glass is pushed into quartz ampoule pipe outer end close to the position of thermocouple.Lead to after being evacuated to pressure≤5Pa inside device, then to inside device
Entering hydrogen makes its internal pressure be restored to normal pressure；It then keeps being passed through H2, H2Flow is 700mL/min, constant heating rates sintering to 1000
DEG C, this temperature 40min is maintained, copper wire is made annealing treatment；Then to the mixed gas for being passed through acetylene and hydrogen inside device,
Acetylene flow is 400mL/min, and hydrogen flowing quantity 250mL/min, isothermal holding 4h make carbon atom be deposited on copper wire surface, obtain
To graphene film；
Polymethyl methacrylate/acetone soln that mass fraction is 5% is prepared, the copper wire for bearing graphene film will be wrapped up in
It is dipped to polymethyl methacrylate/acetone soln, then soaking time 10min is placed it in vacuum oven and kept
Temperature is 90 DEG C and is dried；After acetone volatilizees completely, PMMA/ graphene/copper wire is taken out, copper wire one end is polished, removed
The PMMA and graphene for hindering copper to contact with corrosive liquid；Prepare the Fe (NO that mass fraction is 25%3)3Aqueous solution as corrosive liquid,
Then PMMA/ graphene/copper wire is immersed in corrosive liquid, after copper wire is completely dissolved, picks up PMMA/ graphite composite material,
It is rinsed well with deionized water, air-dries, the column PMMA/ graphene composite material of inner hollow can be obtained, which can
For battery electrode material.
Embodiment three
It is successively 25% in ethyl alcohol, deionized water and the mass fraction that mass fraction is 95% by the copper wire that diameter is 20um
Hydrochloric acid solution in clean 12min, it is then dry in high pure nitrogen；It is 2mol/L's that copper wire after taking drying, which is immersed in concentration,
Fe(NO3)3In aqueous solution, soaking time 50s, copper wire passes through Fe (NO3)3Corrode in aqueous solution, after taking out copper wire, draws
Copper wire both ends are stretched, copper wire is made to keep straight configuration；The hydrochloric acid solution that mass fraction is 25% is first used to rush on the copper wire after corrosion
It washes, then reuses deionized water flushing, finally dried in high pure nitrogen；
Copper wire is placed on quartz slide, quartz slide is pushed into quartz ampoule pipe outer end close to the position of thermocouple.It will
After being evacuated to pressure≤5Pa inside device, then its internal pressure is set to be restored to normal pressure to hydrogen is passed through inside device；It then keeps logical
Enter H2, H2Flow is 600mL/min, and constant heating rates sintering maintains this temperature 35min, make annealing treatment to copper wire to 975 DEG C；Then
The mixed gas of acetylene and hydrogen is passed through inside to device, acetylene flow is 350mL/min, hydrogen flowing quantity 200mL/min, is protected
Temperature processing 3-4h, makes carbon atom be deposited on copper wire surface, obtains graphene film；
Polymethyl methacrylate/acetone soln that mass fraction is 5% is prepared, the copper wire for bearing graphene film will be wrapped up in
It is dipped to polymethyl methacrylate/acetone soln, then soaking time 7min is placed it in and kept temperature in vacuum oven
Degree is dried for 80 DEG C；After acetone volatilizees completely, PMMA/ graphene/copper wire is taken out, copper wire one end is polished, removal resistance
The PMMA and graphene for hindering copper to contact with corrosive liquid；Prepare the Fe (NO that mass fraction is 25%3)3Aqueous solution is as corrosive liquid, so
PMMA/ graphene/copper wire is immersed in corrosive liquid afterwards, after copper wire is completely dissolved, picks up PMMA/ graphite composite material, is used
Deionized water is rinsed well, is air-dried, and the column PMMA/ graphene composite material of inner hollow can be obtained, and the composite material is available
In battery electrode material.
The PMMA/ graphene dissolution that embodiment one, embodiment two and embodiment three are prepared in acetone, is then pulled out
Graphene measures single-layer graphene thickness, single-layer graphene prepared by each embodiment is selected five pieces, is superimposed, and surveys
Amount superposition after graphene film heap sheet resistance and work function, using single-layer graphene as anode prepare carboxylated graphene/
Glass-carbon electrode (GO-COOH/GCE), measuring electrode energy conversion efficiency, such as following table embodiment one, embodiment two and embodiment three
Shown in corresponding column data；Graphene is obtained from graphite as a comparison case according to tradition machinery stripping method, measures single-layer graphene
Five pieces of single-layer graphenes are superimposed by thickness, the sheet resistance and work function of graphene film heap after measurement superposition, with list
Layer graphene is that anode prepares carboxylated graphene/glass-carbon electrode (GO-COOH/GCE), measures electrode energy conversion effect
Rate, as shown in following table comparative example column data.By single-layer graphene thickness in following table it can be deduced that preparation method provided by the invention
Prepared graphene is single layer structure, and the graphene for using existing machinery stripping means to prepare is multi-layer graphene stacking
Gained.Graphene surface resistance provided by the invention is smaller, and work function is larger, and after being prepared into electrode, energy conversion efficiency
It is high.Therefore, graphene electric property prepared by the present invention is more excellent.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (4)
1. a kind of Graphene electrodes material and preparation method thereof, which is characterized in that the Graphene electrodes material is by polymethyl
Sour methyl esters and graphene film preparation.
2. Graphene electrodes material according to claim 1 and preparation method thereof, which is characterized in that the preparation method includes
Following steps,
It washes, wash and each 8-15min of pickling Step 1: copper wire successively to be passed through to alcohol, it is then dry in high pure nitrogen；Take drying
Copper wire afterwards is immersed in corrosive liquid, soaking time 45-60s, then takes out copper wire, is stretched copper wire both ends, is kept copper wire
Straight configuration；By the copper wire elder generation pickling after corrosion, then washes, finally dried in high pure nitrogen again；
Step 2: will be evacuated to inside device close to vacuum, then its internal pressure is set to be restored to normal pressure to hydrogen is passed through inside device；
It then keeps being passed through H2, H2Flow is 500-700 mL/min, and for constant heating rates sintering to 950-1000 DEG C, maintaining this temperature is 30-
40min makes annealing treatment copper wire；Then to the mixed gas for being passed through acetylene and hydrogen inside device, acetylene flow is
300-400mL/min, hydrogen flowing quantity are 150-250 mL/min, and isothermal holding 3-4h makes carbon atom be deposited on copper wire surface, obtains
To graphene film；
Step 2: preparing polymethyl methacrylate/acetone soln that mass fraction is 5%, the copper for bearing graphene film will be wrapped up in
Silk is dipped to polymethyl methacrylate/acetone soln, then soaking time 5-10min is placed it in vacuum oven
It keeps temperature to be 75-90 DEG C to be dried；After acetone volatilizees completely, PMMA/ graphene/copper wire is taken out, copper wire one end is beaten
Mill, the PMMA and graphene that removal hinders copper to contact with corrosive liquid；Then PMMA/ graphene/copper wire is immersed in corrosive liquid,
After copper wire is completely dissolved, PMMA/ graphite composite material is picked up, is rinsed well with deionized water, is dried in high pure nitrogen
Obtain the column PMMA/ graphene composite material of inner hollow.
3. Graphene electrodes material according to claim 2 and preparation method thereof, which is characterized in that the step 1 and step
Corrosive liquid is the Fe (NO that concentration is 1-3mol/L in rapid two3)3Solution.
4. Graphene electrodes material according to claim 2 and preparation method thereof, which is characterized in that alcohol in the step 1
Wash operation use mass fraction for 95% ethyl alcohol, pickling operation use mass fraction for 25% hydrochloric acid.
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| CN201910441450.7A CN110176332A (en) | 2019-05-24 | 2019-05-24 | A kind of Graphene electrodes material and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586869A (en) * | 2012-01-20 | 2012-07-18 | 中国科学院上海硅酸盐研究所 | Three-dimensional grapheme tube and preparation method thereof |
| CN104827021A (en) * | 2015-04-09 | 2015-08-12 | 山东师范大学 | Method for preparing high-conductivity stretchable sponge graphene-based electrode material |
| US20150273737A1 (en) * | 2014-04-01 | 2015-10-01 | National Taiwan University | Flexible and stretchable graphene film and preparing method of the same |
| CN105449016A (en) * | 2015-12-16 | 2016-03-30 | 苏州矩阵光电有限公司 | Graphene silicon solar cell and manufacturing method |
-
2019
- 2019-05-24 CN CN201910441450.7A patent/CN110176332A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586869A (en) * | 2012-01-20 | 2012-07-18 | 中国科学院上海硅酸盐研究所 | Three-dimensional grapheme tube and preparation method thereof |
| US20150273737A1 (en) * | 2014-04-01 | 2015-10-01 | National Taiwan University | Flexible and stretchable graphene film and preparing method of the same |
| CN104827021A (en) * | 2015-04-09 | 2015-08-12 | 山东师范大学 | Method for preparing high-conductivity stretchable sponge graphene-based electrode material |
| CN105449016A (en) * | 2015-12-16 | 2016-03-30 | 苏州矩阵光电有限公司 | Graphene silicon solar cell and manufacturing method |
Non-Patent Citations (1)
| Title |
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