CN111341568A - Preparation method of graphene mixed film - Google Patents
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- CN111341568A CN111341568A CN202010187411.1A CN202010187411A CN111341568A CN 111341568 A CN111341568 A CN 111341568A CN 202010187411 A CN202010187411 A CN 202010187411A CN 111341568 A CN111341568 A CN 111341568A
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- 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
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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Abstract
The invention provides a preparation method of a graphene mixed film, which comprises the following steps: step 1, mixing and dispersing graphene and another nano material in a proper surfactant and solvent combination at normal temperature to obtain a stable mixed dispersion liquid; step 2, taking the porous filter membrane as a substrate at normal temperature, carrying out vacuum filtration on the mixed dispersion liquid, and stacking the graphene and another nano material on the surface of the porous filter membrane to form a graphene mixed film; and drying the surface moisture of the graphene mixed film to obtain the graphene mixed film. The invention has the beneficial effects that: the method is characterized in that a proper surfactant and solvent combination is selected, then graphene and the nano material are mixed and dispersed in the selected surfactant and solvent combination to obtain a stable mixed dispersion liquid, and the stable mixed dispersion liquid is subjected to vacuum filtration to prepare the graphene mixed film, wherein the thickness and the material proportion of the graphene mixed film are accurate and adjustable. The method has the advantages of simple process, low cost, convenience for large-scale production, economy and practicality.
Description
Technical Field
The invention relates to the technical field of nano material films, in particular to a preparation method of a graphene mixed film.
Background
The nano material shows some unique properties on a nano scale, such as small size effect, surface effect and the like, so that the nano material shows special excellent performance in many aspects such as thermal, mechanical, magnetic and chemical properties. Among them, zero-dimensional nanomaterials, such as fullerene C60 and quantum dots, and one-dimensional nanomaterials, such as silver nanowires, manganese dioxide nanowires, carbon nanotubes, etc., have been widely used in the fields of catalysis, electronics, biomedicine, aerospace, etc.
Graphene is a two-dimensional honeycomb lattice structure formed by closely arranging monolayer carbon atoms in six-membered rings, which is discovered for the first time in 2004, and has special electrical properties and physicochemical properties. The direct application of graphene also faces a great challenge, and the application of graphene film as a two-dimensional material in the fields of OLEDs, energy storage, flexible electronics, sensors, filter membranes and the like gradually enters commercialization.
The preparation of the graphene film mainly comprises the following methods: coating, spin coating, self-assembly, electrophoresis, electrochemical, spray coating, and suction filtration. The vacuum filtration method has the advantages of simple and accurate control of the thickness of the film, normal-temperature preparation, simple process and the like, and is widely used in practical application. In patent CN 107331523B (grant date: 2019.10.15), three carbon nanomaterials of activated carbon, carbon nanotubes and graphene are mixed and filtered to form a three-dimensional composite film, and thermal reduction is performed at 300-350 ℃.
The relevant documents are as follows:
Vaia,Richard A.,and H.Daniel Wagner.Framework forNanocomposites.Materi als Today 2004,7(11):32–37,DOI:10.1016/S1369-7021(04)00506-1.
Rao,C.N.R.,A.K.Sood,K.S.Subrahmanyam,and A.Govindaraj.Graphene:TheNew Two-Dimensional Nanomaterial.Angewandte Chemie 2009,48(42):7752–77,DOI:10.1002/anie.200901678.
Raccichini,Rinaldo,Alberto Varzi,Stefano Passerini,and BrunoScrosati.T he Role of Graphene for Electrochemical Energy Storage.NatureMaterials 2015,14(3):271–79,DOI:10.1038/nmat4170.
Xu,Chaohe,Binghui Xu,Yi Gu,Zhigang Xiong,Jing Sun,and X.S.Zhao.Graphene-Based Electrodes for Electrochemical Energy Storage.Energy andEnvironment al Science 2013,6(5):1388–1414,DOI:10.1039/C3EE23870A.
Eda,Goki,Giovanni Fanchini,and Manish Chhowalla.Large-Area UltrathinFil ms of Reduced Graphene Oxide as a Transparent and Flexible ElectronicMaterial.Nature Nanotechnology 2008,3(5):270–74,DOI:10.1038/nnano.2008.83.
Becerril,Héctor A.,Jie Mao,Zunfeng Liu,Randall M.Stoltenberg,ZhenanBa o,and Yongsheng Chen.Evaluation of Solution-Processed Reduced GrapheneOxide F ilms as Transparent Conductors.ACS Nano 2008,2(3):463–70,DOI:10.1021/nn700375n.
Zhuangnan Li,Srinivas Gadipelli,Hucheng Li,Christopher A.Howard,DanJ.L.Brett,Paul R.Shearing,Zhengxiao Guo,Ivan P.Parkin and Feng Li.Tuning th einterlayer spacing of graphene laminate films for efficient pore utilizationt owards compact capacitive energy storage.Nature Energy 2020,5:160–168,DOI:10.1038/s41560-020-0560-6.
the active carbon/carbon nano tube/graphene composite material and the preparation method and the application thereof are as follows: CN201710612851.5,2017.07.25 are provided.
Disclosure of Invention
The invention provides a preparation method of a graphene mixed film, which comprises the steps of selecting a proper surfactant and solvent combination according to zeta potential, mixing and dispersing graphene and a nano material in the combination to obtain a stable mixed dispersion liquid, and carrying out vacuum filtration to prepare the graphene mixed film. The thickness and the material proportion of the graphene mixed film are accurate and adjustable, and the method is a technical invention with pertinence and practicability in the technical field.
The preparation method of the graphene mixed film comprises the following steps:
Preferably, the surfactant and solvent combination used in step 1 includes Sodium Dodecyl Sulfate (SDS) and water combination.
Preferably, a proper surfactant and solvent combination is selected according to the Zeta potential; when the combination is used for preparing a graphene dispersion liquid and another nano material dispersion liquid respectively, the Zeta potential value of the obtained dispersion liquid is more than 30mV, so that when the combination is used for preparing a mixed dispersion liquid of graphene and a nano material, the Zeta potential value of the obtained mixed dispersion liquid is more than 30 mV.
Preferably, the material ratio of the graphene mixed thin film can be controlled by controlling the mass of the graphene raw material and the other nanomaterial used for preparing the mixed dispersion liquid in step 1.
Preferably, the thickness of the graphene mixed thin film can be controlled by the volume or mass of the mixed dispersion used in the vacuum filtration in the step 2.
Preferably, the nanomaterial in step 1 is a carbon-based material such as activated carbon, carbon nanotubes and the like or a non-carbon-based material such as MnO2And the like.
Preferably, the dispersing method in step 1 includes: sonication, cell disruptor treatment, and the like.
Preferably, the material of the porous filter membrane in the step 2 includes polyvinylidene fluoride (PVDF), Polytetrafluoroethylene (PTFE), and aluminum oxide (Al)2O3) Polyether sulfone (PES), polypropylene (PP), and the like.
The invention provides a preparation method of a graphene mixed film, which selects a proper combination of a surfactant and a solvent to respectively prepare a graphene dispersion liquid and another nano-material dispersion liquid, wherein the Zeta potential value of the obtained dispersion liquid is more than 30 mV. And then mixing and dispersing the graphene and the nano material in the selected surfactant and solvent combination to obtain stable mixed dispersion liquid, and performing vacuum filtration to prepare the graphene mixed film. The thickness and the material proportion of the graphene mixed film are accurate and adjustable, and the method is a technical invention with pertinence and practicability in the technical field. The method has the advantages of simple process, low cost, convenience for large-scale production, economy and practicality.
Drawings
FIG. 1 is a flow chart of a method for preparing a graphene hybrid film;
FIG. 2 is an optical diagram of graphene, different nanomaterials, and a mixed dispersion of the two materials;
FIG. 3 is a graph of Zeta potential measurements for different dispersions;
FIG. 4 is an SEM (scanning electron microscope) image of different graphene mixed films;
FIG. 5 is a one-dimensional topography of different graphene mixed films measured by a step profiler;
FIG. 6 is a graph showing the relationship between the thickness and the specific mass per unit area of a graphene/carbon nanotube (1:1) mixed film obtained from a one-dimensional topography;
FIG. 7 is an I-V curve diagram of graphene/activated carbon mixed films in different proportions;
FIG. 8 is a graph showing the relationship between sheet resistance and mass per unit area of graphene/activated carbon mixed films in different ratios;
FIG. 9 is a schematic structural diagram of a supercapacitor using a graphene hybrid film as an electrode material;
FIG. 10 is a graph of electrochemical performance of a supercapacitor using a graphene/activated carbon (1:1) mixed film as an electrode material;
FIG. 11 is a graph of specific capacitance and energy density of a supercapacitor with graphene/activated carbon mixed films of different proportions as electrode materials;
fig. 12 is a graph of specific capacitance and energy density of a supercapacitor using graphene/activated carbon (1:1) mixed films of different unit area mass ratios as electrode materials.
Description of reference numerals: a current collector 1, an electrode material 2, a separator 3 and an organic electrolyte 4.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples are set forth merely to aid in the understanding of the invention. It should be noted that, for a person skilled in the art, several modifications can be made to the invention without departing from the principle of the invention, and these modifications and modifications also fall within the protection scope of the claims of the present invention.
The terminology used herein is for the purpose of describing particular example embodiments only and is not intended to be limiting, as the mass-metered form (5% wt.) and the time-metered form (0.5 hour) used herein may also represent other masses and times.
Fig. 1 is a process for preparing a graphene hybrid film. Firstly, a graphene raw material and another nano material are mixed by combining surfactant Sodium Dodecyl Sulfate (SDS) and solvent deionized water at normal temperature, and a mixed dispersion liquid is prepared by adopting methods of ultrasound, crushing and the like. The adopted graphene raw material is 5 wt% of graphene slurry, and the other nano material can be activated carbon, multi-walled carbon nano tube or MnO2. The graphene mixed film with different mass ratios can be obtained by changing the mass of the mixed graphene raw material and the nano material. The ultrasonic dispersion time was 0.5 hour, and then the mixed dispersion was obtained after disruption treatment for 1 hour (disruption intensity of 50%) using a cell disrupter (sonic VCX 750). Optical photographs of the prepared graphene dispersion, different nanomaterial dispersions, and graphene/different nanomaterial mixed dispersion are shown in fig. 2. A graph of the Zeta potential values for the different dispersions, as determined by means of a dynamic light scattering particle sizer (Brookhaven, Nono Brook Omni), is shown in FIG. 3. Graphene (GR) dispersion, 48.35mV (± 2.98); activated Carbon (AC) dispersion, 76.56mV (± 1.82); graphene-activated carbon (GR-AC) dispersion, 55.72mV (± 0.38); carbon Nanotube (CNTs) dispersion, 58.35mV (± 1.29); graphene-carbon nanotube (GR-CNTs) dispersion, 54.28mV (± 2.42); manganese dioxide (MnO)2) Dispersion, 46.39mV (± 1.66); graphene-manganese dioxide (GR-MnO)2) Dispersion, 50.16mV (± 1.25); under the condition of the same surface active agent,the Zeta potential values of all the dispersions of the graphene and the single nanometer material are both larger than 40mV, the Zeta potential values of the obtained mixed dispersion of the graphene and the nanometer material are both larger than 40mV and larger than 30mV required by stable dispersion, and the graphene and the mixed nanometer material can be stably and uniformly dispersed in the mixed dispersion simultaneously, so that the preparation of the graphene mixed film becomes possible.
And then, taking the porous filter membrane as a substrate, and stacking the graphene in the dispersion liquid and the mixed nano material on the filter membrane to form a film by vacuum filtration at normal temperature. The porous filter membrane used was a PVDF filter membrane. And drying the surface moisture to obtain the graphene mixed film on the filter membrane. The quality and thickness of the graphene mixed film can be accurately controlled by controlling the capacity of the mixed dispersion liquid subjected to suction filtration.
SEM electron micrographs of different graphene mixed films are shown in fig. 4. The specific mass per unit area of the mixed film was 0.72mg/c m2It is clear that the thin film is formed from graphene and mixed nanomaterial stacks. (a) Is a graphene/carbon nanotube (1:1) mixed film. (b) Is a graphene/activated carbon (1:1) mixed film. (c) Is graphene/MnO2(1:1) mixing the films.
The one-dimensional morphology of the graphene hybrid film measured by a step profiler (Bruker, Dektak XT-A) is shown in FIG. 5. (a) Is a mixed film of graphene/carbon nano tube (1:1) and has a specific mass per unit area of 0.07mg/cm2. The average thickness of the obtained mixed film was 1.5 μm, and the roughness was 0.26. mu.m. (b) Is a graphene/active carbon (1:1) mixed film with the mass per unit area of 0.72mg/cm2. The average thickness of the obtained mixed film was 18 μm, and the roughness was 1.13. mu.m.
The thickness curve of the graphene/carbon nanotube mixed film with different unit area specific masses obtained according to the measured one-dimensional topography is shown in fig. 6. The thickness of the hybrid film increases linearly with increasing specific mass per unit area.
By means of I14V23The I-V curve graph of the graphene/activated carbon mixed film with different proportions measured by the four-probe method is shown in FIG. 7. The adopted equipment is Solartron ModuLab XM electrochemistryA workstation. The specific mass per unit area of all the films was 0.72mg/cm2. The voltage varies linearly with the current, and the hybrid film exhibits a resistance characteristic.
By using a four-probe dual combination method (I)14V23And I12V34Combination) of graphene/activated carbon mixed films at different ratios are shown in fig. 8. The measuring equipment is a Suzhou crystal lattice ST2263 four-probe tester. When the specific mass is relatively small, the graphene mixed thin film exhibits a permeation (Percolation) phenomenon.
Fig. 9 shows a schematic structural diagram of a supercapacitor using a graphene mixed film as an electrode material. The current collectors 1 are positive and negative aluminum shells; the electrode material 2 is a graphene/activated carbon mixed film with the diameter of 12 mm; the diaphragm 3 is a PVDF porous filter membrane; the organic electrolyte 4 was 1M LiTFSI (DME: DOL ═ 1: 1).
The electrochemical performance test curve of the supercapacitor taking the graphene/activated carbon (1:1) mixed film as the electrode material is shown in fig. 10, and the specific mass per unit area is 0.72mg/cm2. (a) C-V cyclic voltammograms at different scanning rates; (b) is a charge-discharge curve under different current densities; under different current densities, the charge-discharge curves are linear and symmetrical, and higher charge-discharge efficiency is shown; (c) the cycle performance is shown. The current density is 0.5A/g, after 10000 charge-discharge cycles, the specific capacitance of the device is hardly degraded, and good coulombic efficiency is kept.
Specific capacitance and energy density maps of supercapacitors with different ratios of graphene/activated carbon mixed films as electrode materials under different current densities are shown in FIG. 11, and the specific mass per unit area is 0.72mg/cm2. Specific capacitance and energy density of supercapacitors with different graphene/activated carbon (1:1) mixed films in unit area mass as electrode materials at different current densities are shown in fig. 12.
Claims (2)
1. A preparation method of a graphene mixed film is characterized by comprising the following steps:
step 1, mixing and dispersing graphene and another nano material in a proper surfactant and solvent combination at normal temperature to obtain a stable mixed dispersion liquid;
step 2, taking the porous filter membrane as a substrate at normal temperature, carrying out vacuum filtration on the mixed dispersion liquid, and stacking the graphene and another nano material on the surface of the porous filter membrane to form a graphene mixed film; and drying the surface moisture of the graphene mixed film to obtain the graphene mixed film.
2. The method for preparing the graphene mixed thin film according to claim 1, wherein: selecting a proper surfactant and solvent combination according to Zeta potential; when the combination is used for preparing a graphene dispersion liquid and another nano material dispersion liquid respectively, the Zeta potential value of the obtained dispersion liquid is more than 30mV, and when the combination is used for preparing a mixed dispersion liquid of graphene and the nano material, the Zeta potential value of the obtained mixed dispersion liquid is more than 30 mV.
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| CN114613615A (en) * | 2022-04-08 | 2022-06-10 | 浙江浙能技术研究院有限公司 | Ultrathin polyoxyethylene-based solid electrolyte film and preparation method thereof |
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