CN114914100A - graphene/MXene composite film and preparation method thereof - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000004793 Polystyrene Substances 0.000 claims abstract description 40
- 229920002223 polystyrene Polymers 0.000 claims abstract description 40
- 239000002077 nanosphere Substances 0.000 claims abstract description 38
- 239000007864 aqueous solution Substances 0.000 claims abstract description 33
- 239000006185 dispersion Substances 0.000 claims abstract description 22
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 9
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- 229920002301 cellulose acetate Polymers 0.000 claims description 4
- 229920002492 poly(sulfone) Polymers 0.000 claims description 4
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- 238000004519 manufacturing process Methods 0.000 claims 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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 discloses a graphene/MXene composite film and a preparation method thereof, wherein the preparation method comprises the following steps: preparing MXene aqueous solution, graphene oxide aqueous solution and polystyrene nanosphere dispersion liquid; mixing the MXene aqueous solution, the graphene oxide aqueous solution and the polystyrene nanosphere dispersion liquid, performing ultrasonic dispersion to obtain a mixed solution, and covering the mixed solution on the surface of a film through vacuum filtration to obtain a composite film; and calcining the composite film in an inert atmosphere to obtain the graphene/MXene composite film. The preparation method provided by the invention is simple, the reaction condition is mild, and the large-scale production is easy to realize, the prepared graphene/MXene composite film has a multistage mesoporous structure, the aggregation of graphene and MXene is weakened, so that the graphene/MXene composite film has better capacitance performance, has good bending flexibility, and is expected to be directly used as an electrode material of a flexible supercapacitor.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a graphene/MXene composite film and a preparation method thereof.
Background
Graphene and MXene have gained much attention in recent years due to their unique lamellar structure and excellent physicochemical properties. The graphene has low density, is easy to prepare, has excellent thermal and chemical stability, and is easy to compound with other materials, and the form of the graphene assembly is various. MXene is a two-dimensional nano material and has the advantages of good hydrophilicity, adjustable conductivity and rich surface functional groups. The composite film material based on the two is expected to be applied to the fields of electromagnetic shielding, coating, piezoresistive sensors, capacitance deionized water purification and the like.
The prior art discloses a plurality of preparation methods of graphene oxide and MXene composite membranes, but most of the two-dimensional materials are compositely loaded on the surface of a microfiltration membrane by a vacuum filtration method, but the graphene and the MXene are easy to aggregate, are not stable in combination and are easy to fall off in the using process.
Disclosure of Invention
In view of this, the invention provides a graphene/MXene composite film and a preparation method thereof, so as to solve the problem that the existing graphene/MXene composite film is poor in performance.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a preparation method of a graphene/MXene composite film comprises the following steps:
s1, preparing MXene aqueous solution, graphene oxide aqueous solution and polystyrene nanosphere dispersion liquid;
s2, mixing the MXene aqueous solution, the graphene oxide aqueous solution and the polystyrene nanosphere dispersion liquid, performing ultrasonic dispersion to obtain a mixed solution, and covering the mixed solution on the surface of a film through vacuum filtration to obtain a composite film;
and S3, calcining the composite film in an inert atmosphere to obtain the graphene/MXene composite film.
Optionally, in step S1, the concentration of the MXene aqueous solution is in a range of 2mg/mL to 4mg/mL, the concentration of the graphene oxide aqueous solution is in a range of 2mg/mL to 6mg/mL, and the concentration of the polystyrene nanosphere dispersion is in a range of 10mg/mL to 20 mg/mL.
Optionally, in the polystyrene nanosphere dispersion, the diameter of the polystyrene nanospheres is in the range of 100nm to 300 nm.
Optionally, in the mixed solution in step S2, the ratio of the MXene, the graphene oxide, and the polystyrene nanospheres in parts by mass is (3-6): (5-10): (1-2).
Optionally, in step S2, the time of the ultrasonic dispersion is in the range of 10min to 30 min.
Alternatively, in step S3, the calcination is at a temperature in the range of 500 ℃ to 600 ℃ for a time in the range of 2h to 4 h.
Optionally, the material of the film comprises one of polysulfone, polyethersulfone, polyvinylidene fluoride, cellulose acetate and mixed cellulose ester.
On the basis of the scheme, the second purpose of the invention is to provide the graphene/MXene composite film, which is prepared by the preparation method of the graphene/MXene composite film.
Optionally, the graphene/MXene composite film has a multilevel mesoporous structure.
Compared with the prior art, the invention has the following advantages:
the preparation method provided by the invention is simple, the reaction condition is mild, and the large-scale production is easy to realize, the prepared graphene/MXene composite film has a multistage mesoporous structure, the aggregation of graphene and MXene is weakened, so that the graphene/MXene composite film has better capacitance performance, has good bending flexibility, and is expected to be directly used as an electrode material of a flexible supercapacitor.
Drawings
In order to more clearly illustrate the technical solutions of the present invention or the prior art, some brief descriptions will be given below to the drawings used in the description of the embodiments or the prior art, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a scanning electron microscope image of the graphene/MXene composite film according to embodiment 1 of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
It should be noted that in the description of the embodiments herein, the description of the term "some embodiments" means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. Throughout this specification, the schematic representations of the terms used above do not necessarily refer to the same implementation or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The term "in.. range" as used herein includes both ends, such as "in the range of 1 to 100" including both ends of 1 and 100.
MXene(Ti 3 C 2 T x ) Is a novel two-dimensional transition metal carbide or carbonitride, and the MAX phase (Ti) is selectively removed by chemical etching and other methods 3 AlC 2 ) A atomic layer of (a). MXene can be represented by the chemical general formula M n+1 X n T x (wherein M is an early transition metal element, X represents carbon or nitrogen, and T is a surface-attached active group). MXene has high specific surface area, adjustable and controllable interlayer spacing and components, and rich-OH, O and other hydrophilic functional groups on the surface, so that MXene can be well dispersed in an aqueous solution. The nano composite film constructed by MXene as a matrix and graphene oxide has very strong plasticity and flexibility. However, graphene and MXene are easy to aggregate, and the two are combined and combinedTherefore, how to construct a composite membrane with stable structure and good electrochemical performance is a valuable subject at present.
In order to solve the above problem, an embodiment of the present invention provides a preparation method of a graphene/MXene composite film, including the following steps:
s1, preparing MXene aqueous solution, graphene oxide aqueous solution and polystyrene nanosphere dispersion liquid;
s2, mixing the MXene aqueous solution, the graphene oxide aqueous solution and the polystyrene nanosphere dispersion liquid, performing ultrasonic dispersion to obtain a mixed solution, and covering the mixed solution on the surface of the film through vacuum filtration to obtain a composite film;
and S3, calcining the composite film in an inert atmosphere to obtain the graphene/MXene composite film.
Specifically, in step S1, commercial MXene, graphene oxide, and polystyrene nanospheres are dispersed in deionized water to prepare 2-4mg/mL MXene aqueous solution, 2-6mg/mL graphene oxide aqueous solution, and 10-20mg/mL polystyrene nanosphere aqueous dispersion. Of course, the above-mentioned materials may be self-made, and are not particularly limited herein.
Preferably, the polystyrene nanospheres have a diameter in the range of 100nm to 300 nm.
Specifically, in step S2, the ratio of MXene to graphene oxide to polystyrene nanosphere in parts by mass is (3-6): (5-10): (1-2), magnetically stirring, and dispersing in an ultrasonic cleaning instrument for 10-30min to obtain a mixed solution.
Fixing the film on a vacuum filtration device, pouring the mixed dispersion into a vacuum filtration cup, starting a vacuum pump, and continuing to carry out vacuum filtration for 30-40min after water is completely filtered to obtain the composite film.
Wherein, the material of the film comprises one of polysulfone, polyethersulfone, polyvinylidene fluoride, cellulose acetate and mixed cellulose ester.
Specifically, in step S3, the composite membrane is placed in a tube furnace and calcined at 500-600 ℃ for 2-4h,
further, the inert atmosphere includes argon or nitrogen, preferably an argon atmosphere.
Therefore, in the embodiment of the invention, the graphene oxide, MXene and polystyrene nanospheres are uniformly mixed in water, and then the mixture is subjected to suction filtration to obtain the composite film, and then the composite film is calcined at a high temperature to obtain the graphene/MXene composite film. The preparation process is simple and convenient, complex reaction conditions and equipment are not needed, the polystyrene nanospheres participate in the formation of the composite film in the suction filtration process, and the polystyrene nanospheres are derived into carbon during high-temperature calcination, so that the composite film has a multistage mesoporous structure, and the aggregation of graphene and MXene is weakened; in addition, in the composite film, the graphene, MXene and polystyrene derived carbon act synergistically, so that the capacitance performance of the composite film is improved, and the graphene/MXene composite film has good bending flexibility and is expected to be directly used as an electrode material of a flexible supercapacitor.
On the basis of the scheme, another embodiment of the invention provides a graphene/MXene composite film, which is prepared by the preparation method of the graphene/MXene composite film.
On the basis of the above embodiments, the present invention is further illustrated by the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The following examples are examples of experimental procedures not specified under specific conditions, generally according to the conditions recommended by the manufacturer. Unless otherwise indicated, percentages and parts are by mass.
Example 1
The embodiment provides a preparation method of a graphene/MXene composite film, which comprises the following steps:
1) preparing MXene into an aqueous solution with the concentration of 2mg/mL, preparing graphene oxide into an aqueous solution with the concentration of 4mg/mL, and preparing a polystyrene nanosphere with the diameter of 100nm into an aqueous dispersion with the concentration of 10 mg/mL;
2) mixing MXene solution, graphene oxide solution and polystyrene nanosphere water dispersion liquid, and performing ultrasonic treatment for 15min, wherein the mass part ratio of MXene to graphene oxide to polystyrene nanospheres is 3: 6: 2, performing suction filtration on the polyvinylidene fluoride filter membrane to obtain a composite membrane;
3) and calcining the composite film for 3 hours at 500 ℃ in an argon atmosphere to obtain the graphene/MXene composite film.
The graphene/MXene composite film prepared in example 1 is characterized to obtain a scanning electron microscope image shown in fig. 1, and as can be seen from fig. 1, the graphene/MXene composite film has a layered multilevel structure.
The graphene/MXene composite film prepared in example 1 was directly used as a working electrode, a silver/silver chloride electrode as a reference electrode, a platinum wire as a counter electrode, and 1mol/L sulfuric acid as a supporting electrolyte, and charge and discharge tests were performed at a current density of 1A/g. Measuring the specific capacitance of the graphene/MXene composite film to be 562F/g; after 100 times of bending, the specific capacitance of the composite film was again measured to be 534F/g. It can be seen that the specific capacitance does not change much after 100 times of bending, that is, the graphene/MXene composite film has good specific capacitance performance and can be used as a flexible supercapacitor electrode material.
Example 2
The embodiment provides a preparation method of a graphene/MXene composite film, which comprises the following steps:
1) MXene is prepared into aqueous solution with the concentration of 3mg/mL, graphene oxide is prepared into aqueous solution with the concentration of 4mg/mL, and polystyrene nanospheres with the diameters of 200nm are prepared into aqueous dispersion with the concentration of 15 mg/mL;
2) mixing MXene solution, graphene oxide solution and polystyrene nanosphere water dispersion, and performing ultrasonic treatment for 10min, wherein the mass part ratio of MXene to graphene oxide to polystyrene nanospheres is 3: 6: 1, performing suction filtration on a polysulfone filter membrane to obtain a composite membrane;
3) and calcining the composite film for 2.5h at 550 ℃ under argon atmosphere to obtain the graphene/MXene composite film.
The graphene/MXene composite film prepared in example 2 was directly used as a working electrode, a silver/silver chloride electrode as a reference electrode, a platinum wire as a counter electrode, and 1mol/L sulfuric acid as a supporting electrolyte, and charge and discharge tests were performed at a current density of 1A/g. Measuring the specific capacitance of the composite film to be 504F/g; after bending 100 times, the specific capacitance of the composite film was measured again to be 473F/g.
Example 3
The embodiment provides a preparation method of a graphene/MXene composite film, which comprises the following steps:
1) preparing MXene into an aqueous solution with the concentration of 4mg/mL, preparing graphene oxide into an aqueous solution with the concentration of 2mg/mL, and preparing a polystyrene nanosphere with the diameter of 300nm into an aqueous dispersion with the concentration of 20 mg/mL;
2) mixing MXene solution, graphene oxide solution and polystyrene nanosphere water dispersion, and performing ultrasonic treatment for 10min, wherein the mass part ratio of the MXene to the graphene oxide to the polystyrene nanosphere is 2: 8: 2, carrying out suction filtration on the polyether sulfone filter membrane to obtain a composite membrane;
3) and calcining the composite film for 2 hours at 600 ℃ in an argon atmosphere to obtain the graphene/MXene composite film.
The graphene/MXene composite film prepared in example 3 was directly used as a working electrode, a silver/silver chloride electrode as a reference electrode, a platinum wire as a counter electrode, and 1mol/L sulfuric acid as a supporting electrolyte, and charge and discharge tests were performed at a current density of 1A/g. Measuring the specific capacitance of the composite film to be 513F/g; after 100 times of bending, the specific capacitance of the composite film was again measured to be 464F/g.
Example 4
The embodiment provides a preparation method of a graphene/MXene composite film, which comprises the following steps:
1) preparing MXene into an aqueous solution with the concentration of 2mg/mL, preparing graphene oxide into an aqueous solution with the concentration of 6mg/mL, and preparing the polystyrene nanospheres with the diameters of 150nm into an aqueous dispersion with the concentration of 15 mg/mL;
2) mixing MXene solution, graphene oxide solution and polystyrene nanosphere water dispersion, and performing ultrasonic treatment for 10min, wherein the mass part ratio of MXene to graphene oxide to polystyrene nanospheres is 3: 6: 2, carrying out suction filtration on the cellulose acetate filter membrane to obtain a composite membrane;
3) and calcining the composite film for 2 hours at 500 ℃ in an argon atmosphere to obtain the graphene/MXene composite film.
The graphene/MXene composite film prepared in example 4 was directly used as a working electrode, a silver/silver chloride electrode as a reference electrode, a platinum wire as a counter electrode, and 1mol/L sulfuric acid as a supporting electrolyte, and charge and discharge tests were performed at a current density of 1A/g. Measuring the specific capacitance of the composite film to be 453F/g; after 100 bends, the specific capacitance of the composite film was again measured to be 422F/g.
Comparative example 1
The comparative example provides a method of preparing a composite film comprising the steps of:
1) preparing MXene into an aqueous solution with the concentration of 2mg/mL, and preparing graphene oxide into an aqueous solution with the concentration of 4 mg/mL;
2) mixing the MXene solution and the graphene oxide solution, performing ultrasonic treatment for 15min, wherein the mass part ratio of the MXene to the graphene oxide is 3, and performing suction filtration on a polyvinylidene fluoride filter membrane to obtain a composite film;
3) calcining the composite film obtained in the step 2) for 3 hours at 500 ℃ in an argon atmosphere to obtain the graphene/MXene composite film.
The composite film prepared in comparative example 1 was directly used as a working electrode, a silver/silver chloride electrode as a reference electrode, a platinum wire as a counter electrode, and 1mol/L sulfuric acid as a supporting electrolyte, and a charge/discharge test was performed at a current density of 1A/g. Measuring the specific capacitance of the composite film to be 356F/g; after 100 times of bending, the specific capacitance of the composite film was again measured to be 312F/g.
In conclusion, the embodiment shows that the polystyrene nanospheres are added, the polystyrene nanospheres participate in the formation of the composite film in the suction filtration process, and the polystyrene nanospheres are derived into carbon during high-temperature calcination, so that the composite film has a multistage mesoporous structure, and the graphene, MXene and polystyrene derived carbon have synergistic effects, thereby improving the capacitance performance of the composite film.
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Various changes and modifications may be effected therein by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present disclosure, and these changes and modifications are intended to be within the scope of the present disclosure.
Claims (9)
1. The preparation method of the graphene/MXene composite film is characterized by comprising the following steps:
s1, preparing MXene aqueous solution, graphene oxide aqueous solution and polystyrene nanosphere dispersion liquid;
s2, mixing the MXene aqueous solution, the graphene oxide aqueous solution and the polystyrene nanosphere dispersion liquid, performing ultrasonic dispersion to obtain a mixed solution, and performing vacuum filtration on the mixed solution to cover the surface of a film to obtain a composite film;
and S3, calcining the composite film in an inert atmosphere to obtain the graphene/MXene composite film.
2. The preparation method according to claim 1, wherein in step S1, the concentration of the MXene aqueous solution is in a range of 2mg/mL to 4mg/mL, the concentration of the graphene oxide aqueous solution is in a range of 2mg/mL to 6mg/mL, and the concentration of the polystyrene nanosphere dispersion is in a range of 10mg/mL to 20 mg/mL.
3. The method of claim 2, wherein the polystyrene nanosphere dispersion has a diameter of polystyrene nanospheres ranging from 100nm to 300 nm.
4. The preparation method according to any one of claims 1 to 3, wherein in the mixed solution in the step S2, the ratio of MXene, graphene oxide and polystyrene nanospheres in parts by mass is (3-6): (5-10): (1-2).
5. The production method according to claim 4, wherein in step S2, the time for ultrasonic dispersion is in the range of 10min to 30 min.
6. The method according to claim 4, wherein in step S3, the calcining temperature is in the range of 500 ℃ to 600 ℃ and the calcining time is in the range of 2h to 4 h.
7. The method according to claim 4, wherein the material of the film comprises one of polysulfone, polyethersulfone, polyvinylidene fluoride, cellulose acetate and mixed cellulose ester.
8. The graphene/MXene composite film is characterized by being prepared by the preparation method of the graphene/MXene composite film according to any one of claims 1-7.
9. The graphene/MXene composite film according to claim 8, wherein the graphene/MXene composite film has a hierarchical mesoporous structure.
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| CN115521553A (en) * | 2022-10-11 | 2022-12-27 | 昆明理工大学 | Preparation method and application of graphene/MXene/polystyrene composite material |
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