CN114864297B - Preparation method of MXene/zinc oxide/graphene composite material - Google Patents

Preparation method of MXene/zinc oxide/graphene composite material Download PDF

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CN114864297B
CN114864297B CN202210577801.9A CN202210577801A CN114864297B CN 114864297 B CN114864297 B CN 114864297B CN 202210577801 A CN202210577801 A CN 202210577801A CN 114864297 B CN114864297 B CN 114864297B
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mxene
zinc oxide
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graphene composite
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CN114864297A (en
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苗保记
杨一帆
侯梦瑶
张永辉
陈秋玲
冯亚刚
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Henan University of Technology
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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
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/46—Metal oxides
    • 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
    • H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
    • 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
    • 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
    • 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
    • Y02E60/13—Energy storage using capacitors

Abstract

The invention discloses aA preparation method of an MXene/zinc oxide/graphene composite material belongs to the field of electrode materials of super capacitors. The preparation method comprises the following steps: by using concentrated hydrochloric acid and lithium fluoride to react with Ti 3 AlC 2 Etching to obtain MXene; then compounding the graphene oxide and zinc acetylacetonate to prepare a zinc oxide/graphene composite material; adding MXene and zinc oxide/graphene composite material powder into deionized water, transferring the mixture into a reaction kettle, and carrying out hydrothermal reaction to obtain the MXene/zinc oxide/graphene composite material. By adopting the preparation method, the problem of poor conductivity of zinc oxide of the conventional supercapacitor electrode material is solved, volume expansion in the charge-discharge process of the capacitor is prevented, the conductivity of the zinc oxide is improved, the number of active sites on the surface of the material is increased, the cycle performance is improved, the electrochemical performance and the stability of the composite material are improved, and the preparation method is simple in process and low in cost.

Description

Preparation method of MXene/zinc oxide/graphene composite material
Technical Field
The invention relates to the technical field of electrode materials of super capacitors, in particular to a preparation method of an MXene/zinc oxide/graphene composite material.
Background
The super capacitor is a novel energy storage device between a traditional capacitor and a battery, has the characteristics of high power density, high charge-discharge rate, good cycle stability and the like, and has important application in various fields such as vehicle energy, electronic products and the like. The electrode material is one of the key components of the super capacitor and plays a crucial role in the performance of the super capacitor.
Zinc oxide is an important wide bandgap semiconductor material, the bandgap width of which is 3.37eV, and has excellent characteristics in electrochemistry. The zinc oxide has the advantages of strong charge storage capacity, high energy density, large specific capacitance and the like, so that the zinc oxide has good application prospect in energy storage materials such as super capacitor batteries and the like, but the zinc oxide has the defects of poor conductivity, fast capacity attenuation and the like, and the zinc oxide is limited in wide application.
Therefore, compounding zinc oxide materials with other materials to improve the conductivity of the materials and improve the cycle performance of the materials, and preparing electrode materials meeting the expected electrochemical performance is an important way for promoting the development of capacitors.
Disclosure of Invention
The invention aims to provide a preparation method of an MXene/zinc oxide/graphene composite material, which solves the problem of poor conductivity of zinc oxide of the existing electrode material of a super capacitor, prevents volume expansion in the charge and discharge processes of the capacitor, improves the cycle performance, improves the electrochemical performance and stability of the composite material, and has simple process and low cost.
In order to achieve the purpose, the invention provides a preparation method of an MXene/zinc oxide/graphene composite material, which comprises the following steps:
s1, ti is reacted with concentrated hydrochloric acid and lithium fluoride 3 AlC 2 Etching, ultrasonically centrifuging, washing and drying to obtain MXene;
s2, compounding zinc acetylacetonate and graphene oxide by an in-situ synthesis method to obtain zinc oxide/graphene composite material powder;
s3, adding the MXene into 30ml of deionized water, and carrying out ultrasonic treatment to obtain a solution a;
s4, adding the prepared zinc oxide/graphene powder into the solution a, and stirring to obtain a solution b;
and S5, transferring the solution b into a reaction kettle for hydrothermal reaction, cooling, washing and drying to obtain the MXene/zinc oxide/graphene composite material.
Preferably, the specific step of step S1 is to add lithium fluoride into concentrated hydrochloric acid solution, stir until the lithium fluoride is dissolved, the stirring time is 15min, and then add Ti 3 AlC 2 Stirring the powder, heating and stirring for 60h at the reaction temperature of 35 ℃, washing and centrifuging the powder by using water, 2mol/L diluted hydrochloric acid and ethanol after the reaction is finished, washing for at least 10 times until the pH value is neutral,drying to obtain MXene.
Preferably, ti in said step S1 3 AlC 2 The mass of lithium fluoride and the volume ratio of the concentrated hydrochloric acid solution are 2g:2.5g:40mL.
Preferably, the specific steps of step 2 are to weigh the graphene oxide and add the graphene oxide into deionized water, perform ultrasonic processing, then add zinc acetylacetonate into the graphene oxide dispersion solution and stir the mixture, transfer the mixed solution into a polytetrafluoroethylene lining after the stirring is finished, seal the lining and put the lining into a high-pressure reaction kettle to perform hydrothermal reaction, cool the lining to room temperature after the reaction is finished, wash and centrifuge and dry the lining, and obtain the zinc oxide/graphene composite material.
Preferably, the graphene oxide is 0.03g in mass, the zinc acetylacetonate is 0.3886g in mass, the deionized water is 30mL, the ultrasonic time is 2h, the stirring time is 15min, the hydrothermal reaction temperature is 220 ℃, the hydrothermal reaction time is 12h, washing is performed by washing with deionized water and absolute ethyl alcohol for 2 times, and drying is performed at 60 ℃ for 24h.
Preferably, the MXene mass in the step S3 is 0.01-0.1 g, and the ultrasonic time is 1min.
Preferably, in the step S4, the mass of the zinc oxide/graphene powder is 0.01 to 1g, and the stirring time is 1min.
Preferably, the hydrothermal reaction in step S5 is carried out at 180 ℃ for 12h, the washing is carried out 3-5 times by using deionized water, the washing is carried out 3-5 times by using absolute ethyl alcohol, and the drying is carried out in a vacuum drying oven at 70 ℃ for 12h.
Preferably, the prepared MXene/zinc oxide/graphene composite material is used for preparing a supercapacitor negative electrode material.
Preferably, the specific steps for preparing the supercapacitor negative electrode material by using the MXene/zinc oxide/graphene composite material are as follows: mixing MXene/zinc oxide/graphene composite material, conductive carbon black and polyvinylidene fluoride according to the mass ratio of 8:1:1, fully and uniformly mixing, then coating on the foamed nickel, and drying to obtain the super capacitor negative electrode material.
Therefore, the preparation method of the MXene/zinc oxide/graphene composite material has the following beneficial effects:
(1) According to the invention, MXene and graphene are added in the preparation process, and a three-dimensional network structure formed by MXene and graphene on zinc oxide is beneficial to increase of the specific surface area, and a buffer area is formed by redundant space among zinc oxide, MXene and graphene, so that redundant electrolyte ions can be temporarily stored, the volume expansion in the charging and discharging process is prevented, and the cycle performance is improved;
(2) The MXene/zinc oxide/graphene composite material prepared by the method has a three-dimensional porous open structure, the three materials are mutually constrained, the interface of the MXene/zinc oxide/graphene composite material is effectively utilized, the number of active sites is increased, the three materials exert a synergistic effect, the defects of the materials are optimized on the basis of keeping respective electrochemical characteristics, and the electrochemical performance and the stability of the composite material are improved;
(3) The method used by the invention is a hydrothermal method, the material obtained by the hydrothermal method has small crystal size, uniform distribution and good electrochemical performance, and the method is clean and environment-friendly, has simple process and low cost.
The technical solution of the present invention is further described in detail by the following examples.
Drawings
Fig. 1 is an X-ray diffraction spectrum image of the MXene/zinc oxide/graphene composite of example 1;
fig. 2 is a scanning electron microscope image of the MXene/zinc oxide/graphene composite material of example 1;
fig. 3 is an electrochemical impedance spectrum of the MXene/zinc oxide/graphene composite material of example 1;
fig. 4 is a cyclic voltammogram of the MXene/zinc oxide/graphene composite of example 1.
Detailed Description
The invention provides a preparation method of an MXene/zinc oxide/graphene composite material, which comprises the following steps:
s1, treating Ti by concentrated hydrochloric acid and lithium fluoride 3 AlC 2 Etching, ultrasonically centrifuging, washing and drying to obtain MXene; the method comprises the specific steps of adding lithium fluoride into concentrated hydrochloric acid solution, stirring until the lithium fluoride is dissolved, and stirringFor 15min, then Ti is added 3 AlC 2 Stirring the powder, heating and stirring for 60h at the reaction temperature of 35 ℃, washing and centrifuging the powder by using water, 2mol/L dilute hydrochloric acid and ethanol after the reaction is finished, washing for at least 10 times until the pH value is neutral, and drying to obtain MXene, wherein Ti is 3 AlC 2 The mass of lithium fluoride and the volume ratio of the concentrated hydrochloric acid solution are 2g:2.5g:40mL.
S2, compounding zinc acetylacetonate and graphene oxide by an in-situ synthesis method to obtain zinc oxide/graphene composite material powder; weighing 0.03g of graphene oxide, adding the graphene oxide into 30mL of deionized water, performing ultrasonic treatment for 2 hours, adding 0.3886g of zinc acetylacetonate into the graphene oxide dispersion liquid, stirring for 15min, transferring the mixed solution into a polytetrafluoroethylene lining after stirring is finished, sealing, placing the polytetrafluoroethylene lining into a high-pressure reaction kettle for hydrothermal reaction at the temperature of 220 ℃ for 12 hours, cooling to room temperature after the reaction is finished, washing with ionized water and absolute ethyl alcohol for 2 times, performing centrifugal drying, and drying at the temperature of 60 ℃ for 24 hours. And obtaining the zinc oxide/graphene composite material.
S3, adding the MXene into 30ml of deionized water, and carrying out ultrasonic treatment for 1min to obtain a solution a, wherein the mass of the added MXene is 0.01-0.1 g;
s4, adding the prepared zinc oxide/graphene powder into the solution a, and stirring for 1min to obtain a solution b, wherein the mass of the added zinc oxide/graphene powder is 0.01-1 g;
and S5, transferring the solution b into a reaction kettle for hydrothermal reaction at 180 ℃ for 12 hours, washing the solution b for 3-5 times by using deionized water, and drying the solution b for 12 hours in a vacuum drying oven at 70 ℃ to obtain the MXene/zinc oxide/graphene composite material.
The prepared MXene/zinc oxide/graphene composite material is used for preparing a super capacitor negative electrode material. The method comprises the following specific steps: mixing MXene/zinc oxide/graphene composite material, conductive carbon black and polyvinylidene fluoride according to the mass ratio of 8:1:1, fully and uniformly mixing, then coating on the foamed nickel, and drying to obtain the super capacitor negative electrode material.
The technical solution of the present invention is further illustrated by the following examples.
Example 1
A preparation method of an MXene/zinc oxide/graphene composite material comprises the following steps:
s1, ti is reacted with concentrated hydrochloric acid and lithium fluoride 3 AlC 2 Etching to obtain MXene; the reaction is carried out by hydrochloric acid and lithium fluoride to Ti 3 AlC 2 The specific steps of etching are as follows: 2.5g of lithium fluoride are weighed into 40mL of concentrated hydrochloric acid solution and stirred for 10min, followed by 2g of Ti 3 AlC 2 And (3) stirring the powder while adding, transferring the powder into an oil bath at the temperature of 30 ℃ after stirring for 15min, heating and stirring for 72h, cooling to room temperature after the reaction is finished, and centrifugally washing at 3500rpm until the pH value is more than 6 to obtain MXene.
S2, adding 0.03g of graphene oxide into 30ml of deionized water, carrying out ultrasonic treatment for 2 hours, weighing 0.3886g of zinc acetylacetonate, adding the zinc acetylacetonate into the graphene oxide dispersion liquid, stirring for 15min, transferring the mixed solution into a polytetrafluoroethylene lining after stirring is finished, sealing, placing the polytetrafluoroethylene lining into a high-pressure reaction kettle, reacting for 12 hours at 220 ℃, cooling to room temperature after the reaction is finished, washing with the deionized water and absolute ethyl alcohol respectively for twice centrifugation, and drying in an oven at 60 ℃ for 24 hours to obtain the zinc oxide/graphene composite material.
And S3, adding 0.03g of MXene into 30ml of deionized water, and carrying out ultrasonic treatment to obtain a solution a.
And S4, adding 0.15g of zinc oxide/graphene powder into the solution a, and stirring to obtain a solution b.
And S5, transferring the solution b into a reaction kettle for hydrothermal reaction at the temperature of 140 ℃ for 12h, washing the solution b for 3 times by using deionized water, and drying the solution b for 12h in a vacuum drying oven at the temperature of 70 ℃ to obtain the MXene/zinc oxide/graphene composite material. And preparing the obtained material into a super capacitor electrode slice for electrochemical performance test.
FIG. 1 is an XRD pattern of a nanocomposite prepared according to the scheme of example 1, with Ti at 8 ℃ in FIG. 1 3 C 2 Is the main characteristic diffraction peak of graphene, the diffraction peak at the position of 26.5 degrees is the main diffraction peak of graphene because of the main diffraction peak of grapheneThe component is carbon. In addition, the diffraction peaks of the (100), (002) and (101) crystal planes of ZnO are respectively at the positions of 31.908 degrees, 34.551 degrees and 36.376 degrees, which shows that the composite material contains three substances and has better composite effect. Scanning electron microscope images of the MXene/zinc oxide/graphene composite prepared in this example are shown in fig. 2. As can be seen from the figure, the MXene/zinc oxide/graphene composite material has a clear and interconnected three-dimensional structure. The three-dimensional pore size of the MXene/zinc oxide/graphene composite material is 10-40nm, the pore wall is formed by crosslinking a graphene nanosheet and an MXene nanosheet, zinc oxide is successfully adsorbed on the surface of the MXene, a small part of zinc oxide is also between the layers of the MXene nanosheets, and the MXene/zinc oxide/graphene composite material, the MXene nanosheets and the MXene nanosheets coexist in a large visual field range. Fig. 3 is an electrochemical impedance spectrum of the MXene/zinc oxide/graphene composite material of example 1. From the numerical ranges of the real part and the imaginary part of the spectrogram and the radius of the circular arc, the resistance of the interface charge transfer of the composite material is smaller than that of most materials. Therefore, the composite material has better conductivity. Fig. 4 is a cyclic voltammogram of the MXene/zinc oxide/graphene composite material of example 1, the transition time of the capacitor is small, and the curve can reach a stable current soon after the external signal is changed, as shown in fig. 4. The lower the transition time, the lower the resistance of the material and the higher the ionic conductivity. Meanwhile, the shape of the CV curve is close to a rectangle, which shows that the performance of the capacitor material is more stable and ideal. Example 2
A preparation method of an MXene/zinc oxide/graphene composite material comprises the following steps:
s1, ti is reacted with concentrated hydrochloric acid and lithium fluoride 3 AlC 2 Etching to obtain MXene; the reaction is carried out by hydrochloric acid and lithium fluoride to Ti 3 AlC 2 The specific steps of etching are as follows: 2.5g of lithium fluoride are weighed into 40mL of concentrated hydrochloric acid solution and stirred for 10min, followed by 2g of Ti 3 AlC 2 And (3) stirring the powder while adding, transferring the powder into an oil bath at the temperature of 30 ℃ after stirring for 15min, heating and stirring for 60h, cooling to room temperature after the reaction is finished, and centrifugally washing at 3500rpm until the pH value is neutral to obtain MXene.
S2, adding 0.03g of graphene oxide into 30ml of deionized water, carrying out ultrasonic treatment for 2 hours, weighing 0.3886g of zinc acetylacetonate, adding the zinc acetylacetonate into the graphene oxide dispersion liquid, stirring for 15min, transferring the mixed solution into a polytetrafluoroethylene lining after stirring is finished, sealing, placing the polytetrafluoroethylene lining into a high-pressure reaction kettle, reacting for 12 hours at 220 ℃, cooling to room temperature after the reaction is finished, washing with the deionized water and absolute ethyl alcohol respectively for twice centrifugation, and drying in an oven at 60 ℃ for 24 hours to obtain the zinc oxide/graphene composite material.
And S3, adding 0.03g of MXene into 30ml of deionized water, and carrying out ultrasonic treatment to obtain a solution a.
And S4, adding 0.09g of zinc oxide/graphene powder into the solution a, and stirring to obtain a solution b.
And S5, transferring the solution b into a reaction kettle for hydrothermal reaction at 180 ℃ for 12 hours, washing the solution b for 3 times by using deionized water, and drying the solution b for 12 hours in a vacuum drying oven at 70 ℃ to obtain the MXene/zinc oxide/graphene composite material. And preparing the obtained material into a super capacitor electrode slice for electrochemical performance test. The measured result shows that the specific capacitance value of the electrode material reaches 1307F/g when the current density is 0.5A/g.
Example 3
A preparation method of an MXene/zinc oxide/graphene composite material comprises the following steps:
s1, ti is reacted with concentrated hydrochloric acid and lithium fluoride 3 AlC 2 Etching to obtain MXene; the reaction is carried out by hydrochloric acid and lithium fluoride to Ti 3 AlC 2 The specific steps of etching are as follows: 2.5g of lithium fluoride are weighed into 40mL of concentrated hydrochloric acid solution and stirred for 10min, followed by 2g of Ti 3 AlC 2 And (3) stirring the powder while adding the powder, transferring the powder into an oil bath at the temperature of 30 ℃ after stirring for 15min, heating and stirring the powder for 60h, cooling the powder to room temperature after the reaction is finished, and centrifugally washing the powder at 3500rpm until the pH value is neutral to obtain MXene.
S2, 0.03g of graphene oxide is taken and added into 30ml of deionized water, ultrasonic treatment is carried out for 2 hours, and then 0.3886g of zinc acetylacetonate (Zn (acac) is weighed 2 ) Adding into graphene oxide dispersion, stirring for 15min, transferring the mixed solution into polytetrafluoroethylene lining after stirring, sealing, and placing under high pressureAnd reacting in a kettle at 220 ℃ for 12h, cooling to room temperature after the reaction is finished, washing twice by using deionized water and absolute ethyl alcohol respectively, centrifuging, and drying in an oven at 60 ℃ for 24 hours to obtain the zinc oxide/graphene composite material.
And S3, adding 0.06g of MXene into 30ml of deionized water, and carrying out ultrasonic treatment to obtain a solution a.
And S4, adding 0.09g of zinc oxide/graphene powder into the solution a, and stirring to obtain a solution b.
And S5, transferring the solution b into a reaction kettle for hydrothermal reaction at 180 ℃ for 12 hours, washing the solution b for 3 times by using deionized water, and drying the solution b for 12 hours in a vacuum drying oven at 70 ℃ to obtain the MXene/zinc oxide/graphene composite material. And preparing the obtained material into a super capacitor electrode slice for electrochemical performance test. The measured result shows that the specific capacitance value of the electrode material reaches 1307F/g when the current density is 0.5A/g.
Therefore, the preparation method of the MXene/zinc oxide/graphene composite material solves the problem that the zinc oxide of the existing super capacitor electrode material is poor in conductive capacity, prevents volume expansion in the charging and discharging processes of a capacitor, improves cycle performance, improves electrochemical performance and stability of the composite material, and is simple in process and low in cost.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.

Claims (10)

1. The preparation method of the MXene/zinc oxide/graphene composite material is characterized by comprising the following steps:
s1, ti is reacted with concentrated hydrochloric acid and lithium fluoride 3 AlC 2 Etching, ultrasonic centrifuging, washing and drying to obtain MXene；
S2, compounding zinc acetylacetonate and graphene oxide by an in-situ synthesis method to obtain zinc oxide/graphene composite material powder;
s3, adding the MXene into 30ml of deionized water, and carrying out ultrasonic treatment to obtain a solution a;
s4, adding the prepared zinc oxide/graphene powder into the solution a, and stirring to obtain a solution b;
and S5, transferring the solution b into a reaction kettle for hydrothermal reaction, cooling, washing and drying to obtain the MXene/zinc oxide/graphene composite material.
2. The method for preparing the MXene/zinc oxide/graphene composite material according to claim 1, wherein the specific steps of the step S1 comprise adding the lithium fluoride into a concentrated hydrochloric acid solution, stirring for 15min to dissolve, and adding Ti to dissolve 3 AlC 2 Stirring the powder, heating and stirring for 60h, wherein the reaction temperature is 35 ℃, washing and centrifuging with water, 2mol/L diluted hydrochloric acid and ethanol after the reaction is finished, washing for at least 10 times until the pH value is neutral, and drying to obtain MXene.
3. The preparation method of the MXene/zinc oxide/graphene composite material according to claim 2, wherein the preparation method comprises the following steps: ti in said step S1 3 AlC 2 The mass of lithium fluoride and the volume ratio of the concentrated hydrochloric acid solution are 2g:2.5g:40mL.
4. The preparation method of the MXene/zinc oxide/graphene composite material according to claim 1, wherein the preparation method comprises the following steps: weighing graphene oxide, adding the graphene oxide into deionized water, performing ultrasonic treatment, adding zinc acetylacetonate into the graphene oxide dispersion liquid, stirring, transferring the mixed solution into a polytetrafluoroethylene lining after stirring, sealing, placing the polytetrafluoroethylene lining into a high-pressure reaction kettle for hydrothermal reaction, cooling to room temperature after the reaction is finished, washing, centrifuging and drying to obtain the zinc oxide/graphene composite material.
5. The preparation method of the MXene/zinc oxide/graphene composite material according to claim 4, wherein the preparation method comprises the following steps: the graphene oxide is 0.03g in mass, the zinc acetylacetonate is 0.3886g in mass, the deionized water is 30mL, the ultrasonic time is 2 hours, the stirring time is 15min, the hydrothermal reaction temperature is 220 ℃, the hydrothermal reaction time is 12 hours, washing is carried out by washing with deionized water and absolute ethyl alcohol for 2 times, and drying is carried out at 60 ℃ for 24 hours.
6. The preparation method of the MXene/zinc oxide/graphene composite material according to claim 1, wherein the preparation method comprises the following steps: in the step S3, the mass of MXene is 0.01-0.1 g, and the ultrasonic time is 1min.
7. The preparation method of the MXene/zinc oxide/graphene composite material according to claim 1, wherein the preparation method comprises the following steps: in the step S4, the mass of the zinc oxide/graphene powder is 0.01-1 g, and the stirring time is 1min.
8. The preparation method of the MXene/zinc oxide/graphene composite material according to claim 1, wherein the preparation method comprises the following steps: the hydrothermal reaction condition in the step S5 is reaction for 12 hours at 180 ℃, the washing is washing for 3-5 times by using deionized water, washing for 3-5 times by using absolute ethyl alcohol, and drying is drying for 12 hours in a vacuum drying oven at 70 ℃.
9. The preparation method of the MXene/zinc oxide/graphene composite material according to any one of claims 1 to 8, wherein: the prepared MXene/zinc oxide/graphene composite material is used for preparing a super capacitor negative electrode material.
10. The method for preparing the MXene/zinc oxide/graphene composite material according to claim 9, wherein the specific steps of preparing the supercapacitor negative electrode material by using the MXene/zinc oxide/graphene composite material are as follows: mixing MXene/zinc oxide/graphene composite material, conductive carbon black and polyvinylidene fluoride according to the mass ratio of 8:1:1, fully and uniformly mixing, then coating on the foamed nickel, and drying to obtain the super capacitor negative electrode material.
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CN110980797B (en) * 2019-12-16 2022-04-05 岭南师范学院 Preparation method of graphene/porous zinc oxide composite film
CN113628893B (en) * 2021-07-16 2022-12-23 哈尔滨工程大学 MXene/graphene/carbon nanotube gel with high multiplying power and long service life, and preparation method and application thereof

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