CN111943208A - Method for preparing titanium carbide (MXene) flexible electrode based on high-temperature carbonization of polymer and application of method - Google Patents
Method for preparing titanium carbide (MXene) flexible electrode based on high-temperature carbonization of polymer and application of method Download PDFInfo
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Abstract
The invention belongs to the technical field of nano composite material preparation, and particularly relates to a method for preparing a titanium carbide (MXene) flexible electrode based on high-temperature carbonization of a polymer and application thereof, which aims to further improve Ti content3C2TxMethod for electrochemical performance of titanium carbide, the invention uses Ti3C2TxAs a substrate, taking polymer polyacrylonitrile and/or benzoquinone-phenylenediamine mixture as a filler, and preparing Ti by high-temperature carbonization treatment3C2Tx(MXene) Flexible electrode, Ti prepared by the method of the invention3C2Tx(MXene) Flexible electrode MembraneHas better flexibility, can be bent and folded, has excellent electrochemical performance, and the area specific capacitance can reach 239mF cm‑2(ii) a In addition, the invention firstly carries out vacuum filtration and then high-temperature carbonization treatment, and directly forms, has simple and easy operation, does not need any binder, and reduces the production cost and the process complexity.
Description
Technical Field
The invention belongs to the technical field of nano composite material preparation, and particularly relates to a method for preparing a titanium carbide (MXene) flexible electrode based on high-temperature carbonization of a polymer and application thereof.
Background
In recent years, as electronic products are miniaturized, and portable, flexible functions have become a trend. In the aspect of energy storage, a super capacitor has been a hot spot of current research due to its advantages of long service life, large charge-discharge current density, and the like. The electrode, the electrode lug, the diaphragm and the packaging material are indispensable components for forming the supercapacitor, wherein the electrode is one of key components and is an extremely important part in the whole system. Therefore, the research on the electrode having high electrochemical performance and certain flexibility and safety is the focus of the current research work.
Polymers, which have a certain flexibility due to their long chain-like microstructures, are often used in flexible devices, making them widely used. However, the electrochemical performance is poor, and even if some materials have certain electrochemical performance, the structure is unstable in the charging and discharging process, the cycle life is short, and the like.
Two-dimensional materials (e.g. graphene, MoS)2Black phosphenes, MXenes, etc.), which have a lamellar morphology, are used in flexible devices in many applications. Among them, MXenes, a novel two-dimensional material, is generally obtained by selectively etching away an element a (generally, Si or Al) in the MAX phase, and has the advantages of good electron conductivity, strong hydrophilicity, large specific surface area, and abundant surface active functional groups, and thus has been a hot point of recent research. Ti3C2Tx(titanium carbide, T)xRepresenting surface termination functional groups such as-F, -O, -OH, etc.) is one of the most widely studied MXenes materials, and shows great appeal in the application of flexible device electrode materials. However, since some agglomeration occurs during the preparation process, when the polymer is used as an active material of a supercapacitor, the electrochemical performance is limited, thereby affecting the practical application. Therefore, further improvement of Ti was investigated3C2TxThe method of electrochemical performance is of great significance.
Disclosure of Invention
In order to overcome the disadvantages of the prior art, the invention provides a method for preparing Ti based on high-temperature carbonization of polymer3C2Tx(MXene) method of flexible electrode.
It is a second object of the present invention to provide Ti prepared by the above method3C2Tx(MXene) Flexible electrode.
The third object of the present invention is to provide Ti prepared by the above method3C2TxApplication of (MXene) flexible electrode in preparing flexible device.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a method for preparing Ti based on high-temperature carbonization of polymer3C2Tx(MXene) Flexible electrode method, i.e. with Ti3C2TxTi is prepared by taking polymer Polyacrylonitrile (PAN) and/or benzoquinone-phenylenediamine mixture as a filler through high-temperature carbonization treatment as a substrate3C2Tx(MXene) Flexible electrode.
In consideration of the electrical property and functional application of the flexible device, the invention adopts a mode of making up for the weakness by Ti3C2Tx(titanium carbide) as a substrate, providing electrochemically active sites; the polymer (polyacrylonitrile and/or benzoquinone-phenylenediamine mixture) is used as a filler, reduces the agglomeration of active substances and provides flexibility; in addition, as some polymers are not conductive, the conductivity of the polymers is increased by adopting a high-temperature carbonization mode, so that the Ti is further improved3C2TxAnd (4) exerting electrochemical performance.
Preferably, one of the above mentioned is based on the preparation of Ti by high temperature carbonization of a polymer3C2TxThe method for the (MXene) flexible electrode specifically comprises the following steps:
s1 preparation of Ti3C2TxA suspension;
s2, preparing a polymer solution: polyacrylonitrile solution and/or benzoquinone-phenylenediamine mixture solution;
s3, dissolvingLiquid mixing: mixing Ti of step S13C2TxMixing the suspension with the polymer solution of step S2;
s4, assembling the membrane: carrying out suction filtration and drying on the mixed solution obtained in the step S3 to obtain an electrode diaphragm prefabricated sample;
s5, high-temperature carbonization: carrying out high-temperature carbonization treatment on the membrane prefabricated sample obtained in the step S4 to obtain Ti3C2Tx(MXene) Flexible electrode.
Preferably, Ti described in step S13C2TxThe suspension is prepared by LiF + HCl (aqueous HCl solution of LiF) and Ti3AlC2Prepared by reaction under certain conditions.
Specifically, the Ti3C2TxThe preparation method of the suspension comprises the following steps: LiF is gradually added into HCl aqueous solution (the concentration is 6 mol. L)-1) Completely dissolving the mixture to prepare a mixed solution with the concentration of (0.05-0.08) g/mL; gradually adding Ti to the above mixed solution3AlC2(Ti3AlC2The mass ratio of the mixed solution to LiF is 1-3:1), stirring for 10-60min at room temperature to ensure that the mixed solution is uniform; transferring the mixed solution to the reaction temperature of 35-40 ℃ for reaction for 24-45 h; after the reaction is finished, centrifuging and washing at the rotation speed of 3500-; then, ultrasonically dispersing for 1h in an inert gas (such as argon and nitrogen) atmosphere, wherein the ultrasonic power is 80W; then centrifuging at 3500prm for 1h, and collecting the supernatant to obtain Ti3C2TxAnd (3) suspension.
Preferably, the benzoquinone-phenylenediamine mixture in step S2 is obtained by mixing benzoquinone and phenylenediamine in a molar ratio of (2-3) to 1, and more preferably, the molar ratio of benzoquinone to phenylenediamine is 3:1 or 2: 1.
Preferably, the high temperature carbonization in step S5 is performed at 5-10 deg.C/min under inert gas (such as argon and nitrogen) atmosphere-1The temperature rise rate is raised to 750 ℃ and 950 DEG CKeeping the temperature for 0.5-4 h.
Preferably, Ti is used in step S33C2TxThe suspension and the polymer solution are mixed according to the following formula (1-2): (1-2), more preferably, the Ti is mixed3C2TxThe mass ratio of the suspension to the polymer solution was 2:1, 1: 2.
Preferably, the mass concentration of the polyacrylonitrile solution in the step S2 is 1% to 8%.
Specifically, polyacrylonitrile is dispersed in dimethyl formamide (DMF) to prepare a polyacrylonitrile solution.
Preferably, the mass concentration of the benzoquinone-phenylenediamine mixture solution in step S2 is 0.5% to 1%.
Specifically, the benzoquinone-phenylenediamine mixture is dispersed into absolute ethyl alcohol and is stirred uniformly to prepare a benzoquinone-phenylenediamine mixture solution.
Preferably, the suction filtration in the step S4 is vacuum filtration with a filter membrane with a pore size of 0.2-0.45 μm; the drying is vacuum freeze drying.
Preferably, Ti is used in step S33C2TxAnd after the suspension is mixed with the polymer solution, stirring at room temperature for not less than 24 hours to fully mix the suspension and the polymer solution.
The invention also provides Ti prepared by the method3C2Tx(MXene) Flexible electrode.
The invention also provides Ti prepared by the method3C2TxApplication of (MXene) flexible electrode in preparing flexible device.
Preferably, the flexible device includes, but is not limited to, a flexible capacitor including, but not limited to, a flexible supercapacitor.
Ti prepared by the method of the invention3C2TxThe (MXene) flexible electrode has better flexibility and can be bent and folded; the electrochemical performance is excellent, and the area specific capacitance can reach 239mF cm-2And is expected to be used as a novel electrode material of a flexible device.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a method for preparing Ti based on high-temperature carbonization of polymer3C2Tx(MXene) Flexible electrode method, i.e. with Ti3C2TxTi is prepared by taking polymer Polyacrylonitrile (PAN) and/or benzoquinone-phenylenediamine mixture as a filler through high-temperature carbonization treatment as a substrate3C2Tx(MXene) Flexible electrode, Ti prepared by the method of the invention3C2TxThe (MXene) flexible electrode diaphragm not only has better flexibility, can be bent and folded, but also has excellent electrochemical performance, and the area specific capacitance can reach 239mF cm-2(ii) a In addition, the invention firstly carries out vacuum filtration and then high-temperature carbonization treatment, and directly forms, the operation is simple and easy, and the prepared electrode does not need any binder, thereby reducing the production cost and the process complexity.
Drawings
FIG. 1 is a diagram of Ti production based on high temperature carbonization of polymers3C2Tx(MXene) Process flow schematic of Flexible electrode;
FIG. 2 shows Ti prepared based on high temperature carbonization of polymer3C2Tx(MXene) photograph of flexible electrode in bent state;
FIG. 3 shows Ti prepared based on high-temperature carbonization of polymer in example 13C2Tx(MXene) electrochemical performance profile of flexible electrode;
FIG. 4 shows Ti prepared based on high temperature carbonization of polymer in example 43C2Tx(MXene) electrochemical performance curves for flexible electrodes.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
EXAMPLE 1 preparation of Ti based on Polymer high temperature carbonization3C2TxMethod for (MXene) flexible electrode
As shown in fig. 1, the method comprises the following process steps:
(1)Ti3C2Txpreparation of the suspension: 1.98g of LiF were gradually added to a 30ml of aqueous solution of LHCl (concentration 6mol L)-1) Completely dissolving the mixture to prepare a mixed solution with the concentration of 0.066 g/mL; to the mixture was gradually added 3g of Ti3AlC2Stirring for 60min at room temperature by using a magnetic stirrer, and uniformly stirring; transferring the mixed solution into a hydrothermal kettle made of Teflon materials, wherein the reaction temperature is 40 ℃, and the reaction time is 45 hours; after the reaction is finished, centrifuging and washing at the rotation speed of 3500prm for 5min each time, repeating the centrifuging for 8 times totally until the pH value is about 6, and washing the reaction product by using absolute ethyl alcohol and deionized water as washing reagents (the reaction product is washed by using the absolute ethyl alcohol and the deionized water alternately); then, ultrasonically dispersing for 1h in an argon atmosphere; then, the mixture was centrifuged at 3500prm for 1 hour, and the supernatant was collected and kept for further use.
(2) Preparation of polymer solution: polyacrylonitrile (PAN) is dispersed in dimethyl formamide (DMF) and stirred to form a uniform solution, with the mass concentration of PAN being 8%.
(3) Solution mixing: mixing Ti in the step (1)3C2TxSuspension and polymer solution in step (2) the ratio of 2:1, and stirring at room temperature for 24 hours.
(4) Assembling the membrane: and (4) carrying out vacuum filtration on the mixed solution in the step (3) by using a filter membrane (the aperture is 0.45 mu m), and then carrying out vacuum freeze drying to obtain an electrode membrane prefabricated sample.
(5) Carbonizing treatment: placing the film sheet prefabricated sample obtained in the step (4) in an argon atmosphere, and keeping the temperature for 5 ℃ min-1The temperature rising rate is increased to 750 ℃, the temperature is preserved for 4 hours for carbonization treatment, and finally the temperature is cooled to room temperature to obtain Ti prepared based on high-temperature carbonization of polymer3C2Tx(MXene) Flexible electrode.
Prepared Ti3C2Tx(MXene) flexible electrode has better flexibility, can be bent and folded, and the bent state is shown in fig. 2.
Example 2 preparation of Ti based on Polymer high temperature carbonization3C2TxMethod for (MXene) flexible electrode
As shown in fig. 1, the method comprises the following process steps:
(1)Ti3C2Txpreparation of the suspension: 1.98g of LiF were gradually added to a 30ml of aqueous solution of LHCl (concentration 6mol L)-1) Completely dissolving the mixture to prepare a mixed solution with the concentration of 0.066 g/mL; to the mixture was gradually added 3g of Ti3AlC2Stirring for 60min at room temperature by using a magnetic stirrer, and uniformly stirring; transferring the mixed solution into a hydrothermal kettle made of Teflon materials, wherein the reaction temperature is 35 ℃, and the reaction time is 24 hours; after the reaction is finished, centrifuging and washing at the rotating speed of 5000prm for 10min each time, repeating the centrifuging for 8 times totally until the pH value is about 6, and using washing reagents of absolute ethyl alcohol and deionized water (the reaction product is washed by alternately using the absolute ethyl alcohol and the deionized water); then, ultrasonically dispersing for 1h in an argon atmosphere; then, the mixture was centrifuged at 3500prm for 1 hour, and the supernatant was collected and kept for further use.
(2) Preparation of polymer solution: polyacrylonitrile (PAN) is dispersed in dimethyl formamide (DMF) and stirred to form a uniform solution, with the mass concentration of PAN being 8%.
(3) Solution mixing: mixing Ti in the step (1)3C2TxThe suspension and the polymer solution in step (2) were mixed in a ratio of 1:1, and stirring at room temperature for 24 hours.
(4) Assembling the membrane: and (4) carrying out vacuum filtration on the mixed solution in the step (3) by using a filter membrane (the aperture is 0.45 mu m), and then carrying out vacuum freeze drying to obtain an electrode membrane prefabricated sample.
(5) Carbonizing treatment: placing the film sheet prefabricated sample obtained in the step (4) in an argon atmosphere, and keeping the temperature for 10 ℃ min-1The temperature is raised to 850 ℃ at the temperature raising rate, the temperature is kept for 2h for carbonization treatment, and finally the temperature is cooled to room temperature to obtain Ti prepared based on high-temperature carbonization of polymer3C2Tx(MXene) flexibilityAnd an electrode.
Prepared Ti3C2TxThe (MXene) flexible electrode has better flexibility, and can be bent and folded.
EXAMPLE 3 preparation of Ti based on Polymer high temperature carbonization3C2TxMethod for (MXene) flexible electrode
As shown in fig. 1, the method comprises the following process steps:
(1)Ti3C2Txpreparation of the suspension: 1.98g of LiF were gradually added to a 30ml of aqueous solution of LHCl (concentration 6mol L)-1) Completely dissolving the mixture to prepare a mixed solution with the concentration of 0.066 g/mL; to the mixture was gradually added 3g of Ti3AlC2Stirring for 60min at room temperature by using a magnetic stirrer, and uniformly stirring; transferring the mixed solution into a hydrothermal kettle made of Teflon material, wherein the reaction temperature is 35 ℃, and the reaction time is 40 h; after the reaction is finished, centrifuging and washing at the rotation speed of 3500prm for 10min each time, repeating centrifuging for 6 times totally until the pH is about 6, wherein the used washing reagents are absolute ethyl alcohol and deionized water (the absolute ethyl alcohol and the deionized water are alternately used for washing the reaction product); then, ultrasonically dispersing for 1h in an argon atmosphere; then, the mixture was centrifuged at 3500prm for 1 hour, and the supernatant was collected and kept for further use.
(2) Preparation of polymer solution: polyacrylonitrile (PAN) is dispersed in dimethyl formamide (DMF) and stirred to form a uniform solution, with the mass concentration of PAN being 8%.
(3) Solution mixing: mixing Ti in the step (1)3C2TxThe suspension and the polymer solution in step (2) were mixed in a ratio of 1:2, and stirring at room temperature for 24 hours.
(4) Assembling the membrane: and (4) carrying out vacuum filtration on the mixed solution in the step (3) by using a filter membrane (the aperture is 0.22 mu m), and then carrying out vacuum freeze drying to obtain an electrode membrane prefabricated sample.
(5) Carbonizing treatment: placing the film sheet prefabricated sample obtained in the step (4) in an argon atmosphere, and keeping the temperature for 10 ℃ min-1The temperature rising rate is increased to 950 ℃, the temperature is preserved for 0.5h for carbonization treatment, and finally the temperature is cooled to room temperature to obtain the polymer-based high temperatureTi prepared by carbonization3C2Tx(MXene) Flexible electrode.
Prepared Ti3C2TxThe (MXene) flexible electrode has better flexibility, and can be bent and folded.
EXAMPLE 4 preparation of Ti based on Polymer high temperature carbonization3C2TxMethod for (MXene) flexible electrode
As shown in fig. 1, the method comprises the following process steps:
(1)Ti3C2Txpreparation of the suspension: 1.98g of LiF were gradually added to a 30ml of aqueous solution of LHCl (concentration 6mol L)-1) Completely dissolving the mixture to prepare a mixed solution with the concentration of 0.066 g/mL; to the mixture was gradually added 3g of Ti3AlC2Stirring for 60min at room temperature by using a magnetic stirrer, and uniformly stirring; transferring the mixed solution into a hydrothermal kettle made of Teflon materials, wherein the reaction temperature is 40 ℃, and the reaction time is 45 hours; after the reaction is finished, centrifuging and washing at the rotation speed of 3500prm for 5min each time, repeating the centrifuging for 8 times totally until the pH value is about 6, and washing the reaction product by using absolute ethyl alcohol and deionized water as washing reagents (the reaction product is washed by using the absolute ethyl alcohol and the deionized water alternately); then, ultrasonically dispersing for 1h in an argon atmosphere; then, the mixture was centrifuged at 3500prm for 1 hour, and the supernatant was collected and kept for further use.
(2) Preparation of polymer solution: benzoquinone and phenylenediamine were mixed in a ratio of 3:1, then dispersed in absolute ethanol at a mass concentration of 1% of the benzoquinone-phenylenediamine mixture, and stirred until the solution turns dark brown.
(3) Solution mixing: mixing Ti in the step (1)3C2TxSuspension and polymer solution in step (2) the ratio of 2:1, and stirring at room temperature for 24 hours.
(4) Assembling the membrane: and (4) carrying out vacuum filtration on the mixed solution in the step (3) by using a filter membrane (the aperture is 0.45 mu m), and then carrying out vacuum freeze drying to obtain an electrode membrane prefabricated sample.
(5) Carbonizing treatment: placing the film sheet prefabricated sample obtained in the step (4) in an argon atmosphere at 5 ℃ min-1The temperature rising rate is increased to 750 ℃, the temperature is preserved for 4 hours for carbonization treatment, and finally the temperature is cooled to room temperature to obtain Ti prepared based on high-temperature carbonization of polymer3C2Tx(MXene) Flexible electrode.
Prepared Ti3C2TxThe (MXene) flexible electrode has better flexibility, and can be bent and folded.
Experimental example 1 electrochemical Performance test
Measurement of area specific capacitance: respectively using Ti after high-temperature carbonization in example 1 and example 43C2Tx(MXene) flexible electrode diaphragm as working electrode, activated carbon electrode as counter electrode, Ag/AgCl electrode (3mol L)-1KCl solution) as a reference electrode; with 1mol L-1H of (A) to (B)2SO4Is an electrolyte and is assembled into a three-electrode testing device. And then performing electrochemical test in an electrochemical workstation by adopting a scanning cyclic voltammetry method, wherein the scanning rate of the test is 2-100mV/s, the number of scanning circles is 5, and the capacitance is used for taking the data of the fifth circle. Finally, the scanning rate (mV/s) is taken as an abscissa, and the area ratio capacitance (mF cm) is taken-2) The electrochemical performance curve is plotted as the ordinate. The results are shown in FIGS. 3 and 4.
The preparation method of the active carbon counter electrode comprises the following steps: mixing the activated carbon and PTFE emulsion according to the weight ratio of 90: 10, adding water to prepare a pasty mixture (the solid content is about 40 percent), and rolling to form a sheet with the thickness of about 0.1 mm; and finally, placing the mixture in a vacuum oven at 100 ℃ for 4h, cooling to room temperature, and storing in a drying oven to be used as a counter electrode for later use.
Currently, in the field of flexible electrodes, carbon flexible electrodes have good electrochemical performance and wide application, and the area specific capacitance of the carbon flexible electrodes is 57-85 mF-cm-2. As can be seen from the electrochemical performance curve of FIG. 3, the voltage at 10mV · s-1Ti of example 13C2TxThe area specific capacitance of the (MXene) flexible electrode is as high as 239mF cm-2. As can be seen from the electrochemical performance curve of FIG. 4, the voltage at 10mV · s-1Ti of example 43C2Tx(MXene) Flexible electrodeHas an area specific capacitance of 201mF cm-2. Thus, the Ti prepared by the method of the invention3C2TxThe (MXene) flexible electrode has more excellent electrochemical performance and is expected to become a novel flexible electrode material.
In addition, Ti obtained in example 2 and example 33C2TxThe area specific capacitance of the (MXene) flexible electrode is not much different from that of example 2.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (10)
1. Preparation of Ti based on high-temperature carbonization of polymer3C2Tx(MXene) Flexible electrode Process, characterized in that Ti is used3C2TxAs a substrate, taking polymer polyacrylonitrile and/or benzoquinone-phenylenediamine mixture as a filler, and preparing Ti by high-temperature carbonization treatment3C2Tx(MXene) Flexible electrode.
2. The method for preparing Ti based on high-temperature carbonization of polymer according to claim 13C2TxA method of (MXene) flexible electrodes, comprising the steps of:
s1 preparation of Ti3C2TxA suspension;
s2, preparing a polymer solution: polyacrylonitrile solution and/or benzoquinone-phenylenediamine mixture solution;
s3, mixing the solution: mixing Ti of step S13C2TxMixing the suspension with the polymer solution of step S2;
s4, assembling the membrane: carrying out suction filtration and drying on the mixed solution obtained in the step S3 to obtain an electrode diaphragm prefabricated sample;
s5, high-temperature carbonization:carrying out high-temperature carbonization treatment on the membrane prefabricated sample obtained in the step S4 to obtain Ti3C2Tx(MXene) Flexible electrode.
3. The method for preparing Ti based on high-temperature carbonization of polymer according to claim 23C2Tx(MXene) Flexible electrode production method, characterized in that Ti in step S13C2TxThe suspension is prepared by LiF + HCl and Ti3AlC2Prepared by reaction under certain conditions.
4. The method for preparing Ti based on high-temperature carbonization of polymer according to claim 23C2TxThe method for manufacturing the (MXene) flexible electrode is characterized in that the benzoquinone-phenylenediamine mixture obtained in the step S2 is obtained by mixing benzoquinone and phenylenediamine according to a molar ratio of (2-3) to 1.
5. The method for preparing Ti based on high-temperature carbonization of polymer according to claim 23C2Tx(MXene) Flexible electrode Process, characterized in that the high temperature carbonization in step S5 is carried out at 5-10 ℃ min under inert gas atmosphere-1The temperature rise rate is increased to 750 ℃ and 950 ℃, and the temperature is kept for 0.5 to 4 hours.
6. The method for preparing Ti based on high-temperature carbonization of polymer according to claim 23C2Tx(MXene) Flexible electrode method, characterized in that, step S3 said Ti3C2TxThe suspension and the polymer solution are mixed according to the following formula (1-2): (1-2) in the above-mentioned mass ratio.
7. The method for preparing Ti based on high-temperature carbonization of polymer according to claim 23C2TxThe method for preparing the (MXene) flexible electrode is characterized in that the mass concentration of the polyacrylonitrile solution in the step S2 is 1% -8%.
8. A polymer-based polymer according to claim 2Preparation of Ti by high-temperature carbonization of compound3C2TxThe method for manufacturing the (MXene) flexible electrode is characterized in that the mass concentration of the benzoquinone-phenylenediamine mixture solution in the step S2 is 0.5% -1%.
9. Ti obtainable by a process according to any one of claims 1 to 83C2Tx(MXene) Flexible electrode.
10. The Ti of claim 93C2TxApplication of (MXene) flexible electrode in preparing flexible device.
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| CN113005567A (en) * | 2021-02-25 | 2021-06-22 | 同济大学 | Preparation and application of novel MXene modified porous carbon fiber composite electrode |
| CN113115581A (en) * | 2021-04-13 | 2021-07-13 | 郑州大学 | Ti3C2Tx composite and preparation method thereof |
| CN113163698A (en) * | 2021-04-23 | 2021-07-23 | 郑州大学 | Honeycomb composite material and preparation method thereof |
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