CN112510187A - Electrostatic self-assembly spherical molybdenum trioxide/MXene composite material and preparation method and application thereof - Google Patents

Electrostatic self-assembly spherical molybdenum trioxide/MXene composite material and preparation method and application thereof Download PDF

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CN112510187A
CN112510187A CN202011368919.8A CN202011368919A CN112510187A CN 112510187 A CN112510187 A CN 112510187A CN 202011368919 A CN202011368919 A CN 202011368919A CN 112510187 A CN112510187 A CN 112510187A
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solid
composite material
molybdenum trioxide
mxene
stirring
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黄流春
唐新村
李星
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Central South University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative 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

Abstract

The invention discloses a static self-assembly spherical molybdenum trioxide/MXene composite material and a preparation method and application thereof, wherein the composite material is prepared by dissolving soluble molybdenum acetylacetonate in ethanol, stirring to obtain a mixed solution, carrying out solvothermal reaction at 150-280 ℃, carrying out furnace cooling, washing and filtering, drying, and calcining at 400-600 ℃ to obtain a solid A; adding the solid A into a poly (diallyldimethylammonium chloride) solution, stirring, and centrifugally washing to obtain a solid B; dripping MXene aqueous solution into the solid B aqueous solution, stirring, standing, centrifuging, washing, and freeze-drying to obtain solid C; and calcining the solid C at 400-600 ℃ under the protection of nitrogen. The composite material is self-assembled on an MXene nanosheet substrate through electrostatic action, the substrate can effectively accommodate the volume effect of molybdenum trioxide in the charging and discharging processes, and the composite material has excellent charging and discharging cycle performance, rate capability and high first coulombic efficiency.

Description

Electrostatic self-assembly spherical molybdenum trioxide/MXene composite material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of lithium ion battery cathode materials, and particularly relates to an electrostatic self-assembly spherical molybdenum trioxide/MXene composite material as well as a preparation method and application thereof.
Background
With the progress of society and the rapid development of economy, the energy problem faced by human is increasingly prominent. Lithium ion batteries are widely used in various electronics, electric tools, and electric vehicles due to their advantages of high energy density, long cycle life, and environmental friendliness. However, the theoretical capacity of the graphite cathode of the traditional lithium ion battery is 372mAh/g, and the requirement of rapidly increasing high energy density is difficult to meet. There is an urgent need to develop a new electrode material to obtain a new lithium ion battery with higher energy density, longer cycle life and fast charge and discharge capability.
Therefore, in order to improve the electrochemical performance and application potential of the lithium ion battery, it is necessary to develop an alternative anode material having a relatively high capacity and high rate while maintaining good cycle stability. Among various alternative anode materials, metal oxides, particularly metal oxides with a nano-scale structure, have the advantages of high theoretical capacity, high rate performance, low price and environmental friendliness, and are expected to become powerful competitors of anode materials in LIBs. Among the various metal oxides, MoO3The lithium ion battery has the advantages of high chemical stability, high theoretical lithium intercalation capacity (about 1117mAh/g, about three times of that of a graphite cathode), environmental friendliness and the like, and is widely concerned by researchers. However, MoO3Formation of Mo and Li during the conversion reaction2At O, bulk MoO3Middle Li+The kinetics of diffusion are poor and the destruction of the structure is caused by the huge volume expansion, thus preventing its practical application. Which on the one hand will affect the contact between the active material and the current collector, hindering the electron transport process; on the other hand, the solid electrolyte interface film is gradually thickened in the circulation process, so that lithium ions are continuously consumed, the internal impedance of the battery is increased, the capacity and the coulombic efficiency are continuously attenuated, and the cycle life is reduced. Therefore, it is necessary to buffer the volume effect generated during the charge and discharge processes thereof, thereby improving the cycle stability thereof as much as possible.
In order to solve the above problems, the method of compounding the metal oxide with a highly conductive nano carbon material (graphene, carbon nanotube, etc.), a porous carbon material, a conductive polymer, etc. is an effective way to improve the electrochemical performance of the metal oxide. The transition metal carbide or nitride, also called MXene, has a graphene-like two-dimensional lamellar structure, and has a great prospect in the application field of lithium ion batteries due to good electronic conductivity, low operating voltage range, low diffusion barrier and special mechanical properties. And MXene sheets can be used as a substrate to be hybridized with metal oxides. In the hybrid reaction, MXene can increase the conductivity and reduce the volume change of the metal oxide, and the metal oxide provides high capacity. Thus, MXene/metal oxide hybridization can achieve high capacity, stable cycling and good rate performance. The existing molybdenum trioxide composite material only carries out simple mechanical coating on the molybdenum trioxide material, and has limited capacity exertion and cycle life improvement. According to the invention, a spherical molybdenum trioxide material is synthesized by a hydrothermal method, and the molybdenum trioxide and MXene are firmly combined together by adopting an electrostatic self-assembly method, so that MXene oxidation can be effectively avoided due to mild reaction conditions, the capacity of a molybdenum trioxide active substance is fully exerted, and meanwhile, the excellent conductivity and nano-layered structure of MXene are utilized, and the volume expansion of molybdenum trioxide in the charge-discharge process is inhibited. Particularly, no patent reports exist at present, and spherical molybdenum trioxide is electrostatically self-assembled on MXene nano-sheets to form a composite material with a 3D structure.
Disclosure of Invention
In order to overcome the defects and shortcomings of the carbon negative electrode material and similar composite materials in the prior art in the application of the high-energy-density lithium ion battery, the invention mainly aims to provide the electrostatic self-assembly spherical molybdenum trioxide/MXene composite material. The composite material has a good three-dimensional flexible structure, can fully exert the capacity of the molybdenum trioxide particles, can effectively contain the volume effect of the molybdenum trioxide particles in the charge and discharge processes, and has good conductivity, excellent multiplying power and cycle performance.
The invention also aims to provide a preparation method of the electrostatic self-assembly spherical molybdenum trioxide/MXene composite material.
Still another object of the present invention is to provide a use of the electrostatic self-assembled spherical molybdenum trioxide/MXene composite material.
The purpose of the invention is realized by the following technical scheme:
a preparation method of an electrostatic self-assembly spherical molybdenum trioxide/MXene composite material comprises the following steps:
(1) dissolving soluble molybdenum acetylacetonate in ethanol, stirring to obtain a mixed solution, carrying out a solvothermal reaction at 150-280 ℃, cooling along with a furnace, washing, filtering, drying, and calcining at 400-600 ℃ to obtain a solid A;
(2) adding the solid A into a poly (diallyldimethylammonium chloride) solution, stirring, and washing to obtain a solid B;
(3) dripping MXene aqueous solution into the solid B aqueous solution, stirring, standing, washing, and freeze-drying to obtain solid C;
(4) and calcining the solid C at 400-600 ℃ under the protection of nitrogen to obtain the spherical molybdenum trioxide/MXene composite material.
To further achieve the object of the present invention, preferably, in step (1), the soluble molybdenum acetylacetonate is analytically pure; the concentration of the acetylacetone molybdenum ethanol solution is 0.01-0.1 mol/L; the solvothermal reaction time is 48 hours; the stirring in the steps (1), (2) and (3) is magnetic stirring.
Preferably, the stirring speed in the step (1) is 100-500 rpm, and the stirring time is 5-60 minutes.
Preferably, the washing in the step (1) is centrifugal washing, the washing speed is 5000 revolutions per minute, and the washing mode is washing with water and ethanol for 3-5 times respectively; the calcining atmosphere is air, and the calcining time is 2-4 h.
Preferably, the mass ratio of the poly (diallyldimethylammonium chloride) to the solid A in the poly (diallyldimethylammonium chloride) solution in the step (2) is (0.05-1): 1.
preferably, the concentration of the MXene aqueous solution in the step (3) is 0.1-1 mg/L, the concentration of the B aqueous solution is 0.1-1 mg/L, and the mass ratio of the MXene to the solid B is (0.1-1): 1.
preferably, the stirring time in the step (3) is 12-24 hours, and the standing time is 24-48 hours.
Preferably, the calcining temperature in the step (4) is 400 ℃, the heating rate is 2 ℃/min, and the calcining time is 2 h.
An electrostatic self-assembly spherical molybdenum trioxide/MXene composite material is prepared by the preparation method.
The electrostatic self-assembly spherical molybdenum trioxide/MXene composite material is used as a negative electrode material of a lithium ion battery.
The method comprises the steps of dissolving soluble molybdenum acetylacetonate in ethanol, and growing molybdenum trioxide nanosheets into spherical structures through simple solvothermal reaction. Then adding the solution into a PDDA solution to coat a layer of PDDA on the surface of the spherical molybdenum trioxide, and carrying out positive charge. And then, placing the MXene solution with negative charge into spherical molybdenum trioxide with positive charge, uniformly dispersing and stirring the MXene solution and the spherical molybdenum trioxide to enable the MXene solution and the spherical molybdenum trioxide to be self-assembled to form a three-dimensional porous structure under the action of static electricity, and finally placing the composite into a high-temperature nitrogen atmosphere for sintering. In the material, MXene nano-sheets and molybdenum trioxide are combined very tightly under the action of static electricity, and meanwhile, ordered interconnected porous structures are formed among the sheets. In the negative electrode material obtained by the technical scheme, the molybdenum trioxide spheres and MXene form a three-dimensional structure through electrostatic self-assembly, and finally a three-dimensional porous structure is obtained.
Compared with the prior art, the invention has the following advantages and effects:
1. the active material molybdenum trioxide in the invention is a spherical structure self-generated by the single crystal nano-sheet, which is beneficial to fully exerting gram capacity and maintaining excellent cycling stability in the charge-discharge cycling process. And in addition, the MXene ball which grows electrostatically supports the MXene layer, so that the layered structure is prevented from collapsing and the MXene layer is prevented from being stacked again, a good flexible structure is kept, the active substance is convenient to contact with the electrolyte better, an effective channel is provided for the transmission of electrons and lithium ions, and the spherical molybdenum trioxide/MXene composite material has good rate performance.
2. According to the invention, the carbonized PDDA layer outside the spherical molybdenum trioxide isolates the spherical molybdenum trioxide from directly contacting with the electrolyte, so that the solid electrolyte interface film is ensured to be on the surface of MXene, and a stable solid electrolyte interface film is formed. The molybdenum trioxide ball has a supporting effect on MXene, so that a good flexible structure can be kept, the volume effect of molybdenum trioxide in the charging and discharging process can be effectively contained, high specific capacity is kept, and the molybdenum trioxide ball has excellent charging and discharging cycle performance and rate capability and high first coulomb efficiency.
Drawings
FIG. 1 is a scanning electron microscope image of the electrostatic self-assembled spherical molybdenum trioxide/MXene composite material prepared in example 2.
FIG. 2 is an X-ray diffraction pattern of the electrostatic self-assembled spherical molybdenum trioxide/MXene composite material prepared in example 2 and molybdenum trioxide and MXene.
FIG. 3 is a graph comparing the cycle performance of the electrostatic self-assembled spherical molybdenum trioxide/MXene composite material prepared in example 2 with that of molybdenum trioxide and MXene.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
All materials in the examples are commercially available.
Example 1
1. 1mmol of MoO2(acac)2Adding the mixture into 50mL of ethanol, and stirring to obtain a solution A;
2. pouring the solution A obtained in the step 1 into a stainless steel reaction kettle, then placing the stainless steel reaction kettle into a forced air drying oven, heating the solution A to 200 ℃, preserving heat for 48 hours, cooling the solution A along with the oven, then carrying out centrifugal washing, and drying the solution A to obtain a solid B;
3. putting the solid B in the step 2 into a rapid heating resistance furnace, heating to 450 ℃ in an air atmosphere, and preserving heat for 3 hours to obtain a solid C;
4. adding 0.1mL of 20 wt.% polydiallyldimethylammonium chloride (PDDA) solution into 200mL of deionized water for dilution, adding 200mg of the solid C obtained in the step 3 into the solution, stirring for a period of time, performing centrifugal washing to obtain a solid D, adding deionized water to a concentration of 1mg/mL, and uniformly stirring to obtain a solution E;
5. weighing an aqueous solution containing 25mg of MXene, adding water to dilute the aqueous solution to 25mL, adding the aqueous solution into 225mL of the solution E obtained in the step 4 under the condition of stirring, fully stirring, standing for 24 hours, centrifuging, washing, and drying in a freeze drying box to obtain a solid F;
6. and (3) putting the solid F obtained in the step (5) into a rapid heating resistance furnace, heating to 400 ℃ under the protection of nitrogen, and keeping the temperature for 2 hours to obtain the electrostatic self-assembly spherical molybdenum trioxide/MXene composite material.
Example 2
1. 1mmol of MoO2(acac)2Adding the mixture into 50mL of ethanol, and stirring to obtain a solution A;
2. pouring the solution A obtained in the step 1 into a stainless steel reaction kettle, then placing the stainless steel reaction kettle into a forced air drying oven, heating the solution A to 200 ℃, preserving heat for 48 hours, cooling the solution A along with the oven, then carrying out centrifugal washing, and drying the solution A to obtain a solid B;
3. putting the solid B in the step 2 into a rapid heating resistance furnace, heating to 450 ℃ in an air atmosphere, and preserving heat for 3 hours to obtain a solid C;
4. adding 0.1mL of 20 wt.% polydiallyldimethylammonium chloride (PDDA) solution into 200mL of deionized water for dilution, adding 200mg of the solid C obtained in the step 3 into the solution, stirring for a period of time, performing centrifugal washing to obtain a solid D, adding deionized water until the concentration is 1mg/mL, and uniformly stirring to obtain a solution E;
5. weighing an aqueous solution containing 50mg of MXene, adding water to dilute the aqueous solution to 50mL, adding the aqueous solution into 200mL of the solution E obtained in the step 4 under the condition of stirring, fully stirring, standing for 24 hours, centrifuging, washing, and drying in a freeze drying box to obtain a solid F;
6. and (3) putting the solid F obtained in the step (5) into a rapid heating resistance furnace, heating to 400 ℃ under the protection of nitrogen, and keeping the temperature for 2 hours to obtain the electrostatic self-assembly spherical molybdenum trioxide/MXene composite material.
Example 3
1. Will be provided with1mmol MoO2(acac)2Adding the mixture into 50mL of ethanol, and stirring to obtain a solution A;
2. pouring the solution A obtained in the step 1 into a stainless steel reaction kettle, then placing the stainless steel reaction kettle into a forced air drying oven, heating the solution A to 200 ℃, preserving heat for 48 hours, cooling the solution A along with the oven, then carrying out centrifugal washing, and drying the solution A to obtain a solid B;
3. putting the solid B in the step 2 into a rapid heating resistance furnace, heating to 450 ℃ in an air atmosphere, and preserving heat for 3 hours to obtain a solid C;
4. adding 0.1mL of 20 wt.% polydiallyldimethylammonium chloride (PDDA) solution into 200mL of deionized water for dilution, adding 200mg of the solid C obtained in the step 3 into the solution, stirring for a period of time, performing centrifugal washing to obtain a solid D, adding deionized water until the concentration is 1mg/mL, and uniformly stirring to obtain a solution E;
5. weighing an aqueous solution containing 125mg of MXene, adding water to dilute the aqueous solution to 125mL, adding the aqueous solution into 125mL of the solution E obtained in the step 4 under the condition of stirring, fully stirring, standing for 24 hours, centrifuging, washing, and drying in a freeze drying box to obtain a solid F;
6. and (3) putting the solid F obtained in the step (5) into a rapid heating resistance furnace, heating to 400 ℃ under the protection of nitrogen, and keeping the temperature for 2 hours to obtain the electrostatic self-assembly spherical molybdenum trioxide/MXene composite material.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. An electrostatic self-assembly spherical molybdenum trioxide/MXene composite material and a preparation method and application thereof are characterized by comprising the following steps:
(1) dissolving soluble molybdenum acetylacetonate in ethanol, stirring to obtain a mixed solution, carrying out a solvothermal reaction at 150-280 ℃, cooling along with a furnace, washing, filtering, drying, and calcining at 400-600 ℃ to obtain a solid A;
(2) adding the solid A into a poly (diallyldimethylammonium chloride) solution, stirring, and washing to obtain a solid B;
(3) dripping MXene aqueous solution into the solid B aqueous solution, stirring, standing, washing, and freeze-drying to obtain solid C;
(4) and calcining the solid C at 400-600 ℃ under the protection of nitrogen to obtain the spherical molybdenum trioxide/MXene composite material.
2. The electrostatic self-assembled spherical molybdenum trioxide/MXene composite of claim 1, wherein the soluble molybdenum acetylacetonate of step (1) is analytically pure; the concentration of the acetylacetone molybdenum ethanol solution is 0.01-0.1 mol/L; the solvothermal reaction time is 48 hours; the stirring in the steps (1), (2) and (3) is magnetic stirring.
3. The electrostatic self-assembly spherical molybdenum trioxide/MXene composite material according to claim 1, wherein the stirring speed in step (1) is 100-500 rpm, and the stirring time is 5-60 minutes.
4. The electrostatic self-assembly spherical molybdenum trioxide/MXene composite material according to claim 1, wherein the washing in step (1) is centrifugal washing, the washing speed is 5000 r/min, and the washing mode is 3-5 times washing with water and ethanol respectively; the calcining atmosphere is air, and the calcining time is 2-4 h.
5. The electrostatic self-assembly spherical molybdenum trioxide/MXene composite material according to claim 1, wherein the mass ratio of poly (diallyldimethylammonium chloride) to solid A in the poly (diallyldimethylammonium chloride) solution in step (2) is (0.05-1): 1.
6. the electrostatic self-assembly spherical molybdenum trioxide/MXene composite material according to claim 1, wherein the concentration of MXene aqueous solution in step (3) is 0.1-1 mg/L, the concentration of B aqueous solution is 0.1-1 mg/L, and the mass ratio of MXene to solid B is (0.1-1): 1.
7. the electrostatic self-assembly spherical molybdenum trioxide/MXene composite material according to claim 1, wherein the stirring time in step (3) is 12-24 hours, and the standing time is 24-48 hours.
8. The electrostatic self-assembled spherical molybdenum trioxide/MXene composite material according to claim 6, wherein the calcination temperature in step (4) is 400 ℃, the heating rate is 2 ℃/min, and the calcination time is 2 h.
9. The electrostatic self-assembly spherical molybdenum trioxide/MXene composite material prepared by the preparation method according to any one of claims 1 to 8.
10. The electrostatic self-assembled spherical molybdenum trioxide/MXene composite material as claimed in claim 9 is used as negative electrode material of lithium ion battery.
CN202011368919.8A 2020-11-30 2020-11-30 Electrostatic self-assembly spherical molybdenum trioxide/MXene composite material and preparation method and application thereof Pending CN112510187A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115259874A (en) * 2021-04-29 2022-11-01 中国科学院福建物质结构研究所 Toughened and conductive MXene-zirconia composite ceramic and preparation method thereof
CN115799459A (en) * 2023-02-06 2023-03-14 昆山美淼新材料科技有限公司 Production process of graphene modified metal electrode

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115259874A (en) * 2021-04-29 2022-11-01 中国科学院福建物质结构研究所 Toughened and conductive MXene-zirconia composite ceramic and preparation method thereof
CN115259874B (en) * 2021-04-29 2023-11-17 中国科学院福建物质结构研究所 Toughened and conductive MXene-zirconia composite ceramic and preparation method thereof
CN115799459A (en) * 2023-02-06 2023-03-14 昆山美淼新材料科技有限公司 Production process of graphene modified metal electrode

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