CN108987126B - Ti3C2/Ni composite electrode material and preparation method thereof - Google Patents
Ti3C2/Ni composite electrode material and preparation method thereof Download PDFInfo
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- CN108987126B CN108987126B CN201811134889.7A CN201811134889A CN108987126B CN 108987126 B CN108987126 B CN 108987126B CN 201811134889 A CN201811134889 A CN 201811134889A CN 108987126 B CN108987126 B CN 108987126B
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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
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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
- H01G11/24—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
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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
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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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention belongs to the technical field of materials, and discloses Ti3C2a/Ni composite electrode material and a preparation method thereof. Mixing Ti3AlC2Obtaining Ti with a two-dimensional structure by etching with hydrofluoric acid3C2(ii) a Ti of two-dimensional structure3C2Obtaining Ti with negative charges on the surface by dimethyl sulfoxide intercalation and ultrasonic stripping3C2nanosheets; by reacting a cationic surfactant with Ti3C2Nano-sheet positive and negative charge electrostatic self-assembly method for Ti3C2The nano sheet is loaded on the surface of the foamed nickel to obtain Ti3C2the/Ni composite electrode material. The preparation process is quick and simple, the cost is low, the composite electrode material has excellent electrochemical performance, can be used as an electrode material of a super capacitor, and is Ti3C2The compound of the nanosheets and other metal foams provides a certain theoretical research foundation in the research of electrode materials of the supercapacitor.
Description
Technical Field
The invention belongs to the technical field of materials and discloses Ti3C2a/Ni composite electrode material and a preparation method thereof.
Background
Along with the transient exploitation of non-renewable energy sources such as coal and fossil fuel and serious environmental pollution, the development of green energy sources and the sustainable development thereof are receiving increasing attention, and the research and development of an energy storage and conversion system with high efficiency, environmental protection and low cost is urgent. The super capacitor is a high-efficiency energy storage device, and has attracted extensive attention due to its characteristics of high power density, fast charge and discharge rate, long cycle life, environmental friendliness and the like. At present, the super capacitor is successfully applied to the fields of portable consumer electronic products and the like, and has wide market development prospect.
Supercapacitors can be classified into double layer capacitors and pseudocapacitors according to different energy storage mechanisms. The double electric layer capacitor is charged and discharged at the interface of electrode/solution through the charge confrontation caused by the directional arrangement of electrons or ions; the pseudocapacitor is charged and discharged through highly reversible chemical adsorption and desorption and oxidation reduction reactions of electroactive substances. The electrode material of the pseudo capacitor is usually transition metal oxide, hydroxide, etc. and polymer, but its application is limited due to the defects of poor conductivity and stability. Therefore, the development of a novel supercapacitor electrode material with excellent electrochemical performance becomes a key problem. Ti investigated herein3C2the/Ni composite material is applied to the super capacitor as the anode material for the first time, and provides a new research direction for the development of preparing novel super capacitor electrode materials.
Disclosure of Invention
the invention aims to disclose a Ti3C2a/Ni composite electrode material and a preparation method thereof. Based on Ti3C2The nanosheet has the characteristics of excellent conductivity, negative potential, large amount of oxygen-containing functional groups on the surface and the like, and Ti is prepared by a positive and negative charge electrostatic self-assembly method3C2Nano sheets are loaded on the surface of foamed nickel with a three-dimensional porous structure and high conductivity, and Ti passes through3C2The contact between the nano sheet and the foamed nickel fully exerts the advantages of the nano sheet and the foamed nickel, and the good electrochemical performance is shown.
The technical scheme of the invention is as follows:
Ti3C2the/Ni composite electrode material is fully combined with Ti3C2The advantages of nanosheets and nickel foam, based on two-dimensional Ti3C2The nano-sheet has high conductivity (1-3 multiplied by 10)6S/m), hydrophilicity, surface negative charge and the characteristic of having a large number of oxygen-containing functional groups, the foam nickel has the characteristics of high specific surface area, high conductivity, low density, three-dimensional porous structure and the like, the foam nickel is used as a substrate, the cationic surfactant is used as a bridging agent, and Ti is subjected to positive and negative charge electrostatic self-assembly3C2The nano sheet is loaded on the surface of the foamed nickel, and the Ti which has excellent electrochemical performance and is used as the positive electrode material of the super capacitor is prepared3C2the/Ni composite electrode material. The Ti3C2The nano sheet is loaded on the surface of the foamed nickel, and the loading mass of the nano sheet is 0.2-0.6 mg/square centimeter.
Ti3C2The method for preparing the/Ni composite electrode material comprises the following steps:
First, Ti3AlC2Adding into hydrofluoric acid, reacting for 20-26 hours under the condition of uniform stirring at room temperature, centrifuging, washing with water and vacuum drying to obtain Ti with two-dimensional layered structure3C2；
The mass fraction of the hydrofluoric acid is 40-50%;
Ti3AlC2The mass ratio of the hydrofluoric acid to the hydrofluoric acid is 1: 30-1: 50;
a second step of forming Ti of the two-dimensional layered structure obtained in the first step3C2Adding into dimethyl sulfoxide, stirring at room temperature for 22-27 hr, centrifuging, washing with water, and adding Ti3C2Dispersing in deionized water, performing ultrasonic treatment, and centrifuging for 1 hr to obtain Ti3C2A suspension of nanoplatelets;
ti of two-dimensional layered structure3C2The mass ratio of the dimethyl sulfoxide to the dimethyl sulfoxide is 1: 40-1: 60;
Ti3C2The mass ratio of the deionized water to the deionized water is 1: 30-1: 70;
The ultrasonic time is 1-5 hours;
Thirdly, preparing an aqueous solution of a cationic surfactant
The cationic surfactant is one or more of dodecyl trimethyl ammonium chloride (bromide), tetradecyl trimethyl ammonium chloride (bromide), hexadecyl trimethyl ammonium chloride (bromide), didodecyl trimethyl ammonium chloride (bromide) and octadecyl dimethyl benzyl quaternary ammonium chloride (bromide).
The concentration of the aqueous solution of the cationic surfactant is 1-4 mg/ml;
Fourthly, the foam nickel with clean surface is respectively and alternately dipped in the water solution of the cationic surfactant and Ti3C2In the suspension liquid of the nano-sheets, the dipping time is 2-5 minutes each time, and the dipping is carried out for 5-8 times in total; the rest of Ti3C2Loading the suspension of the nanosheets on the surface of the foamed nickel by a vacuum filtration method to obtain Ti3C2Foamed nickel composite electrode material.
The area of the foamed nickel is 1-8cm2Has high specific surface area (28.5 cm)2Per g), high conductivity, low density (350 g/m)2) And a three-dimensional porous structure.
The Ti3C2The nano sheet has a two-dimensional structure, the thickness is 8-15 nanometers, the diameter is 1-2 micrometers, and the conductivity is 1-3 multiplied by 106S/m, strong hydrophilicity, negative surface charge and 70 percent of oxygen-containing functional groups.
The invention has the beneficial effects that:
1) The invention makes full use of two-dimensional Ti3C2The nano-sheet has high conductivity (1-3 multiplied by 10)6S/cm), hydrophilicity, negative surface charge and a large number of oxygen-containing functional groups, the foam nickel has the advantages of high specific surface area, high conductivity, three-dimensional porous structure and the like, and Ti is prepared by a positive and negative charge electrostatic self-assembly method3C2Nano sheet is loaded on the surface of foam nickel to prepare Ti with excellent electrochemical performance3C2the/Ni composite material can be used as a positive electrode material of a super capacitor and is Ti3C2The composite with other transition metal foam framework structures provides a theoretical basis in the research aspect of electrode materials of the super capacitor.
2) the invention utilizes the positive and negative charge static self-assembly method to prepare Ti3C2the/Ni composite electrode material has simple preparation process, less energy consumption andIs easy to be industrially popularized. By using cationic surfactants with negatively charged Ti3C2the nano-sheets are electrostatically attracted and loaded on the surface of the foamed nickel, so that Ti3C2Oxygen-containing functional groups on the surfaces of the nano sheets are exposed on the surfaces of the nano sheets, and more active sites are subjected to redox reaction, so that the nano sheets have more excellent electrochemical performance and higher specific capacity.
3) Ti obtained by the invention3C2A novel composite electrode material applied to a super capacitor electrode material, namely Ti3C2Preparation of Ti by compounding nanosheet and metallic foam nickel as super capacitor anode material3C2The novel composite with other metal foam substrates provides a certain technical basis.
Drawings
FIG. 1 is Ti3C2Cyclic voltammetry profile of the/Ni composite.
FIG. 2 is Ti3C2Constant current charge and discharge curve diagram of the/Ni composite material.
FIG. 3 is Ti3C2Scanning electron microscope images of the/Ni composite material.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that all of the following examples are only for illustrating the present invention and are not intended to limit the scope of the present invention.
Example 1
Ti3C2The preparation method of the/Ni composite material comprises the following steps:
A. Mixing 1.0 g of Ti3AlC2putting 35 g of hydrofluoric acid with the mass fraction of 40% into a 100 ml plastic beaker, uniformly stirring at a certain rotating speed for 24 hours at room temperature, centrifuging, washing with water and drying in vacuum to obtain Ti with a two-dimensional layered structure3C2。
B. Mixing 1 g of Ti with a two-dimensional layered structure obtained in the step A3C2Adding 50g of dimethyl sulfoxide into a 100 ml beaker, and uniformly stirring for 24 hours at room temperatureAfter centrifugation and water washing, Ti is added3C2Dispersing in 45 g deionized water, performing ultrasonic treatment, and centrifuging at 3500 rpm for 1 hr to obtain Ti3C2A suspension of nanoplatelets.
C. Preparing dodecyl trimethyl ammonium chloride water solution with the mass concentration of 2 mg/ml.
D. Respectively and alternately soaking the foamed nickel with the surface treated clean and 4 square centimeters in dodecyl trimethyl ammonium chloride aqueous solution and Ti3C2In the suspension of the nano-sheets, the dipping time is 3 minutes each time, and the dipping is carried out for 7 times; the rest of Ti3C2Loading the suspension of the nanosheets on the surface of the foamed nickel by a vacuum filtration method to obtain Ti3C2the/Ni composite electrode material.
The electrode material Ti of the super capacitor obtained in the embodiment3C2the test chart of the cyclic voltammetry characteristics of the/Ni composite material is shown in FIG. 1, and a pair of obvious redox peak positions can be seen from the chart, which can illustrate Ti3C2the/Ni composite has a pseudo capacitance phenomenon.
The electrode material Ti of the super capacitor obtained in the embodiment3C2the constant current charge and discharge curve of the/Ni composite material is shown in FIG. 2, and the capacity is 618F/g at the current density of 1A/g.
Ti obtained in example3C2The scanning electron microscope image of the/Ni composite material is shown in FIG. 3. As can be seen from fig. 3: ti of two-dimensional layered structure3C2ti obtained by dimethyl sulfoxide intercalation and ultrasonic stripping3C2Nanosheets, and Ti3C2The nano-sheet layers are loaded on the surface of the foam nickel with the three-dimensional porous structure. The invention provides a certain theoretical basis for the research of novel supercapacitor electrode materials.
Example 2
Ti3C2The preparation method of the/Ni composite material comprises the following steps:
A. Mixing 1.0 g of Ti3AlC2Putting 33 g of hydrofluoric acid with the mass fraction of 40 percent into 100 ml of plastic for sinteringUniformly stirring the mixture in a cup at a certain rotating speed for 22 hours at room temperature, centrifuging, washing with water and drying in vacuum to obtain Ti with a two-dimensional layered structure3C2。
B. mixing 1 g of Ti with a two-dimensional layered structure obtained in the step A3C2adding 55 g of dimethyl sulfoxide into a 100 ml beaker, uniformly stirring for 26 hours at room temperature, centrifuging, washing with water, and adding Ti3C2Dispersing in 50g deionized water, performing ultrasonic treatment, and centrifuging at 3500 rpm for 1 hr to obtain Ti3C2A suspension of nanoplatelets.
C. Preparing the hexadecyl trimethyl ammonium chloride aqueous solution with the mass concentration of 3 mg/ml.
D. Respectively and alternately soaking the foamed nickel with the surface treated clean and the area of 6 square centimeters in dodecyl trimethyl ammonium chloride aqueous solution and Ti3C2In the suspension of the nano-sheets, the dipping time is 2.5 minutes each time, and the dipping is carried out for 8 times; the rest of Ti3C2Loading the suspension of the nanosheets on the surface of the foamed nickel by a vacuum filtration method to obtain Ti3C2the/Ni composite electrode material.
Example 3
Ti3C2The preparation method of the/Ni composite material comprises the following steps:
A. Mixing 1.0 g of Ti3AlC2Putting 40 g of hydrofluoric acid with the mass fraction of 49% into a plastic beaker of 100 ml, uniformly stirring for 26 hours at a certain rotating speed at room temperature, and obtaining Ti with a two-dimensional layered structure after centrifugation, water washing and vacuum drying3C2。
B. Mixing 1 g of Ti with a two-dimensional layered structure obtained in the step A3C2Adding 60 g of dimethyl sulfoxide into a 100 ml beaker, uniformly stirring for 22 hours at room temperature, centrifuging, washing with water, and adding Ti3C2Dispersing in 60 g deionized water, performing ultrasonic treatment, and centrifuging at 3500 rpm for 1 hr to obtain Ti3C2A suspension of nanoplatelets.
C. And preparing an aqueous solution of octadecyl dimethyl benzyl quaternary ammonium chloride with the mass concentration of 3 mg/ml.
D. Respectively and alternately soaking the cleaned foamed nickel with the area of 2 square centimeters in dodecyl trimethyl ammonium chloride aqueous solution and Ti3C2In the suspension of the nano-sheets, the dipping time is 4 minutes each time, and the dipping is carried out for 5 times; the rest of Ti3C2loading the suspension of the nanosheets on the surface of the foamed nickel by a vacuum filtration method to obtain Ti3C2the/Ni composite electrode material.
Claims (6)
1. Ti3C2the/Ni composite electrode material is characterized in that foamed nickel is used as a carrier, a cationic surfactant is used as a bridging agent, and Ti3C2Nano-sheet is loaded on foamed nickel to form Ti with two-dimensional/three-dimensional composite structure3C2a/Ni composite electrode material; ti3C2The loading mass of the nanosheets on the surface of the foamed nickel is 0.2-0.6 mg/cm2。
2. Ti3C2the/Ni composite electrode material and the preparation method thereof are characterized by comprising the following steps:
first, Ti3AlC2Adding into hydrofluoric acid, reacting for 20-26 hours under the condition of uniform stirring at room temperature, centrifuging, washing with water and vacuum drying to obtain Ti with two-dimensional layered structure3C2；
Wherein, Ti3AlC2The mass ratio of the hydrofluoric acid to the hydrofluoric acid is 1: 30-1: 50;
A second step of forming Ti of the two-dimensional layered structure obtained in the first step3C2Adding into dimethyl sulfoxide, stirring at room temperature for 22-27 hr, centrifuging, washing with water, and adding Ti3C2Dispersing in deionized water, performing ultrasonic treatment, and centrifuging for 1 hr to obtain Ti3C2A suspension of nanoplatelets;
Wherein Ti is a two-dimensional layered structure3C2The mass ratio of the dimethyl sulfoxide to the dimethyl sulfoxide is 1: 40-1: 60;
thirdly, preparing an aqueous solution of a cationic surfactant
Fourthly, the foam nickel with clean surface is respectively and alternately dipped in the water solution of the cationic surfactant and Ti3C2In the suspension liquid of the nano-sheets, the dipping time is 2-5 minutes each time, and the dipping is carried out for 5-8 times in total; the rest of Ti3C2Loading the suspension of the nanosheets on the surface of the foamed nickel by a vacuum filtration method to obtain Ti3C2the/Ni composite electrode material.
3. The method according to claim 2, wherein the cationic surfactant is one or more selected from the group consisting of dodecyl trimethyl chloride/ammonium bromide, tetradecyl trimethyl chloride/ammonium bromide, hexadecyl trimethyl chloride/ammonium bromide, didodecyl trimethyl chloride/ammonium bromide, and octadecyl dimethyl benzyl quaternary ammonium chloride/bromide, and the concentration of the aqueous solution of the cationic surfactant is 1-4 mg/ml.
4. The method according to claim 2 or 3, wherein, in the second step, the Ti is added3C2The mass ratio of the deionized water to the deionized water is 1: 30-1: 70; the ultrasonic time is 1-5 hours.
5. The method according to claim 2 or 3, wherein the hydrofluoric acid is contained in the first step in an amount of 40 to 50% by mass.
6. the preparation method according to claim 4, wherein the hydrofluoric acid is contained in an amount of 40 to 50% by mass in the first step.
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| CN109686577A (en) * | 2018-12-17 | 2019-04-26 | 滨州学院 | A kind of Ni3S2/d-Ti3C2/ Ni combination electrode material and preparation method thereof |
| CN109592684B (en) * | 2018-12-18 | 2020-09-01 | 燕山大学 | Petal spherical titanium carbide Ti3C2Mxene and preparation method and application thereof |
| CN113061332A (en) * | 2020-01-02 | 2021-07-02 | 合肥杰事杰新材料股份有限公司 | PC material and preparation method thereof |
| CN112233912B (en) * | 2020-09-21 | 2022-05-27 | 郑州大学 | Foam nickel-loaded MnCo2O4.5Preparation method and application of/MXene composite nano material |
| CN112850712A (en) * | 2021-01-04 | 2021-05-28 | 湖北亿纬动力有限公司 | Preparation method and application of MXene material |
| CN112899510B (en) * | 2021-01-18 | 2021-10-19 | 山东科技大学 | In-situ reaction synthesis method of TiC/Ni composite material |
| CN114604945B (en) * | 2022-01-19 | 2023-05-02 | 湖南大学 | Tungsten oxide/titanium carbide composite electrode material and preparation method and application thereof |
| CN116482185B (en) * | 2023-06-25 | 2023-09-29 | 国网浙江省电力有限公司湖州供电公司 | CO sensor gas-sensitive layer and application thereof in lithium battery energy storage system |
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