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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- 229910009819 Ti3C2 Inorganic materials 0.000 title claims abstract description 58
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 239000007772 electrode material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 86
- 239000002135 nanosheet Substances 0.000 claims abstract description 35
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 29
- KRHYYFGTRYWZRS-UHFFFAOYSA-N hydrofluoric acid Substances F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 26
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000003093 cationic surfactant Substances 0.000 claims abstract description 12
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000000725 suspension Substances 0.000 claims description 15
- 238000007598 dipping method Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000006260 foam Substances 0.000 claims description 8
- 238000011068 loading method Methods 0.000 claims description 7
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 6
- 239000002064 nanoplatelet Substances 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 238000003828 vacuum filtration Methods 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 4
- -1 octadecyl dimethyl benzyl quaternary ammonium chloride Chemical compound 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 4
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 claims 4
- 239000011165 3D composite Substances 0.000 claims 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims 1
- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 239000003990 capacitor Substances 0.000 abstract description 15
- 238000002156 mixing Methods 0.000 abstract description 7
- 238000011160 research Methods 0.000 abstract description 5
- 238000000707 layer-by-layer assembly Methods 0.000 abstract description 4
- 239000006262 metallic foam Substances 0.000 abstract description 4
- 238000009830 intercalation Methods 0.000 abstract description 2
- 230000002687 intercalation Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000005530 etching Methods 0.000 abstract 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 238000011161 development Methods 0.000 description 5
- 125000000524 functional group Chemical group 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 239000010405 anode material Substances 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 101100001674 Emericella variicolor andI gene Proteins 0.000 description 1
- XWMGYUIDSBAERU-UHFFFAOYSA-N [Cl-].C(CCCCCCCCCCC)C([NH+](C)C)CCCCCCCCCCCC Chemical compound [Cl-].C(CCCCCCCCCCC)C([NH+](C)C)CCCCCCCCCCCC XWMGYUIDSBAERU-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- OYDXOJWORLEYQD-UHFFFAOYSA-M dodecyl(trimethyl)azanium chloride hydrate Chemical compound O.[Cl-].CCCCCCCCCCCC[N+](C)(C)C OYDXOJWORLEYQD-UHFFFAOYSA-M 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- CEYYIKYYFSTQRU-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)C CEYYIKYYFSTQRU-UHFFFAOYSA-M 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
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 |
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