CN108987126A - A kind of Ti3C2/ Ni combination electrode material and preparation method thereof - Google Patents
A kind of Ti3C2/ Ni combination electrode material and preparation method thereof Download PDFInfo
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- CN108987126A CN108987126A CN201811134889.7A CN201811134889A CN108987126A CN 108987126 A CN108987126 A CN 108987126A CN 201811134889 A CN201811134889 A CN 201811134889A CN 108987126 A CN108987126 A CN 108987126A
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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 field of material technology, disclose a kind of Ti3C2/ Ni combination electrode material and preparation method thereof.By Ti3AlC2The Ti of two-dimensional structure is obtained by hf etching3C2；By the Ti of two-dimensional structure3C2The negatively charged Ti in surface is obtained by dimethyl sulfoxide intercalation and ultrasound removing3C2Nanometer sheet；Pass through cationic surfactant and Ti3C2Nanometer sheet positive and negative charge electrostatic self-assembled method is by Ti3C2Nanometer sheet is supported on the surface of nickel foam and obtains Ti3C2/ Ni combination electrode material.Preparation process flow of the present invention is quick and easy, at low cost, and combination electrode material has excellent chemical property, can make the electrode material of supercapacitor, while being Ti3C2The compound of nanometer sheet and other metal foams provides certain theoretical research foundation in terms of electrode material for super capacitor research.
Description
Technical field
The invention belongs to field of material technology, it is to disclose a kind of Ti3C2/ Ni combination electrode material and preparation method thereof.
Background technique
Along with the transition exploitation of the non-renewable energy resources such as coal, fossil fuel and severe environmental pollution, green energy resource
Exploitation and its sustainable development are increasingly concerned, and research and develop a kind of high-efficiency environment friendly, and inexpensive energy storage and conversion are
It unites extremely urgent.Supercapacitor is as a kind of high-efficiency energy-storage device, because it is with power density height, charge-discharge velocity
Fastly, the features such as having extended cycle life and be environmental-friendly and attract extensive attention.Currently, supercapacitor has been successfully applied to just
The fields such as formula consumer electronics product are taken, there is extensive market development prospect.
According to different energy storage mechanisms, supercapacitor can be divided into double layer capacitor and pseudocapacitors.Electric double layer capacitance
Device is to cause the face-off of charge to carry out charge and discharge process by electronics or aligning for ion in Cathode/Solution Interface；It is counterfeit
Capacitor is then to carry out charge and discharge electrician by the chemical adsorption desorption and redox reaction of electroactive material generation high reversible
Make.The usual transition metal oxide of the electrode material of pseudocapacitors, hydroxide etc. and polymer, but due to its electric conductivity
And stability it is poor the disadvantages of and apply be restricted.Therefore super capacitor a kind of novel and with excellent electrochemical performance is developed
Device electrode material becomes a critical issue.The Ti studied herein3C2/ Ni composite material for the first time positive electrode and be applied to it is super
Capacitor provides brand-new research direction to prepare the development of Novel super capacitor electrode material.
Summary of the invention
It is an object of the invention to disclose a kind of Ti3C2/ Ni combination electrode material and preparation method thereof.Based on Ti3C2Nanometer
The superior electrical conductivity of piece has the characteristics that negative potential and surface have a large amount of oxygen-containing functional groups, certainly by positive and negative charge electrostatic
Construction from part is by Ti3C2Nanometer sheet is supported on three-dimensional porous structure and with the foam nickel surface of high conductivity, passes through Ti3C2
Contact of the nanometer sheet with nickel foam and the advantage that both gives full play to and show good chemical property.
Technical solution of the present invention:
A kind of Ti3C2/ Ni combination electrode material sufficiently combines Ti3C2The advantages of nanometer sheet and nickel foam, is based on two dimension Ti3C2
Nanometer sheet conductivity height (1~3 × 106S/m), hydrophily, surface is negatively charged and has the characteristics that a large amount of oxygen-containing functional groups, bubble
Foam nickel has the characteristics that high-specific surface area, high conductivity, low-density and three-dimensional porous structure, using nickel foam as substrate, sun from
Sub- surfactant is as bridging agent, by Ti by way of positive and negative charge electrostatic self-assembled3C2Nanometer sheet is supported on nickel foam table
Face is prepared with excellent chemical property and as the Ti of super capacitor anode material3C2/ Ni combination electrode material.Institute
State Ti3C2Nanometer sheet is 0.2~0.6 milli gram/cm in nickel foam area load quality.
A kind of Ti3C2/ Ni combination electrode material and preparation method thereof, steps are as follows:
The first step, by Ti3AlC2It is added in hydrofluoric acid, under conditions of room temperature uniform stirring, reacts 20-26 hours, warp
Centrifugation, washing and vacuum drying are crossed, the Ti with two-dimensional layered structure is obtained3C2；
The mass fraction of hydrofluoric acid is 40%~50%；
Ti3AlC2Mass ratio with hydrofluoric acid is 1:30~1:50；
Second step, the Ti for the two-dimensional layered structure that the first step is obtained3C2It is added to dimethyl sulfoxide, is stirred at room temperature
22-27 hours, after being centrifuged, washing, then by Ti3C2Dispersion carries out ultrasound in deionized water, and centrifugation obtains Ti in 1 hour3C2
The suspension of nanometer sheet；
The Ti of two-dimensional layered structure3C2Mass ratio with dimethyl sulfoxide is 1:40~1:60；
Ti3C2Mass ratio with deionized water is 1:30~1:70；
Ultrasonic time is 1-5 hours；
Third step prepares the aqueous solution of cationic surfactant
Cationic surfactant is that trimethyl chlorine (bromine) changes ammonium, and tetradecyltrimethylammonium chlorine (bromine) changes ammonium,
Cetyl trimethyl chlorine (bromine) changes ammonium, and double trimethyl chlorine (bromine) change ammonium, octadecyl dimethyl benzyl quaternary ammonium chlorine
The mixing of one or more of (bromine) compound.
The concentration of aqueous solution of cationic surfactant is 1-4mg/ml；
4th step, will be surface-treated clean nickel foam difference alternating impregnating cationic surfactant aqueous solution with
Ti3C2In the suspension of nanometer sheet, each dip time is 2-5 minutes, altogether alternating impregnating 5-8 times；By remaining Ti3C2Nanometer
The suspension of piece is supported on foam nickel surface by the method being filtered by vacuum to get Ti is arrived3C2/ nickel foam combination electrode material.
The area of the nickel foam is 1-8cm2, there is high-specific surface area (28.5cm2/ g), high conductivity, low-density
(350g/m2) and three-dimensional porous structure.
The Ti3C2Nanometer sheet has two-dimensional structure, thickness at 8~15 nanometers, diameter at 1~2 micron, conductivity 1~
3×106S/m, hydrophily is strong, and surface is negatively charged and has 70% oxygen-containing functional group.
Beneficial effects of the present invention:
1) present invention makes full use of two-dimentional Ti3C2Nanometer sheet conductivity height (1~3 × 106S/cm), hydrophily, surface band are negative
Electricity and have the characteristics that a large amount of oxygen-containing functional groups, nickel foam is with high-specific surface area, high conductivity and three-dimensional porous structure
The advantages that, by positive and negative charge electrostatic self-assembled method by Ti3C2Nanometer sheet is supported on foam nickel surface and prepares with excellent electricity
Chemical property Ti3C2/ Ni composite material can be used as the positive electrode of supercapacitor, while be Ti3C2With other transition gold
The compound for belonging to foam framework structure provides theoretical basis in terms of electrode material for super capacitor research.
2) present invention prepares Ti using the method for positive and negative charge electrostatic self-assembled3C2/ Ni combination electrode material, preparation process
Simply, energy consumption is less and is easy to industrialization promotion.By utilizing cationic surfactant and negatively charged Ti3C2It receives
Rice piece electrostatic attraction and be supported on foam nickel surface so that Ti3C2The oxygen-containing functional group on nanometer sheet surface is exposed to its surface, more
More active sites carries out redox reaction and has superior chemical property, specific capacity with higher.
3) Ti that the present invention obtains3C2/ Ni combination electrode material is a kind of applied to the novel multiple of electrode material for super capacitor
Composite electrode material, it is this by Ti3C2Nanometer sheet and the compound conduct super capacitor anode material of metal foam nickel are preparation Ti3C2
Certain technical basis is provided with the novel complexes of other metallic foam substrates.
Detailed description of the invention
Fig. 1 is Ti3C2The Cyclic voltamogram curve graph of/Ni composite material.
Fig. 2 is Ti3C2The constant current charge-discharge curve graph of/Ni composite material.
Fig. 3 is Ti3C2The scanning electron microscope (SEM) photograph of/Ni composite material.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that following all examples is merely to illustrate this
It invents rather than limits the scope of the invention.
Embodiment 1
A kind of Ti3C2The preparation method of/Ni composite material, comprising the following steps:
A. by 1.0 grams of Ti3AlC2The hydrofluoric acid for being 40% with 35 gram mass scores is put into 100 milliliters of plastic beaker, and
At room temperature with certain revolving speed uniform stirring 24 hours, by centrifugation, washing and vacuum drying, obtain with two-dimensional layered structure
Ti3C2。
B. by the Ti of the obtained 1 gram of two-dimensional layered structure of step A3C2100 milliliters of burning is put into 50 grams of dimethyl sulfoxides
In cup, uniform stirring 24 hours at room temperature, by centrifugation, washing and then by Ti3C2Be dispersed in 45 grams of deionized waters into
Row ultrasound, is centrifuged 1 hour under 3500 revs/min of revolving speed and obtains Ti3C2The suspension of nanometer sheet.
C. preparing mass concentration is 2 mg/ml dodecyl trimethyl ammonium chloride aqueous solutions.
D. the nickel foam that clean area is 4 square centimeters will be surface-treated and distinguish alternating impregnating in trimethyl
Aqueous ammonium chloride solution and Ti3C2In the suspension of nanometer sheet, each dip time is 3 minutes, co-impregnation 7 times；It will be remaining
Ti3C2The suspension of nanometer sheet is supported on foam nickel surface by the method being filtered by vacuum to get Ti is arrived3C2/ Ni combination electrode material
Material.
The electrode material for super capacitor Ti that the present embodiment obtains3C2/ Ni composite material Cyclic voltamogram test chart is as schemed
Shown in 1, a pair of apparent redox peak position, can illustrate Ti as seen from the figure3C2There is fake capacitance phenomenons for/Ni compound.
The electrode material for super capacitor Ti that the present embodiment obtains3C2/ Ni composite material constant current charge-discharge curve graph such as Fig. 2
Shown, capacity is 618F/g under the current density of 1A/g.
The Ti that the present embodiment obtains3C2/ Ni composite material scanning electron microscope (SEM) photograph is as shown in Figure 3.As seen from Figure 3: two-dimensional layer
The Ti of shape structure3C2The Ti obtained by dimethyl sulfoxide intercalation and ultrasound removing3C2Nanometer sheet, and Ti3C2Nanometer sheet is layer by layer
It is supported on the foam nickel surface of three-dimensional porous structure.The present invention provides centainly for the research of Novel super capacitor electrode material
Theoretical basis.
Embodiment 2
A kind of Ti3C2The preparation method of/Ni composite material, comprising the following steps:
A. by 1.0 grams of Ti3AlC2The hydrofluoric acid for being 40% with 33 gram mass scores is put into 100 milliliters of plastic beaker, and
At room temperature with certain revolving speed uniform stirring 22 hours, by centrifugation, washing and vacuum drying, obtain with two-dimensional layered structure
Ti3C2。
B. by the Ti of the obtained 1 gram of two-dimensional layered structure of step A3C2100 milliliters of burning is put into 55 grams of dimethyl sulfoxides
In cup, uniform stirring 26 hours at room temperature, by centrifugation, washing and then by Ti3C2Be dispersed in 50 grams of deionized waters into
Row ultrasound, is centrifuged 1 hour under 3500 revs/min of revolving speed and obtains Ti3C2The suspension of nanometer sheet.
C. preparing mass concentration is 3 mg/ml hexadecyltrimethylammonium chloride aqueous solutions.
D. the nickel foam that clean area is 6 square centimeters will be surface-treated and distinguish alternating impregnating in trimethyl
Aqueous ammonium chloride solution and Ti3C2In the suspension of nanometer sheet, each dip time is 2.5 minutes, co-impregnation 8 times；It will be remaining
Ti3C2The suspension of nanometer sheet is supported on foam nickel surface by the method being filtered by vacuum to get Ti is arrived3C2/ Ni combination electrode material
Material.
Embodiment 3
A kind of Ti3C2The preparation method of/Ni composite material, comprising the following steps:
A. by 1.0 grams of Ti3AlC2The hydrofluoric acid for being 49% with 40 gram mass scores is put into 100 milliliters of plastic beaker, and
At room temperature with certain revolving speed uniform stirring 26 hours, by centrifugation, washing and vacuum drying, obtain with two-dimensional layered structure
Ti3C2。
B. by the Ti of the obtained 1 gram of two-dimensional layered structure of step A3C2100 milliliters of burning is put into 60 grams of dimethyl sulfoxides
In cup, uniform stirring 22 hours at room temperature, by centrifugation, washing and then by Ti3C2Be dispersed in 60 grams of deionized waters into
Row ultrasound, is centrifuged 1 hour under 3500 revs/min of revolving speed and obtains Ti3C2The suspension of nanometer sheet.
C. preparing mass concentration is 3 mg/ml octadecyl dimethyl benzyl aliquat aqueous solutions.
D. the nickel foam that clean area is 2 square centimeters will be handled and distinguish alternating impregnating in trimethyl chlorination
Aqueous ammonium and Ti3C2In the suspension of nanometer sheet, each dip time is 4 minutes, co-impregnation 5 times；By remaining Ti3C2It receives
The suspension of rice piece is supported on foam nickel surface by the method being filtered by vacuum to get Ti is arrived3C2/ Ni combination electrode material.
Claims (6)
1. a kind of Ti3C2/ Ni combination electrode material, which is characterized in that using nickel foam as carrier, with cationic surfactant
As bridging agent, Ti3C2Nanometer sheet is supported in nickel foam, forms the Ti of two-dimensional/three-dimensional composite construction3C2/ Ni combination electrode material
Material；Ti3C2Nanometer sheet is 0.2~0.6mg/cm in nickel foam area load quality2。
2. a kind of Ti3C2/ Ni combination electrode material and preparation method thereof, which is characterized in that steps are as follows:
The first step, by Ti3AlC2Be added in hydrofluoric acid, under conditions of room temperature uniform stirring, react 20-26 hours, by from
The heart, washing and vacuum drying obtain the Ti with two-dimensional layered structure3C2；
Wherein, Ti3AlC2Mass ratio with hydrofluoric acid is 1:30~1:50；
Second step, the Ti for the two-dimensional layered structure that the first step is obtained3C2It is added to dimethyl sulfoxide, 22-27 is stirred at room temperature
Hour, after being centrifuged, washing, then by Ti3C2Dispersion carries out ultrasound in deionized water, and centrifugation obtains Ti in 1 hour3C2Nanometer
The suspension of piece；
Wherein, the Ti of two-dimensional layered structure3C2Mass ratio with dimethyl sulfoxide is 1:40~1:60；
Third step prepares the aqueous solution of cationic surfactant
4th step will be surface-treated clean nickel foam difference alternating impregnating in the aqueous solution and Ti of cationic surfactant3C2
In the suspension of nanometer sheet, each dip time is 2-5 minutes, altogether alternating impregnating 5-8 times；By remaining Ti3C2Nanometer sheet is hanged
Supernatant liquid is supported on foam nickel surface by the method being filtered by vacuum to get Ti is arrived3C2/ Ni combination electrode material.
3. preparation method according to claim 2, which is characterized in that the cationic surfactant is dodecyl
Trimethyl chlorine (bromine) changes ammonium, tetradecyltrimethylammonium chlorine (bromine) changes ammonium, cetyl trimethyl chlorine (bromine) changes ammonium, double dodecyls
Trimethyl chlorine (bromine) changes ammonium, the mixing of one or more of octadecyl dimethyl benzyl quaternary ammonium chlorine (bromine) compound, sun from
The concentration of aqueous solution of sub- surfactant is 1-4mg/ml.
4. preparation method according to claim 2 or 3, which is characterized in that in second step, the Ti3C2With deionized water
Mass ratio be 1:30~1:70；Ultrasonic time is 1-5 hours.
5. preparation method according to claim 2 or 3, which is characterized in that in the first step, the quality point of the hydrofluoric acid
Number is 40%~50%.
6. the preparation method according to claim 4, which is characterized in that in the first step, the mass fraction of the hydrofluoric acid
It is 40%~50%.
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| CN109592684A (en) * | 2018-12-18 | 2019-04-09 | 燕山大学 | A kind of petal spherical carbide titanium and its preparation method and application |
| 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 |
| CN112233912A (en) * | 2020-09-21 | 2021-01-15 | 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 |
| CN112899510A (en) * | 2021-01-18 | 2021-06-04 | 山东科技大学 | In-situ reaction synthesis method of TiC/Ni composite material |
| 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 |
| CN114604945A (en) * | 2022-01-19 | 2022-06-10 | 湖南大学 | Tungsten oxide/titanium carbide composite electrode material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112233912A (en) * | 2020-09-21 | 2021-01-15 | 郑州大学 | Foam nickel-loaded MnCo2O4.5Preparation method and application of/MXene composite nano material |
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| CN114604945A (en) * | 2022-01-19 | 2022-06-10 | 湖南大学 | Tungsten oxide/titanium carbide composite electrode material and preparation method and application thereof |
| CN116482185A (en) * | 2023-06-25 | 2023-07-25 | 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 |
| 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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