CN113066673B - Ti3C2Tx-TiO2 nanotube array self-supporting film electrode material and preparation method and application thereof - Google Patents

Ti3C2Tx-TiO2 nanotube array self-supporting film electrode material and preparation method and application thereof Download PDF

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CN113066673B
CN113066673B CN202110313326.XA CN202110313326A CN113066673B CN 113066673 B CN113066673 B CN 113066673B CN 202110313326 A CN202110313326 A CN 202110313326A CN 113066673 B CN113066673 B CN 113066673B
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tio
nanotube array
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supporting film
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CN113066673A (en
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马杰
孙怡然
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Tongji University
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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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
    • C02F1/4691—Capacitive deionisation
    • 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
    • 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
    • H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
    • 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
    • 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
    • H01G11/46—Metal oxides
    • 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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • 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 provides a Ti3C2Tx‑TiO2A nanotube array self-supporting film electrode material and a preparation method and application thereof belong to the field of nano materials. The preparation method comprises the following steps: ti3AlC2Etching, cleaning, stripping and centrifuging to obtain few-layer Ti3C2TxAn aqueous dispersion; ti3C2TxVacuum filtering and drying the aqueous dispersion to obtain Ti3C2TxA self-supporting film; ti3C2TxReacting the self-supporting film in hot alkali liquor and rotating at a certain rotation speed, and cleaning and drying to obtain Ti3C2Tx‑TiO2Nanotube arrays self-supporting films. Ti prepared by the invention3C2Tx‑TiO2Ti in nanotube array self-supporting thin film electrode structure3C2Tx‑TiO2The crystal defects and the array structure with less nanotube structures are favorable for electron transmission, a large number of active sites exposed by the nanotube array are favorable for adsorbing ions or target pollutants, the mechanical property of the material is strong, and the material can be directly used as an electrode material in the fields of super capacitors, capacitor deionization, batteries, electric adsorption and the like.

Description

Ti3C2Tx-TiO2Nanotube array self-supporting film electrode material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of synthesis of environmental materials, and particularly relates to Ti3C2Tx-TiO2A nanotube array self-supporting film electrode material, a preparation method and application thereof.
Background
Electrode materials are key factors in determining the performance of batteries, capacitors, electrosorption, and the like. The common powdery electrode material is usually required to be mixed and dissolved with a binder and a conductive material, and a film is prepared by processes such as coating, and the added binder and solubilizer can seriously influence the performance of the material; and the coating process is complex, has higher requirements on the operation level of personnel, and does not utilize the popularization of large-scale application, so that the development of the directly applicable self-supporting electrode material with excellent performance is very important.
Disclosure of Invention
Aiming at the defects in the prior art, the primary object of the invention is to provide Ti3C2Tx-TiO2The nanotube array self-supporting thin film electrode material.
It is a second object of the present invention to provide the above Ti3C2Tx-TiO2A method for preparing a nanotube array self-supporting film electrode material.
It is a third object of the present invention to provide the above Ti3C2Tx-TiO2The application of the nanotube array self-supporting thin film electrode material.
In order to achieve the above purpose, the solution of the invention is as follows:
ti prepared by the invention3C2Tx-TiO2Ti in nanotube array self-supporting thin film electrode structure3C2Tx-TiO2The crystal defects and the array structure with less nanotube structures are favorable for electron transmission, a large number of active sites exposed by the nanotube array are favorable for adsorbing ions or target pollutants, the mechanical property of the material is strong, and the material can be directly used as an electrode material in the fields of super capacitors, capacitor deionization, batteries, electric adsorption and the like.
Ti3C2Tx-TiO2The preparation method of the nanotube array self-supporting thin film electrode material comprises the following steps:
(1)Ti3AlC2etching, cleaning, intercalation stripping and centrifuging to obtain few-layer Ti3C2TxAn aqueous dispersion;
(2)Ti3C2Txvacuum filtering and drying the aqueous dispersion to obtain Ti3C2TxA self-supporting film;
(3)Ti3C2Txreacting the self-supporting film in hot alkali liquor and rotating at a certain rotation speed, and cleaning and drying to obtain Ti3C2Tx-TiO2Nanotube arrays self-supporting films.
Preferably, in the step (1), one of sodium hydroxide, tetramethylammonium hydroxide, tetrabutylammonium hydroxide and dimethyl sulfoxide is adopted for Ti3AlC2Intercalation is carried out, and ultrasonic stripping is adopted.
Preferably, in step (1), the power of ultrasonic stripping is more than 600W, and the time is more than 1 h.
Preferably, in step (1), the centrifugal speed is more than 3500rpm, and the supernatant after centrifugation is Ti-poor3C2TxAn aqueous dispersion.
Preferably, in step (2), Ti3C2TxThe concentration of the aqueous dispersion should be 0.5mg/mL to 5mg/mL, Ti in a single film3C2TxThe mass is 12mg-40 mg.
Preferably, in step (2), the temperature at which the film is dried is 20 ℃ to 60 ℃.
Preferably, in the step (3), the alkali liquor is composed of one of sodium hydroxide and potassium hydroxide, the concentration of the alkali liquor is 8-15 mol/L, the heating temperature is 40-80 ℃, and the heating time is 6-12 h.
Preferably, in step (3), the film is protected by a clamp during rotation, and the rotation speed is 300rpm to 600 rpm.
Ti3C2Tx-TiO2The nanotube array self-supporting film electrode material is obtained by the preparation method.
A Ti as described above3C2Tx-TiO2The nanotube array self-supporting film electrode material can be used in the fields of super capacitors, capacitive deionization, batteries, electro-adsorption and the like.
Due to the adoption of the scheme, the invention has the beneficial effects that:
first, Ti prepared by the present invention3C2Tx-TiO2Ti in nanotube array self-supporting thin film electrode structure3C2Tx-TiO2The nanotube structure has fewer crystal defects and the array structure is favorable for electron transmission.
Secondly, the large number of active sites exposed by the nanotube array structure of the present invention is beneficial for adsorbing ions or target pollutants.
Third, Ti prepared by the invention3C2Tx-TiO2The nanotube array self-supporting film electrode has strong mechanical property, and can be directly used for electrode materials without the treatment of size mixing, film scraping and the like.
Fourthly, the preparation method of the invention has simple equipment and simple and easy process, and is suitable for large-scale production.
In conclusion, the present invention produces Ti having excellent electrical properties3C2TxAnd a self-supporting film of (2) and use of Ti3C2TxIs oxidized in hot alkali solution to obtain Ti3C2Tx-TiO2Heterojunction, and forming the nanotube array by applying centripetal force. Ti obtained by the method3C2Tx-TiO2The nanotube array self-supporting thin film electrode has excellent performance, has the characteristics of few crystal defects, fast electron transmission, rich active sites and the like, is simple and easy in process, is suitable for large-scale production, and can be directly applied to electrode materials in the fields of super capacitors, capacitor deionization, batteries, electro-adsorption and the like.
Detailed Description
The invention provides a Ti3C2Tx-TiO2A nanotube array self-supporting film electrode material, a preparation method and application thereof.
Drawings
FIG. 1 shows Ti in example 13C2Tx-TiO2Scanning electron microscope images of the nanotube array self-supporting thin film electrode material;
FIG. 2 is an impedance spectrum of the self-supporting thin film electrode material of Ti3C2Tx-TiO2 nanotube array in example 1;
FIG. 3 is a diagram of the capacitive deionization and desalination performance of the self-supporting thin film electrode material of Ti3C2Tx-TiO2 nanotube array in example 1.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to limit the scope of the present invention.
Example 1:
ti of the example3C2Tx-TiO2The preparation method of the nanotube array self-supporting thin film electrode material comprises the following steps:
(1) 2g of lithium fluoride and 9M of 40ml of hydrochloric acid were weighed out and stirred in a polytetrafluoroethylene beaker (volume 100ml) for 30min at a speed of 400 rpm.
(2) 2g of Ti3AlC2Slowly adding the mixture into the beaker in the first step, adjusting the reaction temperature to 35 ℃, and continuously stirring for 24 hours.
(3) Ti obtained in the step (2)3C2TxThe product was washed by centrifugation (3500rpm, 5min) with deionized water to remove the lower precipitate and the procedure was repeated to pH>5。
(4) Dispersing the product obtained in the step (3) by deionized water, adding proper amount of dimethyl sulfoxide into the mixture, and adding the dimethyl sulfoxide into the mixture in the presence of N2After 2h of sonication under atmosphere, the supernatant was removed by centrifugation (3500rpm, 5 min). 5mL of the supernatant was dried to determine its concentration.
(5) Diluting the supernatant obtained in the step (4) to 2mg/mL, taking 10mL of the supernatant, taking a water system filter membrane as a substrate, and carrying out vacuum filtration to obtain Ti3C2TxA film.
(6) Naturally drying the film obtained in the step (5) at room temperature, and taking down the water system filter membrane to obtain self-supporting Ti3C2TxA film.
(7) Subjecting the self-supporting Ti obtained in (6)3C2TxThe film was placed in a holder and heated at 50 ℃ for 10h with 10mol/L KOH at 400 rpm.
(8) The product of (7) is removedWashing with water to pH<8, drying in an oven at 60 ℃ to obtain Ti3C2Tx-TiO2Nanotube arrays self-supporting films.
FIG. 1 shows Ti in an example of the present invention3C2Tx-TiO2The scanning electron microscope image of the nanotube array self-supporting film electrode material shows that the nanotube array structure uniformly grown on the surface of the film can be seen, and the nanotube array provides more active sites, thereby being beneficial to the adsorption and electron transmission of target pollutants and ions.
FIG. 2 shows Ti in an example of the present invention3C2Tx-TiO2The impedance spectrum of the nanotube array self-supporting thin film electrode material shows that the internal ohmic resistance and the charge transfer resistance of the electrode are respectively 25.33ohm and 1.99ohm, and the lower resistance is favorable for the transmission of electrons.
FIG. 3 shows Ti in an example of the present invention3C2Tx-TiO2The capacitive deionization and desalination performance diagram of the nanotube array self-supporting thin film electrode material shows that the desalination capacity of the nanotube array self-supporting thin film electrode material is up to 106mg/g under the current density of 30mA/g, and the application potential of the nanotube array self-supporting thin film electrode material in the capacitive deionization direction is shown.
Example 2:
ti of the example3C2Tx-TiO2The preparation method of the nanotube array self-supporting thin film electrode material comprises the following steps:
(1) 2g of lithium fluoride and 9M of 40ml of hydrochloric acid were weighed out and stirred in a polytetrafluoroethylene beaker (volume 100ml) for 30min at a speed of 400 rpm.
(2) 2g of Ti3AlC2Slowly adding the mixture into the beaker in the first step, adjusting the reaction temperature to 35 ℃, and continuously stirring for 24 hours.
(3) Ti obtained in the step (2)3C2TxThe product was washed by centrifugation (3500rpm, 5min) with deionized water to remove the lower precipitate and the procedure was repeated to pH>5。
(4) Dispersing the product obtained in the step (3) by deionized water, adding proper amount of dimethyl sulfoxide into the mixture, and adding the dimethyl sulfoxide into the mixture in the presence of N2After 2h of sonication under atmosphere, centrifugation (3500 r)pm, 5min) and taking the supernatant. 5mL of the supernatant was dried to determine its concentration.
(5) Diluting the supernatant obtained in the step (4) to 1mg/mL, taking 15mL of the supernatant, taking a water system filter membrane as a substrate, and carrying out vacuum filtration to obtain Ti3C2TxA film.
(6) Naturally drying the film obtained in the step (5) at room temperature, and taking down the water system filter membrane to obtain self-supporting Ti3C2TxA film.
(7) Subjecting the self-supporting Ti obtained in (6)3C2TxThe film was placed in a jig and heated at 50 ℃ for 10 hours at 400rpm with 12mol/L NaOH.
(8) Washing the product of (7) with deionized water to pH<8, drying in an oven at 60 ℃ to obtain Ti3C2Tx-TiO2Nanotube arrays self-supporting films.
Ti3C2Tx-TiO2The nanotube array self-supporting film electrode material can be used as an electrode material in the fields of super capacitors, capacitive deionization, batteries, electro-adsorption and the like.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments. Those skilled in the art should appreciate that many modifications and variations are possible in light of the above teaching without departing from the scope of the invention.

Claims (3)

1. Ti3C2Tx-TiO2The preparation method of the nanotube array self-supporting film electrode material is characterized by comprising the following steps:
(1)Ti3AlC2etching, cleaning, stripping and centrifuging to obtain few-layer Ti3C2TxAn aqueous dispersion;
(2)Ti3C2Txvacuum filtering and drying the aqueous dispersion to obtain Ti3C2TxA self-supporting film;
(3) reacting the Ti3C2Tx self-supporting film in hot alkali liquor and rotating at a certain rotation speed, and cleaning and drying to obtain the Ti3C2Tx-TiO2 nanotube array self-supporting film;
in the step (1), one of sodium hydroxide, tetramethyl ammonium hydroxide, tetrabutyl ammonium hydroxide and dimethyl sulfoxide is adopted to react with Ti3AlC2Intercalation is carried out, and ultrasonic stripping is adopted;
in the step (1), the power of ultrasonic stripping is more than 600W, and the time is more than 1 h;
in the step (1), the centrifugal speed is more than 3500rpm, and the supernatant after centrifugation is Ti with few layers3C2TxAn aqueous dispersion;
in the step (2), Ti3C2TxThe concentration of the aqueous dispersion should be 0.5mg/mL to 5mg/mL, Ti in a single film3C2TxThe mass is 12mg-40 mg;
in the step (2), the drying temperature of the film is 20-60 ℃;
in the step (3), the alkali liquor is composed of one of sodium hydroxide and potassium hydroxide, the concentration of the alkali liquor is 8-15 mol/L, the heating temperature is 40-80 ℃, and the heating time is 6-12 h;
in the step (3), the film is protected by a clamp during rotation, and the rotation speed is 300-600 rpm.
2. Ti3C2Tx-TiO2The nanotube array self-supporting film electrode material is characterized in that: which is obtained by the production process according to claim 1.
3. Ti according to claim 23C2Tx-TiO2The nanotube array self-supporting film electrode material is applied to the fields of super capacitors or capacitor deionization or batteries or electric adsorption.
CN202110313326.XA 2021-03-24 2021-03-24 Ti3C2Tx-TiO2 nanotube array self-supporting film electrode material and preparation method and application thereof Active CN113066673B (en)

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