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N-doped MXene material and preparation method and application thereof

A ceramic material, ammonia technology, applied in the manufacture of hybrid/electric double-layer capacitors, hybrid capacitor electrodes, etc., can solve the problems of unfavorable large-scale preparation, destabilized structure, long reaction period, etc., achieve excellent electrochemical performance, improve Safety, compact and regular effect

Inactive Publication Date: 2018-11-16
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

N-doping by solvothermal method often generates many small molecular by-products; N-doping by plasma method can replace some carbon atoms of MXene with nitrogen atoms, but doing so will destroy its own stable structure; using microwave irradiation gas phase method The N doping reaction period is long and the operation is cumbersome, which is not conducive to large-scale preparation; in comparison, the heat treatment method is doped in ammonia gas, no by-products are generated, and it is easy to control
In the process of preparing N-doped MXene by heat treatment in existing reports, in order to improve the effect of nitrogen doping, NH 3 、H 2 Mixed gas with Ar, and nitrogen doping at 600-1000°C, H 2 It is a flammable and explosive gas, so there are potential safety hazards in actual production

Method used

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  • N-doped MXene material and preparation method and application thereof
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  • N-doped MXene material and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0033] To prepare N-doped MXene materials, the specific steps are as follows:

[0034] 1) Single or few layers of Ti 3 C 2 T X Preparation: 3g Ti 3 C 2 Slowly add Al powder to 30mL 48wt% hydrofluoric acid solution, stir at 38°C for 72h, centrifuge to remove the supernatant, pour deionized water, repeat the cleaning-centrifugation process until the pH of the supernatant is 6, and collect the precipitate and vacuum-dried to obtain "accordion-like" multi-layer stacked Ti 3 C 2 Tx, then the resulting Ti 3 C 2 Tx (about 2g) was placed in 20mL DMSO for stirring intercalation treatment, the stirring rate was 800-1000r / min, and then centrifuged for 6-8 times under the condition of water medium, and finally ultrasonic stripping was carried out, and the supernatant liquid was taken by low-speed centrifugation and placed in vacuum at 60°C. Dry in a drying oven for 48 hours to obtain single-layer or few-layer Ti 3 C 2 T X phase material;

[0035] 2) Preparation of N-doped MXen...

Embodiment 2

[0040] Utilize the N-doped MXene material (N-Ti prepared by embodiment 1 3 C 2 T x ) to prepare paper-based microcapacitors, the specific method is as follows: 100mg of Ti 3 C 2 T X Prepare 10mL of an aqueous solution with a concentration of 10mg / mL, and use vacuum filtration to add 0.2mL of 10mg / mL conductive silver paste into a suction filter funnel filled with 300mL of ethyl acetate for suction filtration, and then take 0.2mL of 10mg / mL N-Ti 3 C 2 T x The aqueous solution was placed in 300mL deionized water, and pumped sequentially onto a paper chip made of UV ordered lithography SU-8 glue coated with ordinary filter paper (soak the filter paper in the solution of photosensitive reagent SU-8, make SU-8 Coat evenly on the filter paper under the action of a homogenizer, the homogenization time is 30-120s, and then put the above-mentioned filter paper coated with SU-8 optical glue in an oven, bake at 60-90℃ for 12-24h , UV lithography was carried out under the protecti...

Embodiment 3

[0043] The N-doped MXene material was prepared by a method similar to Example 1. The difference from Example 1 was that the flow rate of ammonia gas was 100 sccm, the flow rate of argon gas was 100 sccm, and the temperature was raised to 300 at a rate of 5 °C / min at room temperature. ℃, heat preservation for 2h for calcination to obtain N-Ti 3 C 2 T x .

[0044] Prepare paper-based microcapacitors, the specific method is as follows: take 100mg of the N-Ti prepared above 3 C 2 T x Prepare 10mL of an aqueous solution with a concentration of 10mg / mL, and use vacuum filtration to add 0.2mL of 10mg / mL conductive silver paste into a suction filter funnel filled with 300mL of ethyl acetate for suction filtration, and then take 0.2mL of 10mg / mL N-Ti 3 C 2 T x The aqueous solution was placed in 300mL deionized water, and sequentially pumped onto a paper chip made of ordinary filter paper coated with SU-8 glue coated with UV-ordered lithography, and taken out and placed at room...

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Abstract

The invention relates to N-doped MXene material and preparation method and application thereof. The N-doped MXene material is obtained by performing intercalation and stripping to obtain single-layeror few-layer of MXene after an MAX-phase ceramic material is etched to remove an A atomic layer and then placing the material in a mixed gas of ammonia gas and argon for calcination. The N-doped MXenematerial provided by the invention has a single-layer sheet-shaped structure, the electrolyte ion transmission rate is improved, an N element is uniformly coated on a surface of the MXene layer, thefaradic pseudo-capacitance and the conductivity of the MXene are improved, the anisotropy of the MXene is reduced, and the MXene arrangement is more compact and in order; moreover, the N element is coated on the surface of the MXene sheet layer, more electrochemical active sites are exposed, great convenience is provided for electrolyte ion transmission and exchange, and the N-doped MXene materialhas more excellent electrochemical performance and superhigh specific capacitance.

Description

technical field [0001] The invention relates to the field of micro-supercapacitors, in particular to an N-doped MXene material, a preparation method thereof, and an application in paper-based microcapacitors. Background technique [0002] The transition metal carbide (MXenes) material was discovered by researchers Yuri Gogotsi and Michel Barsoum of Drexel University in the United States in 2011. It is a new member of the family of two-dimensional materials after graphene. The MXenes material is mainly obtained by selectively etching the A atomic layer in the ternary layered compound material MAX (A represents group IIIA and IVA elements). After selectively etching away the A atomic layer in MAX, a multilayer MXene (M n+ 1 x n Tx) structure, where M represents the early transition metal elements (Sc, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, etc.), X represents carbon or nitrogen, n=1, 2 or 3, and Tx represents Functional groups (-O, -OH, or -F) for surface adsorption. The appearan...

Claims

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Application Information

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IPC IPC(8): H01G11/34H01G11/86
CPCH01G11/34H01G11/86Y02E60/13
Inventor 周爱军孙贺雷孙义民曾伟王若冲
Owner WUHAN INSTITUTE OF TECHNOLOGY
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