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Method for preparing polyhydroxyl functional group Ti3C2Tx material through two-step etching method

A technology of polyhydroxyl functionalization and etching method, which is applied in the field of preparation of polyhydroxyl functional group Ti3C2Tx, can solve the problems of chemical activity and electrochemical performance reduction, and achieve good electrochemical performance, high synthesis efficiency, and process controllable effects

Active Publication Date: 2020-02-14
YANSHAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004]Ti3C2TxDue to its sheet structure, it can be an ion Diffusion provides channels and is an excellent energy storage material. The existing etching methods for Ti3C2Tx are: Lift-off etching of Ti3AlC2[1] with HF proposed by Gogotsi and Barsoum, and its improved version using LiF and HCl in Etching [2] under heating conditions, and using NH4HF to etch [3], the use of NH 4F etches [4] under hydrothermal conditions; because Ti3C2Tx is a competitive reaction, so the distribution of a large number of fluorine functional groups on the surface is random and non-uniform, resulting in a decrease in its chemical activity and electrochemical performance

Method used

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  • Method for preparing polyhydroxyl functional group Ti3C2Tx material through two-step etching method
  • Method for preparing polyhydroxyl functional group Ti3C2Tx material through two-step etching method
  • Method for preparing polyhydroxyl functional group Ti3C2Tx material through two-step etching method

Examples

Experimental program
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Effect test

Embodiment 1

[0026] (1) Prepare 50ml of 50% potassium hydroxide alkaline solution, heat up to 200°C under nitrogen atmosphere, add 1g of Ti 3 AlC 2 Phase material, stirred for 6h, centrifuged at 4200rpm for 10min, washed with water to neutral wash to obtain pre-etched product A;

[0027] (2) Submerge the obtained pre-etching product A in 50 ml of HF aqueous solution, the mass fraction of HF is 40%, and stir and react under nitrogen atmosphere for 24 hours;

[0028] (3) After the reaction in step (2), the reaction solution was centrifuged at 4200 rpm for 10 minutes, washed with water until neutral, and then freeze-dried at -60°C for 24 hours. After drying, Ti 3 C 2 T x Material.

[0029] Depend on figure 1 It can be seen that the (002)(004)(110) peaks and the successful preparation of Ti 3 C 2 T x .

Embodiment 2

[0031] (1) Prepare 50ml of 40% potassium hydroxide alkaline solution, heat up to 150°C under nitrogen atmosphere, add 0.5g of Ti 3 AlC 2 phase material, stirred and reacted for 12 hours, centrifuged at 4200rpm for 10 minutes, washed with water to neutral washing to obtain pre-etched product A;

[0032] (2) Submerge the obtained pre-etching product A in 50 ml of HF aqueous solution, the mass fraction of HF is 40%, and stir and react under nitrogen atmosphere for 24 hours;

[0033] (3) After the reaction in step (2), the reaction solution was centrifuged at 4200 rpm for 10 minutes, washed with water until neutral, and then freeze-dried at -60°C for 24 hours. After drying, Ti 3 C 2 T x Material.

[0034] Depend on image 3 It can be seen that the successful stripping of Ti 3 AlC 2 , yielding Ti with a typical accordion-like structure 3 C 2 T x Material, Figure 4 It can be seen that Ti 3 C 2 T x Two-dimensional sheet structure (with folds).

Embodiment 3

[0036] (1) Prepare 50ml of 30% potassium hydroxide alkaline solution, heat up to 100°C under nitrogen atmosphere, add 0.5g of Ti 3 AlC 2 Phase material, stirred for 18 hours, centrifuged at 4200 rpm for 10 minutes, washed with water to neutral wash to obtain pre-etched product A;

[0037] (2) Submerge the obtained pre-etching product A in 50 ml of HF aqueous solution, the mass fraction of HF is 40%, and stir and react under nitrogen atmosphere for 24 hours;

[0038] (3) After the reaction in step (2), the reaction solution is centrifuged at 4200rpm for 10min, washed with water until neutral, and dried at a temperature of 60°C for 24h. After drying, Ti 3 C 2 T x Material.

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Abstract

The invention relates to the field of material science process technology synthesis and the field of electrochemical technology science, in particular to a preparation method of polyhydroxyl functional group Ti3C2Tx. The method comprises the steps that Ti3AlC2 powder is pre-etched with an alkaline solution as a pre-etching solvent to obtain a product A, the pre-etched product A is re-etched, through centrifuging, washing and drying, polyhydroxyl functional Ti3C2Tx is obtained, through a two-step method, pre-etching is conducted through the alkaline solution to peel part of Al atoms to occupy active sites, and then hydrofluoric acid etching is conducted to achieve the polyhydroxyl purpose. The Ti3C2Tx obtained by treatment through the step-by-step etching method has the high content of hydroxyl functional groups, and reactiveness and electrochemical performance of the Ti3C2Tx active sites are improved. The provided preparation method of the polyhydroxyl Ti3C2Tx has the characteristics of easy and fast operation, high synthesis efficiency, controllable process and low cost.

Description

technical field [0001] The present invention relates to the field of material science process technology synthesis and the field of electrochemical technology science, in particular to a polyhydroxy functional group Ti 3 C 2 T x method of preparation. Background technique [0002] With the rapid development of the world economy and the advancement of modern science and technology, the number of cars has increased sharply, which has brought great convenience to people and made great contributions to the development of human society. environmental challenges. People pay more and more attention to the improvement of energy conversion and storage equipment, and the development of new electrochemical energy storage devices has more and more important significance. Supercapacitors are new energy storage materials between capacitors and conventional batteries, and as one of the potential energy storage and power devices, they have been widely explored due to their excellent per...

Claims

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Application Information

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IPC IPC(8): C01B32/921
CPCC01B32/921C01P2002/72C01P2002/82C01P2004/03C01P2004/04C01P2006/40Y02E60/13
Inventor 王林谭禹田华朱开鑫张如娜李旺于志凤何云逸来媛楠
Owner YANSHAN UNIV
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