Preparation method of ultra-large-size titanium carbide nanosheet with wrinkle structure and application of nanosheet in electrochemical energy storage

A technology of ultra-large size and nano-sheets, applied in the application of electrochemical energy storage, the field of preparation of ultra-large-sized titanium carbide nano-sheets, can solve problems such as hindering electrolyte transmission, achieve strong operability, increase specific surface area, and increase channels Effect

Active Publication Date: 2019-06-14

NANJING UNIV OF POSTS & TELECOMM

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AI-Extracted Technical Summary

Problems solved by technology

However, to maximize the use of Ti 3 C 2 There are still some challenges to be overcome as electrode materials for supercapacitors

For exampl...

Method used

As can be seen from Fig. 8, the electrode mass specific capacitance prepared by ultra-thin Ti3C2 nanosheets is 286.2 F g-1, and the electrode mass specific capacitance prepared by ultra-large size Ti3C2 nanosheets...

Abstract

The invention discloses a preparation method of an ultra-large-size titanium carbide nanosheet with a wrinkle structure. The preparation method comprises the following steps of firstly, preparing an ultra-thin Ti3C2 nanosheet, and then carrying out a hydrothermal reaction on the ultra-thin Ti3C2 nanosheet and Na2S.9H2O to prepare the ultra-large-size Ti3C2 nanosheet with a wrinkle structure, wherein an electrode is prepared on the basis through a vacuum suction filtration technology and the energy storage performance of the electrode is researched. The titanium carbide nanosheet disclosed by the invention has the wrinkle structure, so that the specific surface area is enlarged, and the migration channels of electrolyte ions are increased; the titanium carbide nanosheet has an ultra-large size, and the microscopic size is larger than 10 mm; and the titanium carbide flexible electrode prepared by the vacuum suction filtration technology has the electrochemical energy storage property superior to that of the electrode prepared from the ultrathin titanium carbide nanosheet, the preparation can be completed under the normal-temperature and normal-pressure conditions, and the operabilityis high.

Application Domain

Hybrid capacitor electrodesHybrid/EDL manufacture

Technology Topic

IonElectrochemical energy storage +11

Image

Examples

Experimental program(4)

Example Embodiment

[0031] Example 1: Preparation of ultra-large titanium carbide nanosheets with pleated structure

[0032] Step 1: Ultra-thin Ti 3 C 2 Preparation of nanosheets

[0033] (1) Add 1 g LiF to 20 mL 9 M HCl, magnetically stir until LiF is completely dissolved;

[0034] (2) To prevent local overheating, slowly add 1 g Ti 3 AlC 2;

[0035] (3) Put the mixture in the reactor at 60 o React for 72 h under C;

[0036] (4) Centrifuge the product (3500 rpm/5 min), wash 6 times with deionized water, wash 2 times with ethanol, and dry in vacuum;

[0037] (5) Weigh 0.1 g of the dried product, disperse it in 10 mL of deionized water, and sonicate it for 4 h at 600 W;

[0038] (6) Centrifuge the sonicated product (3500 rpm, 1 h), and the upper liquid is the desired substance.

[0039] figure 1 For ultra-thin Ti 3 C 2 SEM pictures of nanosheets, figure 2 For ultra-thin Ti 3 C 2 TEM picture of the nanosheet.

[0040] Step 2: Super large size Ti with fold structure 3 C 2 Preparation of nanosheets

[0041] (1) 1.4410 g Na 2 S·9H 2 O (6 mmol) was added to 11.125 mL ultrapure water under Ar atmosphere, and stirred until Na 2 S·9H 2 O completely dissolved;

[0042] (2) 0.875 mL ultra-thin Ti 3 C 2 Add nanosheets (0.15 mmol) to (1) and stir for 15 min under Ar atmosphere until they are uniform;

[0043] (3) Put the mixed reactants in step 2 at 180 o Reaction for 12 h under C;

[0044] (4) Centrifuge the product in step 3 (10000 rpm, 10 min), wash with ultrapure water 3 times and ethanol wash once.

[0045] image 3 It is an oversized Ti with a corrugated structure 3 C 2 SEM pictures of nanosheets, Figure 4 It is an oversized Ti with a corrugated structure 3 C 2 TEM picture of the nanosheet.

Example Embodiment

[0046] Embodiment 2: Ti 3 C 2 Preparation of flexible film electrode

[0047] The super-sized Ti with a corrugated structure 3 C 2 Nanosheets are uniformly dispersed by ultrasonic, and Ti is prepared by vacuum filtration technology 3 C 2 Thin-film electrode, and dried at room temperature for 6 h.

[0048] Figure 5 Ti 3 C 2 Front SEM photo of the flexible electrode, Image 6 Ti 3 C 2 SEM photo of the section of the flexible electrode.

Example Embodiment

[0049] Example 3: Ultra-thin Ti 3 C 2 Electrodes made of nanosheets and super-sized Ti with pleated structure 3 C 2 Cyclic Voltammetric Test of Electrodes Prepared by Nanosheets

[0050] 1. Working electrode: ultra-thin Ti 3 C 2 Electrode prepared by nanosheets (original size: 1.8 cm×0.8 cm; immersion size: 0.9 cm×0.8 cm, mass: 0.0035 g); reference electrode: Ag/AgCl; counter electrode: Pt sheet (1 cm×1 cm) ; Electrolyte: 0.5 MH 2 SO 4; CV potential window: -0.3 V~0.3 V; immerse the membrane electrode in the electrolyte, let it stand for 10 min, and activate it until the curve completely coincides with the scan rate of 100 mV/s;

[0051] 2. Working electrode: oversized Ti with corrugated structure 3 C 2 Electrodes prepared by nanosheets (original size: 1.8 cm×0.8 cm; immersion size: 0.9 cm×0.8 cm, mass: 0.0035 g); reference electrode: Ag/AgCl; counter electrode: Pt sheet (1cm×1 cm); Electrolyte: 0.5 MH 2 SO 4; CV potential window: -0.3 V~0.3 V. The membrane electrode was immersed in the electrolyte, and allowed to stand for 10 min. At a scanning rate of 100 mV/s, it was activated until the curves completely overlapped.

[0052] From Figure 7 It can be seen that the ultra-thin Ti 3 C 2 The mass specific capacitance of the electrode prepared by the nanosheet is 241.67 F g -1 , Oversized Ti with pleated structure 3 C 2 The electrode mass specific capacitance prepared by the nanosheet is 319.84 F g -1 , Oversized Ti with pleated structure 3 C 2 Electrochemical performance of electrodes prepared from nanosheets is better than ultra-thin Ti 3 C 2 Electrodes made of nanosheets.

PUM

Property	Measurement	Unit
Mass specific capacitance	241.67	1/fg
Mass specific capacitance	319.84	1/fg
Mass specific capacitance	286.2	1/fg

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