A method for constructing a tellurium-doped cobalt intercalated MXene

By inserting a cobalt layer into MXene and doping it with tellurium atoms, the problems of easy stacking and few active sites of MXene were solved, achieving high-efficiency electrocatalytic hydrogen evolution performance and simplifying the preparation process.

CN117623309BActive Publication Date: 2025-12-12QIQIHAR UNIVERSITY
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Patent Information

Application Number
CN202410023812.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-01-08
Publication Date
2025-12-12
Estimated Expiration
2044-01-08

AI Technical Summary

Technical Problem

MXenes are prone to stacking and have few reactive sites, which affects their electrocatalytic performance.

Method used

Tellurium-doped cobalt-intercalated MXenes were prepared by a simple synthesis method, including hydrothermal reaction and high-temperature calcination steps, by inserting a cobalt layer into MXenes and doping them with tellurium atoms.

Benefits of technology

The electrocatalytic performance of MXene was improved, resulting in excellent electrocatalytic hydrogen evolution performance. Moreover, the synthesis process is simple and the equipment requirements are not high.

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Abstract

The application relates to a construction method of tellurium-doped cobalt intercalated MXene. The purpose of the application is to solve the problems of easy stacking and few active sites of MXene, and provide a construction method of tellurium-doped cobalt intercalated MXene. The prepared MXene has excellent electrocatalytic hydrogen evolution performance. Method: taking cobalt chloride, V2AlC, hydrochloric acid and lithium fluoride as raw materials, a hydrothermal method and a calcination method are adopted to obtain high-efficiency tellurium-doped cobalt intercalated MXene, so as to provide a preparation method for improving the electrocatalytic hydrogen evolution performance of the existing MXene-based materials.
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Description

TECHNICAL FIELD

[0001] The application relates to a construction method of a tellurium-doped cobalt intercalated MXene. BACKGROUND

[0002] Electrocatalytic hydrogen evolution technology is a highly efficient new hydrogen production method that produces hydrogen from water decomposition under normal pressure and room temperature conditions using electrical energy. This technology promotes the decomposition of water into hydrogen and oxygen under the action of an electrocatalyst by applying a voltage to the electrode, achieving efficient utilization of water resources. This technology is valued for its high energy conversion efficiency, environmental friendliness, and use of electrical energy from renewable energy sources. Especially in addressing environmental problems and energy crises caused by traditional fossil fuel hydrogen production methods, electrocatalytic hydrogen evolution technology shows great potential. Currently, one of the focuses of this technology is the development of new and efficient electrocatalysts to achieve higher hydrogen production efficiency and lower energy consumption. With technological advancements and large-scale applications, electrocatalytic hydrogen evolution is expected to become one of the key technologies supporting future clean energy systems, providing strong impetus for low-carbon economic transformation.

[0003] MXene has attracted attention for its high electrical conductivity, high specific mass activity, good mechanical stability, rich surface functional groups, and structural adjustability, but its own problems of easy stacking and few active sites need to be improved. In the process of preparing MXene, cobalt intercalation treatment is carried out by adding cobalt chloride to prevent stacking, and by high-temperature calcination to introduce tellurium atom doping to provide rich electrochemical active sites, thereby improving the electrocatalytic performance, which has important research significance for solving energy pollution problems. SUMMARY

[0004] The purpose of the present application is to overcome the problems of MXene easy stacking and few reaction active sites, and to provide a simple, novel and high-yield construction method.

[0005] The construction method of the tellurium-doped cobalt intercalated MXene of the present application is completed according to the following steps:

[0006] (1) V2AlC, lithium fluoride and cobalt chloride are added to hydrochloric acid, and stirred at room temperature to make them fully dispersed;

[0007] (2) The dispersion system in (1) is transferred to a reaction kettle for hydrothermal reaction, and after the reaction is completed, the precipitate is washed with deionized water to a pH of 6, and the precipitate is placed in an oven for vacuum drying to obtain dried cobalt intercalated MXene;

[0008] (3) 0.1 grams of the dried material in step (2) and tellurium powder are placed in a tube furnace and calcined under N2 protection to obtain a tellurium-doped cobalt intercalated MXene material;

[0009] The mass of V2AlC in the step (1) is 0.5-1 gram, the mass of lithium fluoride is 0.5-1 gram, the mass of cobalt chloride is 40-100 milligrams, the volume of hydrochloric acid is 6-10 milliliters, and the stirring time is 8-12 hours;

[0010] The hydrothermal temperature in the step (2) is 150-200 degrees Celsius, the reaction time is 20-25 hours, the vacuum drying temperature is 30-60 degrees Celsius, and the drying time is 8-15 hours;

[0011] The mass of tellurium powder in the step (3) is 0.05-0.3 gram, the calcination temperature is 600-800 degrees Celsius, and the calcination time is 2-5 hours;

[0012] Compared with the prior art, the beneficial effects of the present application are: the present application constructs a tellurium-doped cobalt intercalated MXene, which can be obtained in a short time during the construction process. In addition, the synthesis of the material does not require complex equipment, and the prepared material has excellent electrocatalytic hydrogen evolution performance. BRIEF DESCRIPTION OF DRAWINGS

[0013] Figure 1 The scanning electron microscope image of the tellurium-doped cobalt intercalated MXene of Example 1;

[0014] Figure 2 The X-ray diffraction spectrum of the tellurium-doped cobalt intercalated MXene of Example 1 and the control group powder;

[0015] Figure 3 The X-ray photoelectron spectrogram of the tellurium-doped cobalt intercalated MXene of Example 1;

[0016] Figure 4 The electrocatalytic hydrogen evolution performance graph of the tellurium-doped cobalt intercalated MXene of Example 1; DETAILED DESCRIPTION

[0017] [ The technical solution of the present application is not limited to the following specific embodiments, and the following specific embodiments are only used to illustrate the present application and are not limited to the technical solution described in the examples of the present application. Those skilled in the art should understand that the present application can still be modified or replaced equivalently to achieve the same technical effect. As long as the use needs are met, it is within the protection scope of the present application.

[0018] The construction method of a tellurium-doped cobalt intercalated MXene of the present embodiment is completed according to the following steps:

[0019] (1) 0.8 grams of V2AlC, 0.8 grams of lithium fluoride and 40 milligrams of cobalt chloride are placed in 8 milliliters of hydrochloric acid, and stirred at room temperature for 10 hours to make them fully dispersed;

[0020] (2) The (1) is transferred to a reaction kettle at 180 degrees Celsius for 24 hours, and after the reaction is completed, the precipitate is washed with deionized water until the pH is 6, and the precipitate after the reaction is placed in a drying oven for vacuum drying at 45 degrees Celsius for 12 hours;

[0021] (3) 0.1 grams of the dried material in step (2) and 0.3 grams of tellurium powder are placed in a tube furnace and calcined at 600 degrees Celsius for 3 hours under N2 protection to obtain tellurium-doped cobalt intercalated MXene;

[0022] The application will be further described below in combination with the accompanying drawings and examples:

[0023] Figure 1 It is a scanning electron microscope image of the tellurium-doped cobalt intercalated MXene of Example 1. The tellurium-doped cobalt intercalated MXene is a handkerchief-shaped nanosheet with nanoparticles intercalated between layers.

[0024] Figure 2 It is a powder X-ray diffraction spectrum of the tellurium-doped cobalt intercalated MXene of Example 1. The diffraction peak appearing at 14.3° corresponds to the (002) crystal plane of MXene, proving that V2AlC is successfully etched, indicating that the product is tellurium-doped cobalt intercalated MXene.

[0025] Figure 3 It is an X-ray photoelectron spectrogram of the tellurium-doped cobalt intercalated MXene of Example 1. From the C 1s spectrum of the tellurium-doped cobalt intercalated MXene, it can be seen that the diffraction peaks appearing at 283.3, 284.8, 285.9 and 289.1 eV correspond to V-C, C-C, C=C and O-C-C. From the V 2p spectrum of the tellurium-doped cobalt intercalated MXene, it can be seen that the diffraction peaks appearing at 515.5, 517.4, 523.1 and 524.9 eV correspond to V-C and C-O. From the Co 2p spectrum of the tellurium-doped cobalt intercalated MXene, it can be seen that the diffraction peaks appearing at 780.5, 788.3, 793.9 and 800.9 eV correspond to Co 0 , Co 2+ , Co 3+ and Co 0 . From the Te 3d spectrum of the tellurium-doped cobalt intercalated MXene, it can be seen that the diffraction peaks appearing at 575.7, 577.7, 580.5, 583.4 and 586.6 eV correspond to Te 0 , TeO x and Te-metal, and the above results show that the product is tellurium-doped cobalt intercalated MXene.

[0026] Figure 4A hydrogen evolution performance chart of the tellurium-doped cobalt intercalated MXene of Example 1. In a 1 molar potassium hydroxide solution, the overpotential is 81 millivolts at a current density of 10 milliampere per square centimeter, indicating that the material has excellent electrocatalytic hydrogen evolution performance.

Claims

1. A method for constructing tellurium-doped cobalt intercalated MXene, the method being completed according to the following steps: (1) adding V 2 AlC, lithium fluoride and cobalt chloride into hydrochloric acid, stirring at room temperature to make them fully dispersed; (2) transferring the dispersion system in (1) into a reaction kettle to perform hydrothermal reaction, naturally cooling after the reaction is completed, washing the precipitate with deionized water until it is neutral, and vacuum drying the precipitate in an oven to obtain dried cobalt intercalated MXene; (3) placing 0.1 g of the dried material in step (2) and tellurium powder in a tube furnace, calcining under N 2 protection to obtain tellurium-doped cobalt intercalated MXene material.

2. The method of claim 1, wherein the method comprises: In the step (1), the mass of V 2 AlC is 0.5-1 g, the mass of lithium fluoride is 0.5-1 g, the mass of cobalt chloride is 40-100 mg, the volume of hydrochloric acid is 6-10 ml, and the stirring time is 8-12 hours. ​ 3. The method of claim 1, wherein the method comprises: In the step (2), the hydrothermal temperature is 150-200 DEG C, the reaction time is 20-25 hours, the vacuum drying temperature is 30-60 DEG C, and the drying time is 8-15 hours. ​ 4.The method of claim 1, wherein the method comprises: In the step (3), the mass of tellurium powder is 0.05-0.3 g, the calcination temperature is 600-800 DEG C, and the calcination time is 2-5 hours.

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