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Preparation method of Ni0. 85Se@NC electro-catalytic material

A technology of electrocatalytic materials and nanosheets, applied in chemical instruments and methods, physical/chemical process catalysts, electrodes, etc., can solve problems such as phase and electronic structure regulation

Pending Publication Date: 2020-12-29
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The present invention provides Ni 0.85 The preparation method of Se@NC electrocatalytic materials solves the current phase and electronic structure control problems of such materials

Method used

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  • Preparation method of Ni0. 85Se@NC electro-catalytic material
  • Preparation method of Ni0. 85Se@NC electro-catalytic material
  • Preparation method of Ni0. 85Se@NC electro-catalytic material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] This embodiment provides a method for preparing nickel-based metal-organic framework nanosheets, which specifically includes the following steps:

[0051] Preparation of Ni-MOF nanosheets: First, 0.145g (0.5mmol) Ni(NO 3 ) 2 ·6H 2 O, 0.056g (0.5mmol) DABCO, 0.105g (0.5mmol) H 3 BTC and 1 g of PVP were dissolved in DMF (10 mL) solution. The solution was stirred at room temperature at a stirring speed of 600 rpm for 30 minutes, then transferred to a 25 mL reaction axe, and placed in an oven at 120° C. for 24 hours after packaging. After cooling to room temperature naturally, centrifuge three times with DMF and methanol to remove unreacted residues and solvent molecules to obtain light green Ni-MOF powder. Finally, the activated Ni-MOF nanosheets were obtained by vacuum drying at 120 °C for 12 h.

[0052] figure 1 For the XRD pattern of the Ni-MOF nanosheets prepared in Example 1, it can be seen that the X-ray diffraction pattern of the synthesized Ni-MOF is in good ...

Embodiment 2

[0059] This embodiment provides a method for preparing Ni@NC, which specifically includes the following steps:

[0060] Take 100 mg of green Ni-MOF nanosheets, grind them in a mortar for 10 min, transfer them to a square porcelain boat in a tube furnace, and heat them at 5 °C min under an argon atmosphere. -1 The heating rate was heated from room temperature to 600 °C, and maintained for 2 h, and the black powder was obtained after waiting for natural cooling, which was recorded as Ni@NC.

[0061] Figure 4 The TEM image of the Ni@NC electrocatalytic material with core-shell structure prepared for Example 2 shows that the surface of the synthesized nanoflakes becomes rough, and many uniformly distributed nanoparticles appear.

[0062] Figure 5 The XRD pattern of the Ni@NC electrocatalytic material with core-shell structure prepared in Example 2 proves that the synthesized material matches well with Ni (PDF#04-0850) and has a high phase purity.

Embodiment 3

[0064] This example provides Ni 0.85 The preparation method of Se@NC specifically includes the following steps:

[0065] (1)NiSe 2 Preparation of @NC: Prepare and weigh 50 mg of black powder Ni@NC and 200 mg of selenium powder in a mortar, mix them evenly, transfer them to a square porcelain boat in a tube furnace, and heat them at 5°C min under an argon atmosphere. -1 The heating rate is from room temperature to 350 ° C, the reaction is maintained for 2 h, and the temperature is naturally lowered to obtain nitrogen-doped carbon-coated nickel diselenide nanoparticles, named NiSe 2 @NC

[0066] (2)Ni 0.85 Preparation of Se@NC: The obtained 50mg NiSe 2 @NC is placed in a square porcelain boat in a tube furnace, and the tube furnace is heated at 800 °C for 2 hours, and after cooling down to room temperature, nitrogen-doped carbon-coated nickel selenide nanoparticles are obtained, denoted as Ni 0.85 Se@NC.

[0067] Figure 6 It is the core-shell structure NiSe prepared in e...

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Abstract

The invention provides a preparation method of a Ni0. 85Se@NC electro-catalytic material, which comprises the following steps: S1, preparing a nickel-based metal organic framework nanosheet by solvothermal reaction, and marking as Ni-MOF, namely [Ni(HBTC) (DABCO)3DMF]; S2, heating and annealing the nickel-based metal organic framework nanosheet in a programmed heating manner, and naturally coolingto obtain nitrogen-doped carbon-coated nickel nanoparticles named as Ni@NC; S3, uniformly mixing the Ni@NC with commercial selenium powder, heating and annealing in a programmed heating manner, and naturally cooling to obtain nitrogen-doped carbon-coated nickel diselenide nanoparticles which are recorded as NiSe2@NC; and S4, enabling the NiSe2@NC to be subjected to high-temperature calcination for 2h at the temperature of 750 DEG C to 850 DEG C, and preparing and marking nitrogen-doped carbon-coated nickel selenide nano particles as Ni0.85Se@NC. Compared with the prior art, the method provided by the invention has the advantages and positive effects that a controllable method for phase change from nickel selenide of an orthorhombic system to nickel selenide of a hexagonal phase is provided, and guidance is provided for synthesis and optimization of a nickel selenide material phase.

Description

technical field [0001] The invention belongs to the field of synthesis of new energy nanomaterials and electrochemical technology, in particular, relates to Ni 0.85 Preparation method of Se@NC electrocatalytic material. Background technique [0002] Electrochemical hydrolysis technology has broad application prospects in the sustainable storage, conversion, and delivery of hydrogen energy, which mainly relies on the thermodynamic and kinetic parameters of the two half-reactions (hydrogen evolution reaction and oxygen evolution reaction). Although Pt-based and Ru / Ir-based electrocatalysts are effective in lowering the reaction energy barrier and enhancing water splitting efficiency, their limited earth abundance and high market price severely hinder their widespread application. Therefore, efforts have been made to find advanced alternatives to noble metal catalysts. Transition metal chalcogenides are promising electrocatalysts for full hydrolysis due to their abundant rese...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C25B1/04C25B11/06
CPCB01J27/24C25B1/04B01J35/33B01J35/396Y02E60/36
Inventor 孙道峰黄招娣戴昉纳
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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