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Nanosheet-nanorod coupled three-dimensional composite Ni-Co modified molybdenum carbide electrocatalysis hydrogen production catalyst and preparation method thereof

A technology of composite materials and nanorods, applied in the field of electrocatalytic hydrogen production, to achieve the effects of simple process operation, accelerated transfer rate, and mature and stable synthesis technology

Active Publication Date: 2018-12-07
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Many researchers have carried out in-depth research on molybdenum carbide-based electrocatalytic materials from the modulation of crystal form, the regulation of microscopic morphology, the doping of heteroatoms, and the combination with carbon-based materials with excellent electrical conductivity. Although they have shown A certain degree of performance improvement, but there is still a huge room for performance improvement

Method used

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  • Nanosheet-nanorod coupled three-dimensional composite Ni-Co modified molybdenum carbide electrocatalysis hydrogen production catalyst and preparation method thereof
  • Nanosheet-nanorod coupled three-dimensional composite Ni-Co modified molybdenum carbide electrocatalysis hydrogen production catalyst and preparation method thereof
  • Nanosheet-nanorod coupled three-dimensional composite Ni-Co modified molybdenum carbide electrocatalysis hydrogen production catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1) Preparation of catalyst:

[0033] a) 2.1g ammonium heptamolybdate tetrahydrate ((NH 4 ) 7 Mo 7 o 24 4H 2O, denoted as AM) was dissolved in 60mL nitric acid aqueous solution, wherein the volume ratio of the solution was: 65% concentrated nitric acid / deionized water=1 / 5; after being completely dissolved, the clear solution was transferred to a 100mL polytetrafluoroethylene reaction kettle , sealed and placed in a homogeneous reactor, and reacted at 200°C for 20h. The solid product obtained by filtration was alternately washed several times with deionized water and absolute ethanol until the washing liquid was neutral, and then dried in an oven at 80°C overnight to obtain off-white MoO 3 Nanorod precursors.

[0034] b) Take 930mg nickel acetate (Ni(CH 3 COO) 2 ) and 97.5mg cobalt chloride (CoCl 2 ·6H 2 O) metal salt is dissolved in the mixed solution of 100ml water and ethanol, fully dissolves; Wherein, the volume ratio of water and ethanol is 1:1, then adds t...

Embodiment 2

[0041] Get 1026mg nickel acetate (Ni(CH 3 COO) 2 ) Metal salt is dissolved in the mixed solution of 100ml water and ethanol, fully dissolves; Wherein, the volume ratio of water and ethanol is 1:1, then add the MoO of 100mg 3 The nanorod precursor was ultrasonicated at room temperature for 30 minutes to form a uniformly dispersed suspension. The suspension was placed in a 90°C water bath for 6 hours. After the reaction was completed, it was cooled to room temperature and allowed to stand overnight. After filtering, washing and drying, a solid powder sample was obtained. . Finally, the solid powder is placed in a muffle furnace and calcined at 500°C for 2 hours to obtain the desired Ni / MoO 3 Precursor.

[0042] Prepare Ni / MoO as above 3 As a precursor, carbonization is carried out according to the temperature-programmed reaction process described in the catalyst preparation step b) in Example 1, and the three-dimensional nanocomposite structure Ni / β-Mo 2 C catalyst.

[004...

Embodiment 3

[0046] Get 1146mg nickel acetate (Ni(CH 3 COO) 2 ) and 214mg cobalt chloride (CoCl 2 ·6H 2 O) metal salt is dissolved in the mixed solution of 100ml water and ethanol, fully dissolves; Wherein, the volume ratio of water and ethanol is 1:1, then adds the MoO of 100mg 3 The nanorod precursor was ultrasonicated at room temperature for 30 minutes to form a uniformly dispersed suspension. The suspension was placed in a 90°C water bath for 6 hours. After the reaction was completed, it was cooled to room temperature and allowed to stand overnight. After filtering, washing and drying, a solid powder sample was obtained. . Finally, the solid powder is placed in a muffle furnace and calcined at 500°C for 2 hours to obtain the desired Ni 0.66 co 0.34 / MoO 3 Precursor.

[0047] Ni was prepared as above 0.66 co 0.34 / MoO 3 As a precursor, carbonization is carried out according to the temperature-programmed reaction process described in the catalyst preparation step b) in Example ...

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Abstract

The invention discloses a nanosheet-nanorod coupled three-dimensional composite Ni-Co modified molybdenum carbide electrocatalysis hydrogen production catalyst and a preparation method thereof. The catalyst is a nanorod structure, and the nanorod is covered with a plicated nanosheet structure. In addition, bimetal Ni and Co are uniformly dispersed on the surface of the catalyst, and the molar ratio of the metal Ni to Co is 1: 0-1:1. The preparation method comprises the following steps; using MoO3 nanorod as a supporting network, adding nickel acetate and cobalt salt and fully stirring to forma suspension; placing the above suspension into water bath of 60-90 DEG C and stirring intensely for 4-7 h, standing overnight, filtering, washing and drying, and roasting in the air atmosphere of 450-550 DEG C. By the surface / interfacial effect between the molybdenum carbide material and loaded metal and based on the morphology features of the material itself, high dispersion of the metal Ni andCo is realized, and the catalytic active site is fully exposed. Meanwhile, with the strong interaction between the molybdenum carbide substrate and the loaded metal, stability of the catalytic material is effectively enhanced.

Description

technical field [0001] The invention belongs to the technical field of electrocatalytic hydrogen production, and in particular relates to a nanosheet-nanorod three-dimensional composite structure Ni-Co / MoC x Electrocatalytic hydrogen production catalyst and preparation method thereof. Background technique [0002] Hydrogen energy is an ideal clean energy carrier with great development value and research significance. Its energy density is high, and its calorific value is much higher than that of fossil fuels, chemical fuels and biofuels. It has the advantages of concentrated heat energy and small heat loss, which can meet the needs of human production and life. The development of hydrogen energy is of great significance and is a driving force. A major move in the progress of human civilization. Hydrogen production by electrolysis of water is an effective way to produce hydrogen energy, and the research and development of efficient and stable HER catalysts has become a rese...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/22C25B1/04C25B11/06
CPCC25B1/04C25B11/04B01J27/22B01J35/33Y02E60/36
Inventor 石川张晓陈冰冰
Owner DALIAN UNIV OF TECH
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