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Method for instantaneous high-temperature synthesis of transition metal carbide nano array by taking oxide as template

A transition metal and nano-array technology, applied in electrolysis process, electrolysis components, electrodes, etc., can solve the problems of long process time, difficult control of carbide morphology and size, high energy consumption, etc., and achieve a unique level, electron migration and transmission The effect of convenient quality and high specific surface area

Active Publication Date: 2022-06-03
YANGTZE DELTA REGION INST OF UNIV OF ELECTRONICS SCI & TECH OF CHINE HUZHOU
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Problems solved by technology

[0013] Aiming at the above-mentioned prior art, the present invention provides a method for instantaneous high-temperature synthesis of transition metal carbide nanoarrays using oxides as templates to solve the problems of long process time, high energy consumption, and the appearance of carbides in the existing preparation methods. And the size is not easy to control and other issues

Method used

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  • Method for instantaneous high-temperature synthesis of transition metal carbide nano array by taking oxide as template
  • Method for instantaneous high-temperature synthesis of transition metal carbide nano array by taking oxide as template
  • Method for instantaneous high-temperature synthesis of transition metal carbide nano array by taking oxide as template

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Embodiment 1

[0044] A method for instantaneous high-temperature synthesis of molybdenum carbide nanoarrays using oxides as templates, comprising the following steps:

[0045] (1) Molybdenum oxide (MoO) with nano-array structure was grown on carbon cloth substrate by hydrothermal method X ), the hydrothermal reaction precursor solution 5mL HNO 3 , 70mL H 2 O, 2.5g (NH 4 ) 6 Mo 7 O 24 ·4H 2 After the O was mixed evenly, carbon was placed in it and reacted at 150 °C for 10 min, and then the carbon cloth was taken out, washed, and dried at 60 °C to obtain molybdenum oxide nanoarrays;

[0046](2) Using the molybdenum oxide nanoarrays supported on carbon cloth as the substrate, the vertical graphene nanosheets (VG) were deposited on the surface by plasma-assisted chemical vapor deposition method, and the process parameters were: Ar, H 2 and CH 4 The flow rates were 20, 10 and 7sccm, the deposition time was 12min, the temperature used was 600°C, and the power of the plasma equipment was 6...

Embodiment 2

[0049] A method for instantaneous high-temperature synthesis of cobalt carbide nanoarrays using oxide as a template, comprising the following steps:

[0050] (1) Cobalt tetroxide (Co3O4) with nano-array structure was grown on carbon cloth substrate by hydrothermal method 3 O 4 ), the hydrothermal reaction precursor solution 70mL deionized water, 2g Co(NO 3 ) 2 , 0.7g NH 4 F. 0.25g Co(NH 2 ) 2 After mixing evenly, the carbon was placed in it and reacted at 115°C for 9 hours, then the carbon cloth was taken out, washed, dried at 60°C, and then calcined at 350°C for 2 hours in an air atmosphere to obtain cobalt oxide nanoarrays;

[0051] (2) Using the cobalt tetroxide nanoarrays supported on carbon cloth as the substrate, the vertical graphene nanosheets (VG) were deposited on the surface by plasma-assisted chemical vapor deposition method, and the process parameters were: Ar, H 2 and CH 4 The flow rates were 10, 5 and 1 sccm, the deposition time was 20 min, the temperatur...

Embodiment 3

[0054] A method for instantaneous high-temperature synthesis of tungsten carbide nanoarrays using oxide as a template, comprising the following steps:

[0055] (1) Preparation of tungsten oxide (WO) by electrodeposition on clean carbon cloth 3 ) seed layer, 0.8 g of sodium tungstate and 2.7 mL of hydrogen peroxide were added to 200 mL of deionized water, the pH was adjusted to 1.2 by adding perchloric acid, and a silver / silver chloride (Ag / AgCl) reference electrode was used. , through constant voltage (-0.7V) deposition for 400s, the carbon cloth loaded with seeds was obtained;

[0056] (2) 2.5g oxalic acid, 3g Na of the hydrothermal reaction precursor 2 WO 4 Dissolve in deionized water to form a clear solution, then add 275 μL of concentrated nitric acid, and dilute the solution to 350 mL, then take 55 mL of the solution and add 4 g of ammonium sulfate to it, then stir until clarification, then put into the reaction kettle, and load the The seeded carbon cloth was also put...

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Abstract

The invention discloses a method for instantaneous high-temperature synthesis of a transition metal carbide nano array by using an oxide as a template, which comprises the following steps: (1) growing a transition metal oxide with a nano array structure on a substrate to obtain a transition metal oxide nano array; (2) taking the transition metal oxide nano array as a substrate, and depositing a graphene nanosheet on the surface of the transition metal oxide nano array; and (3) treating the graphene nanosheets loaded on the metal oxide template under the conditions that the current is 0-20 A and the voltage is 40-80 V, so that the graphene reacts with the metal oxide, the treatment time is 20-100 ms, and the metal carbide with the array morphology is obtained. By reasonably constructing the structure of the transition metal carbide catalyst and designing the specific morphology of the nano material, the number of active sites on a given electrode is increased, so that the activity of an electrocatalyst system is improved.

Description

technical field [0001] The invention relates to the preparation of transition metal carbide nanomaterials, in particular to a method for instantaneous high temperature synthesis of transition metal carbide nanometer arrays using oxides as templates. Background technique [0002] The transition group elements mainly refer to the elements from groups IIIB to VIII of the periodic table, and their biggest feature is that the outermost electron orbitals are in an unfilled unsaturated state. This unique electronic structure endows transition elements and their compounds with excellent functional properties. Common transition metal compounds include sulfides, phosphides, and carbides. Due to their excellent chemical stability, tunable electronic structure, high electrical conductivity, and variety of species, transition metal carbides are often used in catalytic reactions such as water electrolysis. [0003] For catalytic reactions, the activity of electrocatalyst systems can usu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B11/075C25B1/04C25D9/04
CPCC25B11/075C25B1/04C25D9/04Y02E60/36
Inventor 张永起李晨夏新辉
Owner YANGTZE DELTA REGION INST OF UNIV OF ELECTRONICS SCI & TECH OF CHINE HUZHOU
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