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Molybdenum phosphide-based polycrystalline block, preparation method and application thereof

A crystal block and molybdenum-based technology, applied in the field of electrocatalytic hydrogen evolution, can solve the problems of complex procedures and difficult preparation, and achieve the effects of abundant sources, simple equipment and process, and low price.

Pending Publication Date: 2021-11-16
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The preparation of MoP materials with specific micro-nano structures by the above chemical synthesis method mainly prepares molybdenum oxide / molybdenum salt precursors through solvothermal reaction, and then performs high-temperature phosphating reaction in reducing atmosphere to prepare MoP-based materials: the synthesis process involves solvothermal reaction , cleaning, drying, high-temperature heat treatment in reducing atmosphere, and phosphating reaction, etc., the process is complicated and the controllable preparation is difficult; at the same time, high-temperature phosphating treatment requires the use of H 2 、PH 3 and elemental phosphorus sources, etc., and discharge toxic wastewater and waste residues and discharge NH during the synthesis process 3 、PH 3 、H 2 Toxic / dangerous gases such as incomplete reaction

Method used

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  • Molybdenum phosphide-based polycrystalline block, preparation method and application thereof
  • Molybdenum phosphide-based polycrystalline block, preparation method and application thereof
  • Molybdenum phosphide-based polycrystalline block, preparation method and application thereof

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Embodiment 1

[0033] This embodiment provides a method for preparing a MoP polycrystalline solid-state reaction combined with plasma activation sintering, which includes the following steps:

[0034] 1) Taking the elemental Mo powder and P powder with a purity of 99.9% as raw materials, weighing and grinding and mixing according to the MoP stoichiometric ratio to obtain a reactant;

[0035] 2) The reactant obtained in step 1) was vacuum-sealed in a quartz glass tube after being pressed into tablets, and placed in a muffle furnace at 750°C for 48 hours to obtain a reaction product;

[0036] 3) After the polycrystalline powdery product obtained in step 2) is further ground and refined, a dense polycrystalline product is obtained under the conditions of 950° C., 80 MPa, and 10 minutes of heat preservation by using plasma activation sintering;

[0037] 4) The surface of the plasma-activated sintered MoP polycrystalline block can be directly used for electrochemical hydrogen evolution and oxygen...

Embodiment 2

[0041] This embodiment provides a MoP 1-y A method for preparing a polycrystalline solid-state reaction combined with plasma activation sintering, which comprises the following steps:

[0042] 1) Using elemental Mo powder and P powder with a purity of 99.9% as raw materials, according to MoP 1-y (y=0.01) stoichiometric ratio is weighed and ground and mixed to obtain reactants;

[0043] 2) The reactant obtained in step 1) was vacuum-sealed in a quartz glass tube after being pressed into tablets, and placed in a muffle furnace at 750°C for 48 hours to obtain a reaction product;

[0044] 3) After the polycrystalline powdery product obtained in step 2) is further ground and refined, a dense polycrystalline product is obtained under the conditions of 950° C., 80 MPa, and 10 minutes of heat preservation by using plasma activation sintering;

[0045] 4) Plasma activated sintered MoP 0.99 The surface of the polycrystalline block can be directly used for electrochemical hydrogen evo...

Embodiment 3

[0047] This embodiment provides a MoP 1-y Method for the preparation of polycrystalline blocks by solid-state reaction combined with plasma-activated sintering, according to MoP 0.97 (y=0.03) stoichiometric ratio, all the other steps are with embodiment 2.

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Abstract

The invention discloses a molybdenum phosphide-based polycrystalline block, a preparation method and application thereof. The method comprises the following steps: by taking simple substances as raw materials, weighing and uniformly mixing according to a stoichiometric ratio of MoP1-y or Mo1-xAxP1-yBy to obtain a reactant, wherein A is a doping element at the lattice position of Mo and comprises one or more of Nb, Fe, Co and Ni, B is a doping element at the lattice position of P and comprises one or more of S, Se and Te, x and y are the content of the doping elements, x is equal to 0-0.06, and y is equal to 0-0.07; and then carrying out solid-phase reaction under a vacuum condition or an inert condition to obtain a polycrystalline powdery product, and carrying out pressure sintering to obtain the product. According to the invention, the material is directly prepared from elementary substance raw materials through two steps of solid-phase reaction and pressure sintering, is free of by-products, simple in equipment and process, environment-friendly and low in cost, can be directly used as a working electrode for electro-catalytic hydrogen evolution and oxygen evolution, and does not need subsequent treatment.

Description

technical field [0001] The invention relates to the technical field of water electrolysis and electrocatalytic hydrogen evolution in the chlor-alkali industry, in particular to a molybdenum phosphide-based polycrystalline block and its preparation method and application. Background technique [0002] Hydrogen energy has significant advantages such as cleanliness, zero emissions, and high combustion calorific value. Its energy density is as high as 142,500KJ / mol, which is three times that of gasoline (46,100KJ / mol), and it is the next generation of new energy. Hydrogen is an extremely important industrial raw material. It is widely used in petrochemical, electronic, metallurgical, food processing, new energy vehicles, aerospace, medical and other fields, and its uses are extremely broad. At present, the industrial production of hydrogen mainly includes hydrogen production by reforming fossil raw materials, hydrogen production by catalytic thermal decomposition of methane / meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/19C25B11/091C25B1/04
CPCB01J27/19C25B11/04C25B1/04B01J35/33Y02E60/36
Inventor 柳伟雷雨竹何大平唐新峰
Owner WUHAN UNIV OF TECH