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Three-dimensional orderly macroporous ferronickel phosphide material and preparation and application thereof

A three-dimensional ordered, phosphide technology, applied in the direction of phosphides, phosphorus compounds, chemical instruments and methods, etc., can solve the problem that catalyst materials cannot be fully and effectively used, the growth sites of nanosheets cannot be effectively controlled, and pores cannot be obtained Structure and other issues, to achieve the effect of good stability, high specific surface area, large pore volume ratio

Active Publication Date: 2019-02-12
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method cannot effectively control the growth site of the nanosheets, and it is easy to cause the accumulation of the nanosheets, so that it is impossible to obtain a regular and ordered pore structure for material transfer.
In the process of electrocatalytic water splitting, the diffusion resistance of the substance increases, so that the catalyst material cannot be fully and effectively utilized

Method used

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  • Three-dimensional orderly macroporous ferronickel phosphide material and preparation and application thereof
  • Three-dimensional orderly macroporous ferronickel phosphide material and preparation and application thereof
  • Three-dimensional orderly macroporous ferronickel phosphide material and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Synthesis of 3DOM NiFe-P

[0046] (1) Preparation of PMMA colloidal crystals

[0047] Add 300ml of deionized water to a 500ml round bottom flask, then put it into an oil bath, the temperature of the oil bath is 70°C, the rotation speed is 400 rpm, and nitrogen protection gas is introduced at the same time. After the temperature stabilized, add 80 mg of potassium persulfate solid, add 25 ml of methyl methacrylate (MMA) after the solid dissolves, and react for 1.5 hours under the protection of a nitrogen atmosphere to obtain a monodisperse polymethyl methacrylate with a spherical diameter of 300 nm. (PMMA) microspheres white emulsion. After the reaction, the product is centrifuged and washed to remove impurities. The PMMA microsphere emulsion obtained by washing is divided into 10ml glass beakers, and then the above beakers are placed in a water bath at 80° C. to evaporate and remove water to obtain orderly arranged PMMA solids.

[0048] (2) 3DOM NiFeO x preparation o...

Embodiment 2

[0058] Using the 3DOM NiFe-P material obtained in Example 1 as a hydrogen evolution catalyst to prepare a working electrode, the specific steps are as follows:

[0059] The electrochemical performance was tested in a three-electrode system electrolytic cell. The working electrode was a glassy carbon electrode loaded with 3DOM NiFe-P catalyst material, the counter electrode was a carbon rod, and the reference electrode was a saturated calomel electrode. Electrocatalytic performance in N 2 Tested in saturated 1M KOH solution. The sweep speed of LSV test is 2mV s –1 . The experimental test temperature is 25±2°C.

[0060] The preparation method of the working electrode: use an analytical balance to weigh 4 mg of electrocatalyst and use a pipette gun to draw 80 μl of 5wt% Nafion solution and disperse it into 1 ml of a mixed solution of deionized water and ethanol with a volume ratio of 4:1, and uniformly disperse in an ultrasonic instrument to form For the suspension, take 5 μl...

Embodiment 3

[0066] Synthesis method of 3DOM NiFe-P:

[0067] (1) Preparation of PMMA colloidal crystals

[0068] Add 300ml of deionized water to a 500ml round bottom flask, then put it into an oil bath, the temperature of the oil bath is 70°C, the rotation speed is 400 rpm, and nitrogen protection gas is introduced at the same time. After the temperature stabilized, add potassium persulfate solid, add methyl methacrylate (MMA) (the molar ratio of MMA and potassium persulfate is 1:0.001) after the solid dissolves, react under nitrogen atmosphere protection for 2 hours, obtain the A white emulsion of dispersed polymethylmethacrylate (PMMA) microspheres. After the reaction, the product is centrifuged and washed to remove impurities. The PMMA microsphere emulsion obtained by washing is divided into 10ml glass beakers, and then the above beakers are placed in a water bath at 80° C. to evaporate and remove water to obtain orderly arranged PMMA solids.

[0069] (2) 3DOM NiFeO x preparation o...

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Abstract

The invention relates to a three-dimensional orderly macroporous ferronickel phosphide material and preparation and application thereof. The material preparation process comprises the steps that (1) under the inert gas protective atmosphere, a potassium peroxodisulfate solid is added into constant-temperature deionized water, then methyl methacrylate is added, reacting is conducted, centrifuging and cleaning are conducted, evaporating is conducted for removing moisture, and thus a PMMA solid is obtained; (2) ferric nitrite and nickel nitrite are taken and dissolved into ethylene glycol, stirring is conducted, then methyl alcohol and ethylene glycol are added, the PMMA solid continues to be added, vacuum filtration is conducted after stirring, an obtained solid product is dried and calcined, and thus a ferronickel oxide is obtained; and (3) under inert gas protection, the ferronickel oxide and sodium hypophosphite are placed at a low air opening and an upper air opening correspondingly,calcining is conducted, and thus an objective product is obtained. Compared with the prior art, phosphatized ferronickel of a three-dimensional orderly macroporous structure is prepared successfullythrough a simple low-temperature phosphatization method, and the phosphatized ferronickel can serve as HER electrocatalyst to be applied to water electrolysis for hydrogen evolution, and has high catalytic activity, stability and the like.

Description

technical field [0001] The invention belongs to the technical field of electrolytic water catalytic materials, and relates to a three-dimensional ordered macroporous nickel-iron phosphide material and its preparation and application. Background technique [0002] In the 21st century, finding a safe, clean and sustainable energy supply is the most important scientific challenge facing mankind. Energy security, national security, environmental security and economic security all need to be guaranteed by solving energy problems in the next 20 years. With the continuous consumption of traditional fossil fuels (coal, oil, natural gas, etc.), people's demand for energy continues to grow, and energy issues have gradually become an important issue restricting the development of human society. At the same time, the environmental pollution caused by the extensive use of traditional fossil fuels has reached a point that cannot be ignored. [0003] In view of this, countries all over t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/08C25B11/06C25B1/04
CPCC01B25/088C25B1/04C25B11/075Y02E60/36
Inventor 陈作锋汪建营纪律律
Owner TONGJI UNIV
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