Preparation method of cage-shaped ferronickel bimetallic phosphide loaded nitrogen-doped porous carbon material

A nitrogen-doped porous carbon and bimetallic technology, which is applied in the preparation/purification of carbon, phosphides, phosphorus compounds, etc., can solve the problems of poor stability of metal phosphides, improve electrocatalytic performance, and increase charge transfer channel, the effect of increasing conductivity

Pending Publication Date: 2020-11-06
淮安新能源材料技术研究院
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Transition metal phosphides have good OER performance, and low-cost transition metal phosphides have attracted extensive attention in renewable energy applications due to their catalytic activity and long-term stability. Although transition metal phosphides have made some progress in OER electrocatalysis, but The currently prepared metal phosphides are not stable in the hydrogen evolution process

Method used

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  • Preparation method of cage-shaped ferronickel bimetallic phosphide loaded nitrogen-doped porous carbon material
  • Preparation method of cage-shaped ferronickel bimetallic phosphide loaded nitrogen-doped porous carbon material
  • Preparation method of cage-shaped ferronickel bimetallic phosphide loaded nitrogen-doped porous carbon material

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Embodiment 1

[0032] 1. Preparation of roughened melamine sponge (MS): first cut the melamine sponge into 2 × 2 × 2cm with scissors 3 The cube was washed with deionized water in a magnetic stirrer for 15 minutes, and then the cleaned sponge was placed in a 3.0mol / L sodium hydroxide solution, heated in a water bath at 50°C for 30 minutes, and then washed with deionized water Wash 3 times and dry at 60°C to obtain a roughened melamine sponge (MS).

[0033] 2. Preparation of nickel-iron bimetallic Prussian blue precursor coated with melamine sponge: nickel acetate and trisodium citrate were dissolved in 200 mL of deionized water at a molar ratio of 1:1, stirred for 30 minutes, and recorded as solution A ; Put the roughened melamine sponge prepared in step 1 into solution A, and sonicate for 30 minutes. Dissolve potassium ferricyanide, whose molar mass is 1 / 2 that of nickel acetate, in 300 mL of deionized water, and stir the solution until it becomes clear, and record it as solution B. Then s...

Embodiment 2

[0037] 1. Preparation of roughened melamine sponge (MS): first cut the melamine sponge into a cube of 2 × 2 × 2cm3 with scissors, then wash it in a magnetic stirrer with deionized water for 30 minutes, and then place the cleaned sponge in In a 4.0 mol / L sodium hydroxide solution, heat in a water bath at 60°C for 40 minutes, wash with deionized water three times, and dry at 70°C to obtain a roughened melamine sponge (MS).

[0038] 2. Preparation of nickel-iron bimetallic Prussian blue precursor coated with melamine sponge: nickel acetate and trisodium citrate were dissolved in 250 mL of deionized water at a molar ratio of 1:1.2, stirred for 45 minutes, and recorded as solution A; Put the roughened melamine sponge prepared in step 1 into solution A and sonicate for 40 min. Dissolve potassium ferricyanide, whose molar mass is 1 / 2 that of nickel acetate, in 400 mL of deionized water, and stir the solution until it becomes clear, and record it as solution B. Then slowly add the so...

Embodiment 3

[0042] 1. Preparation of roughened melamine sponge (MS): first cut the melamine sponge into a cube of 2 × 2 × 2cm3 with scissors, then wash it in a magnetic stirrer with deionized water for 45 minutes, and then place the cleaned sponge in In a 5.0 mol / L sodium hydroxide solution, heat in a water bath at 70 °C for 45 minutes, wash with deionized water three times, and dry at 80 °C to obtain a roughened melamine sponge (MS).

[0043] 2. Preparation of nickel-iron bimetallic Prussian blue precursor coated with melamine sponge: nickel acetate and trisodium citrate were dissolved in 300 mL of deionized water at a molar ratio of 1:1.5, stirred for 60 minutes, and recorded as solution A ; Put the roughened melamine sponge prepared in step 1 into solution A and sonicate for 45 minutes. Dissolve potassium ferricyanide, whose molar mass is 1 / 2 that of nickel acetate, in 500 mL of deionized water, and stir the solution until it becomes clear, which is referred to as solution B. Then slo...

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Abstract

The invention discloses a preparation method of a cage-shaped nickel-iron bimetallic phosphide loaded nitrogen-doped porous carbon material. The preparation method comprises the following steps: cyanide ions are used as organic ligands, nickel ions and iron ions are used as metal sources; a ferronickel bimetallic Prussian blue compound growing on melamine is prepared through a coprecipitation method, the precursor is etched into a cage-shaped cube through one-step ammonia water, the cage-shaped cube and sodium hypophosphite are calcined at the temperature of 350 DEG C in an Ar atmosphere, andthe cage-shaped ferronickel bimetallic phosphide loaded nitrogen-doped porous carbon material is obtained. The PBA nano hollow cage-shaped particle group obtained by an ammonia water etching method can expose more active sites in the reaction process; the sintered and roughened porous carbon substrate with the melamine sponge three-dimensional structure not only can fix active sites to prevent agglomeration, but also can increase conductivity to accelerate charge transfer; metal phosphide is effectively formed through doping of phosphorus, the electronic structure around nickel and iron can beadjusted, and the charge transfer process can be accelerated.

Description

technical field [0001] The invention relates to the technical field of electrocatalytic material manufacture, in particular to a method for preparing a cage-shaped nickel-iron bimetallic phosphide-loaded nitrogen-doped porous carbon material. Background technique [0002] With the increase of global energy consumption, the reduction of fossil fuels and the deterioration of the environment, water separation reactions have gradually attracted more and more attention from researchers. The water separation reaction includes two parts: oxygen evolution reaction (OER) and hydrogen evolution reaction (HER). Under the action of many metals, the hydrogen evolution reaction is a simple reaction that is easy to occur due to its low overpotential, that is, the energy required for the reaction is less; while the oxygen evolution reaction is relatively complex and the reaction kinetics is slow. It is difficult to happen, the main reason is as follows, the reaction involves the transfer o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/10C01B25/08C01B32/05C01B3/04C25B1/04C25B11/06
CPCB01J27/24B01J35/0033B01J35/10B01J35/1004C01B25/088C01B32/05C01B3/042C25B1/04C01P2002/82C01P2004/03C01P2004/04C01P2006/40C01P2004/30Y02E60/36
Inventor 封平净王自强尹延谋魏奇
Owner 淮安新能源材料技术研究院
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