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a nanoscale Fe 9 ni 9 the s 16 Preparation method of based electrocatalyst

A fe9ni9s16 and catalyst technology, which is applied in the field of preparation of nano-scale Fe9Ni9S16-based electrocatalysts, can solve the problems of unfavorable large particle size, complicated procedures, high energy consumption and the like, and achieves the effects of simple process, low cost and low energy consumption.

Active Publication Date: 2022-04-05
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The object of the present invention is to provide a kind of high activity, high stability nanoscale Fe 9 Ni 9 S 16 In order to develop new, cheap, stable and efficient electrode materials for electrocatalysis and battery energy storage, and to solve the disadvantages of complex procedures, high temperature, high energy consumption and large particle size in the existing preparation methods of this material Problems with large-scale application

Method used

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  • a nanoscale Fe <sub>9</sub> ni <sub>9</sub> the s <sub>16</sub> Preparation method of based electrocatalyst
  • a nanoscale Fe <sub>9</sub> ni <sub>9</sub> the s <sub>16</sub> Preparation method of based electrocatalyst
  • a nanoscale Fe <sub>9</sub> ni <sub>9</sub> the s <sub>16</sub> Preparation method of based electrocatalyst

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Experimental program
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Effect test

Embodiment 1

[0033] Weigh 13mgFeCl 3 ·6H 2 O, 12mgNiCl 2 ·6H 2 0. 50mg of thiourea is a precursor, dissolved in 10mL of deionized water, after adding 1mL of ethanol, then adding 25mg of carbon nanotubes, after continuing to stir for 12h, utilizing liquid nitrogen to freeze, and carry out freeze-drying, the sample after getting the freeze-drying is fully Grind, then put into a caulking boat, put in a 50 sccm Ar flow at 600° C. for 1 h, and use X-ray diffraction (XRD) to study the phase composition of the final sample.

[0034] X-ray testing equipment and conditions: RigakuD / max2500, CuKα rays. Such as figure 1 The XRD pattern of the sample shown, as can be seen from the figure, the diffraction pattern is consistent with the PDF card 75-2024, indicating that the phase structure of the sample is Fe 9 Ni 9 S 16 .

Embodiment 2

[0036] Weigh 13mgFeCl 3 ·6H 2 O, 12mgNiCl 2 ·6H 2 0. 50mg of thiourea is a precursor, dissolved in 10mL of deionized water, after adding 1mL of ethanol, then adding 25mg of carbon nanotubes or 25mg of commercial carbon black (XC-72R), after continuing to stir for 12h, utilizing liquid nitrogen to freeze, and Freeze-drying is carried out, and the freeze-dried sample is fully ground, then put into a burning boat, and placed in a 50 sccmAr airflow at 600 ° C for 1 h, and then its morphology and microstructure are characterized by TEM.

[0037] TEM characterization equipment: Tencai-F20, the voltage used is 200kV. Such as figure 2 (a, b) and (c, d) are the morphologies of samples obtained when using carbon nanotubes and using XC-72R as the carrier, respectively. It can be seen from the morphology of the two samples that, in addition to the difference between the carbon tubes and carbon spheres, the active material Fe 9 Ni 9 S 16 The morphology on the two supports is basic...

Embodiment 3

[0039] Weigh 13mgFeCl 3 ·6H 2 O, 12mgNiCl 2 ·6H 2 O. 50mg of thiourea as a precursor, dissolved in 10mL of deionized water, added 1mL of ethanol, then added 25mg of XC-72R, continued to stir for 12 hours, frozen with liquid nitrogen, and lyophilized, and the lyophilized sample was fully ground , and then placed in a burning boat, placed in a 50 sccm Ar flow at 600 ° C for 1 h, and then tested for its electrocatalytic oxygen production activity.

[0040] Electrocatalytic oxygen generation test conditions: 5 mg of sample is first dispersed in 1 mL of 25 vol% ethanol aqueous solution, and 30 μL of perfluorinated ionic polymer (Nafion) is dropped into it, and then 20 μL of it is dropped into a rotating disk electrode with a diameter of 5 mm in multiple times Above, after natural drying, put it on the rotating disk electrode device produced by Pine Company, the electrode rotation speed is 1600 rpm, use EC-LabVSP300 electrochemical workstation to test, the voltage scanning speed ...

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Abstract

The invention relates to the fields of material preparation, electrocatalysis, and battery energy storage, specifically a nano-scale Fe 9 Ni 9 S 16 The purpose of this paper is to develop new, cheap, stable, and efficient electrode materials for electrocatalysis and battery energy storage, and to solve the problems of complex procedures, high temperature, high energy consumption, and large particle size in the existing preparation methods of this material. problems for large-scale application. The present invention prepares nano-scale pure-phase pyridoxite phase Fe-Ni-S solid solution Fe by mixing iron salt, nickel salt, organic sulfur source and conductive carrier, and reacting at an appropriate temperature in an inert gas 9 Ni 9 S 16 . The material obtained in the invention has simple preparation method, mild temperature, low energy consumption and low cost, is suitable for large-scale preparation, and has broad application prospects in the fields of electrocatalysis, battery energy storage and the like.

Description

technical field [0001] The invention relates to the fields of material preparation, electrocatalysis, and battery energy storage, specifically a nano-scale Fe 9 Ni 9 S 16 method for the preparation of electrocatalysts. Background technique [0002] Electrochemical water splitting to produce oxygen is an important half-reaction in green and efficient energy conversion and energy storage technologies such as electrolysis of water, solar water splitting devices, and rechargeable metal-air batteries. The multi-step reaction process involving up to four electrons makes the oxygen production reaction face a high thermodynamic barrier, requiring a high overpotential to generate the current density required for clean fuel production (10mA / cm 2 ). RuO 2 , IrO 2 Although noble metal-based oxygen-generating electrocatalysts have high activity, their lower crustal reserves and higher market prices limit their larger-scale applications. The development of efficient, stable, and ch...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B11/075C25B1/04H01M4/525H01M4/38H01M10/0525
CPCC25B11/04C25B1/04H01M4/525H01M4/38H01M10/0525Y02E60/36Y02E60/10
Inventor 刘岗张露露杨勇强成会明
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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