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Preparation method and application of a sulfur-doped intrinsically porous nickel-cobalt phosphide nanosheet

A technology of nickel-cobalt phosphide and nanosheets, which is applied in the direction of nanotechnology, hybrid/electric double-layer capacitor manufacturing, structural parts, etc., can solve the problems of poor rate performance and stability of nickel-cobalt phosphide nanomaterials, and achieve improved electric capacity. Chemical properties, increased edge active sites, and convenient preparation

Active Publication Date: 2021-10-29
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Technical problem: In order to solve the problem of poor rate performance and stability performance of nickel-cobalt phosphide nanomaterials, the present invention provides a method for preparing sulfur-doped intrinsically porous nickel-cobalt phosphide nanosheets through structural engineering and defect engineering and application, the method uses nickel foam as the substrate, the preparation process is simple, the energy consumption is low, and the cost is low

Method used

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Experimental program
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Embodiment 1

[0034] The steps of embodiment 1 include:

[0035] (1) Nickel foam pretreatment: the nickel foam was cleaned sequentially in 1 mol / L dilute hydrochloric acid solution, absolute ethanol and distilled water by ultrasonic cleaning for 30 minutes, and then vacuum-dried at 60° C. for 12 hours.

[0036] (2) Preparation of nickel-cobalt phosphide with intrinsic porous lamellar structure: in 60 milliliters of deionized water, dissolve into nickel chloride hexahydrate with a relative content of 5 g / liter, cobalt chloride hexahydrate of 9 grams / liter and 16 g / L of hexamethylenetetramine, magnetically stirred until completely dissolved. The pretreated nickel foam and the above mixed solution were placed in an autoclave and reacted at 100° C. for 8 hours. The precursor prepared above was placed in a muffle furnace for high-temperature calcination. The reaction conditions of the muffle furnace were that the heating rate was 3°C / min, the reaction temperature was 400°C, and the reaction tim...

Embodiment 2

[0041] The steps of embodiment 2 include:

[0042](1) Pretreatment of foamed nickel: Clean the foamed nickel sequentially in 2 mol / L dilute hydrochloric acid solution, absolute ethanol and distilled water for 30 minutes, and vacuum dry at 60° C. for 12 hours.

[0043] (2) Preparation of nickel-cobalt phosphide with an intrinsic porous sheet-like structure: in 60 milliliters of deionized water, dissolve into nickel chloride hexahydrate with a relative content of 4 grams per liter, cobalt chloride hexahydrate at 9 grams per liter and 15 g / L of hexamethylenetetramine, magnetically stirred until completely dissolved. The pretreated nickel foam and the above mixed solution were placed in an autoclave and reacted at 100° C. for 8 hours. The precursor prepared above was placed in a muffle furnace for high-temperature calcination. The reaction conditions of the muffle furnace were that the heating rate was 3°C / min, the reaction temperature was 400°C, and the reaction time was 2 hours...

Embodiment 3

[0048] The steps of embodiment 3 include:

[0049] (1) Pretreatment of foamed nickel: Clean the foamed nickel sequentially in 3 mol / L dilute hydrochloric acid solution, absolute ethanol and distilled water for 30 minutes, and vacuum dry at 60° C. for 12 hours.

[0050] (2) Preparation of nickel-cobalt phosphide with intrinsic porous sheet-like structure: in 60 milliliters of deionized water, dissolve the nickel chloride hexahydrate that relative content is 4 grams / liter, the cobalt chloride hexahydrate of 8 grams / liter and 14 g / L of hexamethylenetetramine, magnetically stirred until completely dissolved. The pretreated nickel foam and the above mixed solution were placed in an autoclave and reacted at 100° C. for 8 hours. The precursor prepared by the reaction is placed in the lower tuyere of the tube furnace, the sodium hypophosphite is placed in the upper tuyere, and the addition amount of the sodium hypophosphite accounts for 7% of the oxide. The heating rate of the tube ...

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Abstract

The present invention provides a preparation method and application of sulfur-doped intrinsically porous nickel-cobalt phosphide nanosheets, specifically comprising: a. preparing sulfur-doped intrinsically porous nickel-cobalt phosphide nanosheets; b. The sulfur-doped intrinsically porous nickel-cobalt phosphide nanosheets were used as the working electrode, the platinum sheet was used as the counter electrode, and the saturated calomel electrode was used as the reference electrode to form a three-electrode system for electrochemical performance testing. This eigenstate effectively solves the problem of poor structural stability of nickel-cobalt phosphide. The prepared sulfur-doped intrinsically porous nickel-cobalt phosphide nanosheet electrode has a specific capacitance of 2050 farads / g at a current density of 1 ampere / g, and 10,000 cycles at a current density of 5 ampere / g After cycling, 85% of the original capacity can still be maintained.

Description

technical field [0001] The invention belongs to the technical field of supercapacitor energy storage, and in particular relates to a method for preparing sulfur-doped intrinsically porous nickel-cobalt phosphide nanosheets. Background technique [0002] As an energy storage device, supercapacitors have performance advantages such as high power density and ultra-fast charge-discharge rate, but at the same time have the problem of low energy density. It is very important to study and prepare a high energy density, high cycle stability electrode material for the practical application of supercapacitors. Nickel-cobalt phosphide nanomaterials are considered to be ideal candidates for supercapacitor electrodes due to their excellent redox activity. However, nickel-cobalt phosphide nanomaterials will be transformed into transition metal hydroxides when undergoing faradaic reactions in alkaline electrolytes, and the phase transition will cause large volume expansion and internal st...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01G11/30H01G11/26H01G11/86H01M4/58B82Y40/00
CPCB82Y40/00H01G11/26H01G11/30H01G11/86H01M4/5805Y02E60/10
Inventor 王育乔王青青宋利黎李东朱世璠
Owner SOUTHEAST UNIV
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