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Preparation method of nickel phosphide microsphere with multilevel structure

A technology of nickel phosphide and microspheres, applied in structural parts, electrochemical generators, nanotechnology for materials and surface science, etc., can solve the problem of small specific surface area of ​​nickel phosphide particles and vibration of nano-scale nickel phosphide Low density and other problems, to achieve the effect of high tap density, mild conditions and simple preparation method

Inactive Publication Date: 2018-11-20
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The present invention aims to solve the technical problems of low tap density and small specific surface area of ​​nickel phosphide particles in the existing nano-scale nickel phosphide, and provides a preparation method of nickel phosphide microspheres with a multi-level structure

Method used

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  • Preparation method of nickel phosphide microsphere with multilevel structure
  • Preparation method of nickel phosphide microsphere with multilevel structure
  • Preparation method of nickel phosphide microsphere with multilevel structure

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specific Embodiment approach 1

[0014] Specific embodiment one: the preparation method of the nickel phosphide microsphere of multi-level structure of the present embodiment, carry out according to the following steps:

[0015] 1. Preparation of precursor:

[0016] According to the molar ratio of nickel acetate and urea is 1: (5-8), nickel acetate and urea are added to water, stirred and dissolved to obtain a mixed solution; then the mixed solution is kept in a water bath with a temperature of 80-90°C for 3 ~ 5 hours, after cooling, centrifuge to collect the solid phase, wash it clean, and then vacuum dry at a temperature of 60-80°C to obtain a precursor;

[0017] 2. Preparation of nickel phosphide microspheres with multi-level structure:

[0018] Put the precursor obtained in step 1 into a porcelain boat, put sodium hypophosphite into another porcelain boat, put the two porcelain boats together into a quartz tube, and continuously pass argon gas protection into the quartz tube, wherein The porcelain boat ...

specific Embodiment approach 2

[0019] Embodiment 2: The difference between this embodiment and Embodiment 1 is that the molar ratio of nickel acetate to urea in step 1 is 1: (6-7). Others are the same as in the first embodiment.

specific Embodiment approach 3

[0020] Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that the concentration of nickel acetate in the mixed solution in step 1 is 4-5 g / L, and the concentration of urea is 7-9 g / L. Others are the same as in the first or second embodiment.

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Abstract

The invention discloses a preparation method of a nickel phosphide microsphere with a multilevel structure, and relates to a preparation method of nickel phosphide. The method aims to solve the technical problem that the existing nickel phosphide is low in tap density. The method comprises the following steps of 1, preparing a precursor by using nickel acetate and urea; 2, putting the precursor into a porcelain boat, and then putting sodium hypophosphite into another porcelain boat, putting the two porcelain boats into a quartz tube together, and continuously pumping argon into the quartz tubefor protection, wherein the porcelain boat containing sodium hypophosphite is placed on the upstream of the air flow, and then heating the quartz tube to 300-400 DEG C, and carrying out heat preservation for 4-6 hours to obtain the nickel phosphide microsphere with the multilevel structure. The nickel phosphide microsphere disclosed by the invention is composed of a nickel phosphide nanosheet with a secondary structure, and the specific surface area of the nickel phosphide microsphere can be improved by utilizing the multilevel structure of the nickel phosphide microsphere, the contact area with an electrolyte is enlarged, the tap density is high, and the volume specific capacity is higher. The preparation method is simple and mild in conditions. The method can be used for manufacturing anegative electrode of a lithium ion battery.

Description

technical field [0001] The invention relates to a preparation method of nickel phosphide. Background technique [0002] With the development of society, the demand for energy storage equipment is getting higher and higher, and the application of reversible lithium-ion batteries is becoming more and more extensive. Electrode materials are an important part of lithium-ion batteries, and it is of great significance to develop new electrode materials with high specific capacity, fast charge and discharge, and long-term cycle stability. Many transition metal oxides are now used in lithium-ion batteries due to their high specific capacity, but the electronic conductivity of transition metal oxides is poor, which makes transition metal oxides poor charge and discharge rate performance. The transition metal phosphides have lower charge and discharge potential, higher electronic conductivity, certain metallic properties, better thermal stability, higher specific capacity and are use...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M10/0525B82Y30/00
CPCB82Y30/00H01M4/5805H01M10/0525H01M2004/021Y02E60/10
Inventor 姜再兴邱胜友
Owner HARBIN INST OF TECH
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