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Method for preparing cage-shaped sphere structured silicon-carbon cathode material

A technology of anode material and small balls, which is applied in the field of preparation of silicon-carbon anode materials, can solve problems such as poor performance, and achieve the effects of alleviating volume expansion stress, fast lithium ion and electron diffusion, and good cycle stability

Inactive Publication Date: 2018-11-13
FUJIAN XFH NEW ENERGY MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

All the obtained samples show a three-dimensional structure of SiOx dispersed together with Si, where Li ions need to migrate through lithium silicate or Li after the first cycle 2 O layers, thus resulting in poor performance

Method used

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  • Method for preparing cage-shaped sphere structured silicon-carbon cathode material
  • Method for preparing cage-shaped sphere structured silicon-carbon cathode material

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preparation example Construction

[0017] The invention discloses a method for preparing a silicon-carbon negative electrode material with a cage-shaped bead structure, which includes the following steps:

[0018] (1) Nano-silicon particles indicate activation: add 0.8-1.2g nano-silicon powder to 0.8-1.5L absolute ethanol to disperse; then add 6-14ml surfactant 3-aminopropyltriethoxysilane (APTES) Ultrasound for 15-25 hours in the silicon powder dispersion system; then, filter and wash with deionized water for 2-5 times to obtain silicon slurry.

[0019] (2) Slurry mixing process: Add the above-mentioned surface-activated silicon slurry into 0.8-1.2L of water, and add 90-110g of citric acid, stir for 1-3h, and sonicate for 1-3h.

[0020] (3) Spray drying and calcination: the above slurry is dried by spray drying equipment to obtain a precursor; then the precursor is put into a tube furnace and calcined for 0.8-2h in an argon atmosphere at 800-1000°C , The heating rate is 1-4°C / min.

Embodiment 1

[0023] A method for preparing a silicon-carbon negative electrode material with a cage-shaped bead structure, comprising the following steps:

[0024] (1) Activated nano-silicon particles: add 1g of nano-silicon powder to 1L of absolute ethanol to disperse; then add 10ml of surfactant 3-aminopropyltriethoxysilane to the dispersion of the silicon powder, and ultrasonicate for 20h; then, Filter and wash with deionized water 3 times to obtain silicon slurry.

[0025] (2) Slurry mixing process: Add the above-mentioned surface-activated silicon slurry into 1L of water, and add 100g of citric acid, stir for 2h, and sonicate for 2h.

[0026] (3) Spray drying and calcination: the above slurry was dried by spray drying equipment to obtain the precursor; then the precursor was put into a tube furnace and calcined for 1 hour in an argon atmosphere at 900°C, with a heating rate of 3°C / min.

[0027] Such as figure 1 Shown, is the scanning electron microscope picture that obtains silicon...

Embodiment 2

[0030] A method for preparing a silicon-carbon negative electrode material with a cage-shaped bead structure, comprising the following steps:

[0031] (1) Activated nano-silicon particles: add 0.8g of nano-silicon powder to 0.9L of absolute ethanol to disperse; then add 7ml of surfactant 3-aminopropyltriethoxysilane to the dispersion of silicon powder, and sonicate for 16h; Then, it was suction-filtered and washed twice with deionized water to obtain a silicon slurry.

[0032] (2) Slurry mixing process: Add the above-mentioned surface-activated silicon slurry into 0.8L of water, and add 90g of citric acid, stir for 1h, and sonicate for 2.1h.

[0033] (3) Spray drying and calcination: The above slurry is dried by spray drying equipment to obtain the precursor; then the precursor is put into a tube furnace and calcined in an argon atmosphere at 800°C for 0.8h, and the heating rate is 1°C / min.

[0034] After testing, the silicon carbon obtained in this example has an initial di...

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Abstract

The invention discloses a method for preparing a cage-shaped sphere structured silicon-carbon cathode material. The method comprises the following steps: (1) carrying out surface activation on nano silicon granules, namely dispersing 0.8-1.2g of nano silicon powder into 0.8-1.5L of absolute ethyl alcohol; further putting 6-14ml of a surfactant, namely 3-aminopropyl triethoxysilane into a silicon powder dispersion system, and carrying out ultrasonic treatment for 15-25 hours; (2) carrying out a slurry mixing process, namely putting the silicon slurry after surface activation into 0.8-1.2L of water, further adding 90-110g of citric acid, stirring for 1-3 hours, and carrying out ultrasonic treatment for 1-3 hours; (3) carrying out spraying drying and calcining. As a buffer phase, the silicon-carbon cathode material prepared by using the method is capable of reducing volume swelling in a reaction circulation period; in addition, an in-situ prepared Si nano structure domain of which the size is smaller than 100nm is uniformly dispersed, so that the volume swelling stress can be effectively alleviated; secondly, due to adoption of a cage-shaped sphere structure, rapid lithium ion and electron diffusion can be allowed, and then excellent electrochemical properties can be achieved in return, particularly better circulation stability and improved velocity properties.

Description

technical field [0001] The invention relates to the technology in the field of negative electrode materials, in particular to a method for preparing a silicon-carbon negative electrode material with a cage-shaped bead structure. Background technique [0002] Due to the impressive theoretical capacity of Si, silicon-based materials are considered to be the best anode materials for next-generation lithium-ion batteries. However, the drastic volume change of Si (~300%) upon lithium deintercalation leads to loss of electrical contact and excessive solid-electrolyte interphase (SEI) growth, which leads to poor rate capability and cycling stability. Recently, two-dimensional silicon, so-called silica gel, has attracted a lot of attention, suggesting promise for lithium-ion batteries. However, buckled honeycomb silicon, and even multilayer silicon, is unstable in air for 24 hours. Alternatively, non-stoichiometric silicon oxides of annealed SiO formed from matrix nanocrystalline ...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/38H01M4/62H01M10/0525B82Y30/00
CPCB82Y30/00H01M4/362H01M4/386H01M4/625H01M10/0525Y02E60/10
Inventor 赵东辉周鹏伟王晓伟
Owner FUJIAN XFH NEW ENERGY MATERIALS CO LTD