Silicide/oxide composite negative electrode material with lithium silicate interface layer and preparation method

A negative electrode material and oxide technology, which is applied in the field of silicon/oxide composite materials and its preparation, can solve the problems of silicon surface instability, volume expansion mismatch, separation of silicon active centers and matrix materials, etc., to promote efficient transmission , the effect of good ionic conductivity

Active Publication Date: 2016-12-21
DALIAN MARITIME UNIVERSITY
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Problems solved by technology

[0008] In order to solve the problem in the prior art that the volume expansion mismatch between silicon and the matrix material, the surface instability of silicon and other influencing factors are likely to cause the separation of the silicon active center and the matrix material in the subsequent cycle process, the present invention provides a Silicon / oxide composite negative electrode material and preparation method of lithium silicate interface layer

Method used

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  • Silicide/oxide composite negative electrode material with lithium silicate interface layer and preparation method
  • Silicide/oxide composite negative electrode material with lithium silicate interface layer and preparation method
  • Silicide/oxide composite negative electrode material with lithium silicate interface layer and preparation method

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Effect test

Embodiment 1

[0044] (1) Mix absolute ethanol (analytical pure) and deionized water at a volume ratio of 1:1 to obtain an ethanol-water mixed solution for later use;

[0045] (2) Dissolve 0.27g of niobium chloride in 40ml of absolute ethanol solution for later use;

[0046] (3) Put 0.11g of nano-silicon powder (average particle size is 40nm) into the niobium chloride / ethanol solution, and ultrasonically vibrate for 30min to make a silicon powder-niobium chloride / ethanol solution;

[0047] (4) Prepare lithium hydroxide into a 0.02mol / L lithium hydroxide / ethanol-water mixed solution (the volume ratio of ethanol:water is 1:1);

[0048] (5) Take 250ml of lithium hydroxide / ethanol-water mixed solution (20mmol / L), and add it dropwise to the silicon powder-niobium chloride / ethanol solution. : 1) washing 3 times until the filtrate is neutral, and drying in vacuum at 70° C. for 8 hours;

[0049] ⑹ Place the dried sample in a tube furnace, raise the temperature from room temperature to 600 °C at a ...

Embodiment 2

[0054] (1) Mix ethylene glycol (analytical pure) and deionized water at a volume ratio of 2:1 to obtain an ethylene glycol-water mixed solution for later use;

[0055] (2) Dissolve 0.27g niobium chloride in 40ml ethylene glycol solution for later use;

[0056] (3) Put 0.13g of nano-silicon powder (40nm) into the niobium chloride / ethylene glycol solution and oscillate ultrasonically for 30 minutes to make a silicon powder-niobium chloride / ethylene glycol solution;

[0057] (4) Use lithium hydroxide to prepare a 20mmol / L lithium hydroxide / ethylene glycol-mixed solution (the volume ratio of ethanol:water is 2:1);

[0058] (5) Take 250ml of lithium hydroxide / ethylene glycol-mixed solution (20mmol / L), and add it dropwise to the silicon powder-niobium chloride / ethylene glycol solution. After the reaction is completed, precipitate and filter, and use the ethanol-water mixed solution (2 : 1) Washing twice until the filtrate is neutral, and drying in vacuum at 60° C. for 10 hours;

...

Embodiment 3

[0062] ⑴ Mix ethanol (analytical pure) and deionized water at a volume ratio of 1:1 to obtain an ethanol-water mixed solution for later use;

[0063] (2) Dissolve 0.27g niobium chloride and 0.34g tetrabutyl titanate in 40ml ethanol solution for later use;

[0064] (3) Put 0.15g of nano-silicon powder (40nm) into niobium chloride-tetrabutyl titanate / ethanol solution, and ultrasonically oscillate for 30min to make silicon powder-niobium chloride-tetrabutyl titanate / ethanol solution;

[0065] (4) Prepare lithium hydroxide with 20mmol / L lithium hydroxide / ethanol-mixed solution (the volume ratio of ethanol:water is 1:1);

[0066] (5) Take 500ml of lithium hydroxide / ethanol-mixed solution (20mmol / L), add it dropwise to the silicon powder-niobium chloride / ethanol solution, after the reaction is completed, precipitate and filter, and wash with ethanol-water mixed solution (1:1) 3 times until the filtrate is neutral, vacuum dry at 70°C for 8 hours;

[0067] ⑹ Place the dried sample i...

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Abstract

The invention provides a silicide / oxide composite negative electrode material with a lithium silicate interface layer and a preparation method, and belongs to the field of lithium ion batteries. The silicide / oxide composite negative electrode material with the lithium silicate interface layer comprises a silicon active center, an oxide substrate and the lithium silicate interface layer, wherein the lithium silicate interface layer is positioned between the silicon active center and the oxide substrate. By adopting a method that chemical deposition is combined with high-temperature solid-phase reaction, excessive lithium ions are adsorbed by virtue of good adsorption properties of deposition reaction products, so that the lithium silicate interface layer is formed in situ between the silicon active center and the oxide substrate through high-temperature solid-phase reaction of the lithium ions and trace silicon oxide on a silicon surface, not only is a continuous channel for lithium ion transmission provided, but also the lithium silicate interface layer can be used as an effective protection interface to reduce the reaction property of the active center and the oxide substrate, and therefore, good electrochemical circulation properties can be achieved. The processes related to the silicide / oxide composite negative electrode material are very simple, and the composite material prepared by using the method is excellent in interfacial compatibility.

Description

technical field [0001] The invention relates to a lithium ion battery negative electrode material, a preparation method and an application, belonging to the field of lithium ion batteries. Specifically, it relates to a silicon / oxide composite material with high specific capacity and high cycle life that can be used as the negative electrode of lithium-ion batteries, its preparation method and application. Background technique [0002] Compared with other secondary chemical power systems, lithium-ion batteries have the characteristics of high energy density, long life, and no pollution to the environment, and are widely used in energy supply systems for mobile terminals and transportation tools. For carbon anode materials widely used in lithium-ion batteries at present, due to the rapid development of processing technology and assembly technology, the method of further improving its reversible electrochemical energy storage efficiency through the improvement of battery assemb...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/38H01M4/48H01M4/58B82Y30/00H01M10/0525
CPCB82Y30/00H01M4/366H01M4/386H01M4/48H01M4/5825H01M10/0525Y02E60/10
Inventor 文钟晟杜路路王冠琴李嵩孙俊才季世军
Owner DALIAN MARITIME UNIVERSITY
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