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High-temperature solid-phase preparation method of negative electrode material lithium orthosilicate of lithium ion battery

A technology for lithium ion batteries and negative electrode materials, applied in battery electrodes, secondary batteries, circuits, etc., can solve the problems of high lithium intercalation potential and low capacity, achieve high specific capacity, increase electronic conductivity, and the process is simple and easy to implement Effect

Inactive Publication Date: 2014-07-23
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, its lithium intercalation potential (~1.55V) is relatively high and its capacity (theoretical specific capacity is 175mAh / g) is low

Method used

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  • High-temperature solid-phase preparation method of negative electrode material lithium orthosilicate of lithium ion battery
  • High-temperature solid-phase preparation method of negative electrode material lithium orthosilicate of lithium ion battery
  • High-temperature solid-phase preparation method of negative electrode material lithium orthosilicate of lithium ion battery

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] LiOH and SiO 2 Weigh according to the stoichiometric ratio of Li:Si=4:1, mix evenly, use a planetary ball mill, add an appropriate amount of ethanol, just submerge the raw materials, use wet ball milling for 8 hours, and then dry in an oven;

[0040] Then it was heated and pretreated at 300° C. for 5 hours in an air atmosphere, and after natural cooling, a powdery product was obtained;

[0041] In the planetary ball mill, use the same method to ball mill again for 6h, dry in the oven, and 2 Sintering at 680°C for 12 h under air atmosphere to obtain lithium orthosilicate [Li 4 SiO 4 ] Anode material.

[0042] The XRD pattern of the product is shown in figure 1 (a), it can be seen from the figure that a pure-phase monoclinic lithium orthosilicate negative electrode material was synthesized by this high-temperature solid-state sintering method. There is no impurity peak in the spectrogram, and the product has high purity. figure 2 It is a scanning electron microscop...

Embodiment 2

[0045] Combine LiOH and H 2 SiO 3 Weigh according to the stoichiometric ratio of Li:Si=4:1, mix evenly, use a planetary ball mill, add an appropriate amount of ethanol, just submerge the raw materials, use wet ball milling for 12 hours, and then dry in an oven;

[0046] Then it was heated and pretreated at 260°C for 8 hours under a nitrogen atmosphere, and after natural cooling, a powdery product was obtained;

[0047] The above-mentioned powdery product was ball-milled for 5 hours again in the planetary ball mill in the same way. 2 - Sintering at 700° C. for 10 h in an Ar mixed gas atmosphere (hydrogen accounts for 5% of the total volume, and Ar accounts for 95% of the total volume), to obtain a negative electrode material of lithium orthosilicate. Add the acetylene black that accounts for its mass fraction 10wt% in above-mentioned powdery product as carbon source, after manual grinding, in 5% H 2 -Ar mixed gas atmosphere, heat preservation at 350°C for 4h to obtain carbon...

Embodiment 3

[0050] LiNO 3 and H 2 SiO 3 Take by weighing according to the stoichiometric ratio of Li:Si=4:1, grind 40min in the agate mortar, mix well;

[0051] Then carry out pretreatment at 300°C for 12 hours under air atmosphere, and after natural cooling, a powdery product is obtained;

[0052] Add citric acid accounting for 5 wt% of the above powder product as a carbon source, hand grind it in an agate mortar for half an hour; sinter at 750°C for 6 hours under an argon atmosphere to obtain carbon-coated orthosilicon Lithium Oxide [Li 4 SiO 4 ] Anode material.

[0053] The XRD pattern of the product is shown in Figure 7 (a), it can be seen from the figure that a pure-phase monoclinic lithium orthosilicate negative electrode material was synthesized by high-temperature solid-state sintering. There is no impurity peak in the spectrum, and the product has high purity. Figure 8 Its scanning electron microscope picture. Figure 8 It is a scanning electron microscope picture of t...

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Abstract

The invention discloses a high-temperature solid-phase preparation method of a negative electrode material lithium orthosilicate of a lithium ion battery. The preparation method comprises the steps of uniformly mixing a silicon source and a lithium source according to a mole ratio of lithium to silicon being 4:1, and carrying out ball milling to obtain a precursor; heating the uniformly mixed precursor at the temperature of 200-400 DEG C for 2-12 hours under an air atmosphere, an inert gas atmosphere or a reducing gas atmosphere, and after naturally cooling, grinding to obtain a powder material; carrying out ball-milling on the powder material again for 6-24 hours, arranging the powder material in a tube furnace, sintering at the temperature of 450-1000 DEG C for 4-24 hours under the air atmosphere, the inert gas atmosphere or the reducing gas atmosphere, and naturally cooling to obtain the negative electrode material lithium orthosilicate. The invention further relates to a carbon-coated negative electrode material lithium orthosilicate obtained by adding a carbon material in a preparation process. The high-temperature solid-phase preparation method is simple in process and easy to operate. The negative electrode material lithium orthosilicate synthesized by adopting the preparation method is low in lithium-embedding potential (0.1-1 V) and excellent in cycle performance.

Description

technical field [0001] The present invention relates to a kind of negative electrode material of lithium ion battery, particularly relate to a kind of negative electrode material of lithium ion battery lithium orthosilicate [Li 4 SiO 4 ] High temperature solid phase preparation method. Background technique [0002] Lithium-ion battery is a new generation of green high-energy rechargeable battery; it has high working voltage, small size, light weight, high mass-to-volume specific energy, large output power, long cycle life, fast charge and discharge, low self-discharge rate, no memory Effect and other advantages, it has been widely used in various portable devices, digital products and hybrid vehicles, and has penetrated into every corner of society. [0003] With the commercialization of lithium-ion batteries launched by SONY in 1991, the research on lithium-ion battery-related materials is in full swing. Due to the diversification of functional requirements for various p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1397H01M4/58
CPCH01M4/366H01M4/5825H01M4/625H01M10/0525Y02E60/10
Inventor 赵彦明耿小凤董有忠
Owner SOUTH CHINA UNIV OF TECH
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