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Anode material of composite silicate and preparation method thereof

A composite silicate and positive electrode material technology, which is applied in battery electrodes, electrical components, circuits, etc., can solve the problem of poor overcharge resistance of layered excessive metal oxides, low theoretical capacity of olivine-type lithium iron phosphate, and spinite Poor high-temperature performance of stone-type lithium manganate, etc., to achieve the effect of being convenient for large-scale production, excellent electrochemical performance, and good electrochemical performance

Active Publication Date: 2011-06-08
BTR NEW MATERIAL GRP CO LTD
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

The above three materials have different defects: ① layered excessive metal oxides have poor overcharge resistance; ② olivine-type lithium iron phosphate has low theoretical capacity, low voltage platform, low energy density, and poor conductivity; ③Poor high temperature performance of spinel lithium manganese oxide
[0006] In these synthetic methods, there are some deficiencies. Although the hydrothermal method and the sol-gel method can synthesize silicates with small particle size and uniformity, industrialization It is relatively difficult; the co-precipitation method also has the difficulty of process control and inconvenient industrialization; at the same time, the silicate cathode material, like the phosphate cathode material, has the problem of poor conductivity, which makes it difficult to charge and discharge at a large rate. The improvement reported so far The method generally only stays at the stage of coating carbon, and has not improved the electrical conductivity inside the material through doping.

Method used

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  • Anode material of composite silicate and preparation method thereof
  • Anode material of composite silicate and preparation method thereof
  • Anode material of composite silicate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Accurately weigh 200g of nano-silica, 600g of ferrous oxalate, 687g of lithium acetate, and 40g of glucose, add 2L of deionized water and stir for 1 hour. It was transferred to a ball mill, ball milled at a speed of 500r / min for 10h, and taken out to obtain a uniformly mixed slurry. Then, it is spray-dried and granulated under the condition of 200° C. to obtain a precursor of uniform spheroidized particles. Put the sprayed precursor in the furnace, use nitrogen as the protective atmosphere, the nitrogen flow rate is 6L / min, and the furnace temperature is raised to 650°C at a heating rate of 5°C / min, and then sintered at 650°C for 12h, to be cooled After reaching room temperature, grind the product through a 400-mesh sieve to obtain Li 2 FeSiO 4 / C cathode material. Its carbon content is about 4.5%, such as figure 1 Shown is XRD showing no impurity phases, such as figure 2 As shown, the particle size distribution of the material prepared by this method is excellent...

Embodiment 2

[0035] Accurately weigh 200g of nano-silica, 270g of ferric oxide, 687g of lithium acetate, and 80g of glucose, add 2L of deionized water and stir for 1 hour. It was transferred to a ball mill, ball milled at a speed of 500r / min for 10h, and taken out to obtain a uniformly mixed slurry. Then, it is spray-dried and granulated under the condition of 200° C. to obtain a precursor of uniform spheroidized particles. Put the sprayed precursor in the furnace, use nitrogen as the protective atmosphere, the nitrogen flow rate is 6L / min, and the furnace temperature is raised to 650°C at a heating rate of 5°C / min, and then sintered at 650°C for 12h, to be cooled After reaching room temperature, grind the product through a 400-mesh sieve to obtain Li 2 FeSiO 4 / C cathode material. Its carbon content is about 4.3%, XRD shows that there is no impurity phase, the particle size distribution of the material prepared by this method is excellent, the electrochemical performance is good, and t...

Embodiment 3

[0037] Accurately weigh 715g ethyl orthosilicate, 600g ferrous oxalate, 687g lithium acetate, 80g glucose, add 2L deionized water and stir for 1 hour. It was transferred to a ball mill, ball milled at a speed of 500r / min for 10h, and taken out to obtain a uniformly mixed slurry. Then, it is spray-dried and granulated under the condition of 200° C. to obtain a precursor of uniform spheroidized particles. Put the sprayed precursor in the furnace, use nitrogen as the protective atmosphere, the nitrogen flow rate is 6L / min, and the furnace temperature is raised to 650°C at a heating rate of 5°C / min, and then sintered at 650°C for 12h, to be cooled After reaching room temperature, grind the product through a 400-mesh sieve to obtain Li 2 FeSiO 4 / C cathode material. Its carbon content is about 4.3%, XRD shows that there is no impurity phase, the particle size distribution of the material prepared by this method is excellent, the electrochemical performance is good, and the capac...

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Abstract

The invention discloses a solid phase method for synthesizing an anode material of a composite silicate (Li2-yMyFexMn1-xSiO4 / C, wherein 0<=x<=1, 0<=y<=0.02, and M is one or a plurality of transition state elements of IB-VIIIB) series, and an anode material of the composite silicate. Organic carbon source is added in iron source, manganese source, lithium source, silicon source and organic carbon source doped with metal compound for dispersing and ball milling for a plurality of hours, and the mixture is dried by spray, protected in a vacuum environment or by introduced non-oxide gas and sintered at the temperature of 600 to 950 DEG C for 5 to 24 hours, thus the anode material of the composite silicate with good electrochemical performance is obtained. The preparation method of the anode material has high technical adaptability and is easy to realize industrial production; and the product has extremely good electrochemical performance.

Description

technical field [0001] The present invention relates to a kind of composite type silicate (Li 2-y m y Fe x mn 1-x SiO 4 / C, 0<=x<=1, 0<=y<=0.02, M is one or several transition state elements in IB~VIIIB) series cathode materials, and the preparation method of the materials. Background technique [0002] The increasingly prominent energy problems and the deteriorating environmental problems have prompted governments of various countries to continue to devote themselves to the development of new energy sources. Lithium-ion battery is one of the most promising new energy sources. It not only has the advantages of high energy density and long cycle life, but also is friendly to the environment. The source of power. [0003] The main cathode materials that have been applied to power batteries, including layered transition metal oxides (LiMO 2 ), olivine lithium iron phosphate (LiFePO 4 ) and spinel lithium manganate (LiMn 2 o 4 ). The above three materials ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/136H01M4/58H01M4/62H01M4/1397
CPCY02E60/12Y02E60/122Y02E60/10
Inventor 贺雪琴岳敏陈占军梁奇
Owner BTR NEW MATERIAL GRP CO LTD
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