Production method of lithium ferric metasilicate anode material

A positive electrode material, lithium iron silicate technology, applied in the field of electrochemistry, can solve the problem of difficult balance between material density and electrochemical performance, and achieve the effects of avoiding side reactions of impurity compounds, promoting the roasting process, and facilitating industrial production

Inactive Publication Date: 2009-08-05
CENT SOUTH UNIV
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Problems solved by technology

[0009] Aiming at the problem that the traditional method of synthesizing lithium iron silicate positive electrode material is difficult to balance the material density and electrochemical performance, the present invention provides a hydrolysis co-precipitation-normal temperature reduction method to synthesize silicic acid according to the chemical characteristics of iron salt and silicate The method for lithium iron cathode material, the main steps include: iron, silicon hydrolysis co-precipitation, Fe 3+ Normal temperature reduction, low temperature roasting, etc.

Method used

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  • Production method of lithium ferric metasilicate anode material
  • Production method of lithium ferric metasilicate anode material
  • Production method of lithium ferric metasilicate anode material

Examples

Experimental program
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Effect test

Embodiment 1

[0025] FeCl 3 Aqueous solution, NaOH solution and Na 2 SiO 3 The solution is added into the stirred reactor in parallel, and the pH value of the reaction system is controlled to be 4.5±0.2, so that ferric iron and SiO 3 2- Hydrolysis occurs, and after filtration and washing, a co-precipitate of iron and silicon, FeCl 3 with Na 2 SiO 3 The amount added is controlled by Fe / Si molar ratio of 1:1.

[0026] Mix iron and silicon co-precipitate with lithium oxalate solution, oxalic acid solution and sucrose to form a slurry, ball mill, and Fe 3+ reduced to Fe 2+ , the precursor material for the synthesis of lithium iron silicate is obtained after drying, wherein the amount of oxalic acid added is based on oxalic acid / Fe 3+ The molar ratio is 0.6, the Li / Si molar ratio in the raw material is controlled to be 2, and the amount of sucrose added is controlled according to the residual carbon content in the obtained lithium iron silicate cathode material being 5wt%±0.2.

[0027] ...

Embodiment 2

[0030] Fe(NO 3 ) 3 Aqueous solution, KOH solution and Na 2 SiO 3 The solution is added into the stirred reactor in parallel, and the pH value of the reaction system is controlled to be 3.2±0.2, so that ferric iron and SiO 3 2- Hydrolysis occurs, and after filtration and washing, a co-precipitate of iron and silicon is obtained, Fe(NO 3 ) 3 with Na 2 SiO 3 The amount added is controlled by Fe / Si molar ratio of 1:1.

[0031] Mix iron and silicon co-precipitate with lithium hydroxide solution, oxalic acid solution and carbon gel to form a slurry, ball mill, and Fe 3+ reduced to Fe 2+ , the precursor material for the synthesis of lithium iron silicate is obtained after drying, wherein the amount of oxalic acid added is based on oxalic acid / Fe 3+ The molar ratio is 0.5, the Li / Si molar ratio in the raw material is controlled at 1.96, and the amount of carbon gel added is controlled at 3wt%±0.2 in the obtained lithium iron silicate cathode material.

[0032] The above pre...

Embodiment 3

[0035] Fe 2 (SO 4 ) 3 Aqueous solution, ammonia solution and Na 2 SiO 3 The solution is added into the stirred reactor in parallel, and the pH value of the reaction system is controlled to be 5.0±0.2, so that ferric iron and SiO 3 2- Hydrolysis occurs, and after filtration and washing, a co-precipitate of iron and silicon, Fe 2 (SO 4 ) 3 with Na 2 SiO 3 The amount added is controlled by Fe / Si molar ratio of 1:1.

[0036] Mix iron and silicon co-precipitate with lithium carbonate, oxalic acid solution, carbon nanotubes, and phenolic resin to form a slurry, ball mill, and Fe 3+ reduced to Fe 2+ , the precursor material for the synthesis of lithium iron silicate is obtained after drying, wherein the amount of oxalic acid added is based on oxalic acid / Fe 3+ The molar ratio is 0.6, the Li / Si molar ratio in the raw material is 2 control, the addition amount of carbon nanotube and phenolic resin is 1% according to the content of carbon nanotube in the lithium iron silicat...

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Abstract

The invention relates to a preparation method of lithium iron silicate cathode material. In the method, ferric saline, Na2SiO3 and lye are added into a reactor in a flowing way; the pH value of the reaction system is controlled, so that the hysrolysis reaction between the ferric iron and the SiO3 can occur; the common deposit of iron and silicon is prepared by filtering and washing; the common deposit of iron and silicon, the lithium source compound, the oxalic acid solution and the carbon source compound are mixedto become pulp state; the Fe is reduced to be Fe through ball milling; the precursor material of lithium iron silicate can be prepared by drying; the precursor material is calcinated under the conditions with the protective atmosphere and at the low temperature to form the agglomerated acidic lithium-iron anode material which is composed of nanoparticles. The method has the strong process adaptability; the industrial production can be easily realized; and the product has higher density and excellent electrochemical properties.

Description

technical field [0001] The invention belongs to the field of electrochemistry, and relates to a preparation method of a lithium iron silicate cathode material for a lithium ion battery. Background technique [0002] The energy crisis and environmental pollution pose severe challenges to human survival, and finding clean and renewable secondary energy is an urgent task to be solved to realize the sustainable development of human society. Among many secondary battery systems, lithium-ion batteries have the advantages of high working voltage, high energy density, long cycle life, low self-discharge rate, and environmental protection, and have become the main trend of secondary battery development. [0003] At present, commercial lithium-ion battery cathode materials mainly use α-NaFeO 2 type layered LiCoO 2 , it has the advantages of easy synthesis and stable charge and discharge performance, but LiCoO 2 The synthesis requires a large amount of scarce and expensive cobalt me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/04H01M4/58
CPCY02E60/12Y02E60/10
Inventor 郭华军李黎明李新海王志兴彭文杰胡启阳张云河
Owner CENT SOUTH UNIV
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