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Preparation method of lithium manganese silicate positive pole material

A technology of lithium manganese silicate and cathode material, applied in battery electrodes, electrical components, circuits, etc., can solve the problems of difficult to control reproducibility, harsh reaction conditions, low material purity, etc., to facilitate industrialized large-scale production, reaction Easy-to-control conditions and high-purity results

Active Publication Date: 2014-08-13
SUZHOU GCL ENERGY TECH DEV CO LTD
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its traditional preparation methods mainly include high-temperature solid-phase method, sol-gel method and hydrothermal method, etc., but these methods have the problems of high synthesis temperature, long cycle, or low purity of materials and poor crystallinity.
In 2010, T.Muraliganth et al. synthesized Li by microwave-solvothermal method at 300°C and 30bar pressure. 2 MnSiO 4 Materials (Microwave-Solvothermal Synthesis of Nanostructured Li 2 MSiO 4 / C(M=Mn and Fe)Cathodes for Lithium-Ion Batteries[J].Chem.Mater.,2010,22(20),5754–5761), but the crystallinity is poor, and secondary sintering is required; recently, Devaraju M. Kempaiah et al. used the solvothermal method under harsh conditions (reaction temperature 300 ° C / pressure 38 MPa) to synthesize Li with high purity and good crystallinity. 2 MnSiO 4 Materials (Controlled synthesis of nanocrystalline Li2MnSiO4 particles for high capacity cathode application in lithium-ion batteries[J]Chem.Commun.,2012,48,2698–2700), but this method has harsh reaction conditions, difficult control and poor reproducibility question

Method used

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  • Preparation method of lithium manganese silicate positive pole material
  • Preparation method of lithium manganese silicate positive pole material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take 9ml of ethanol and 1ml of water to prepare a mixed solution, add 5.200g of tetraethyl orthosilicate solution, stir well; add 4.950g of MnCl 2 .4H 2 O, stir evenly; add 2.100g of LiOH to the solution prepared in the above steps, stir evenly; adjust the pH value to 10 with acetic acid and ethylenediamine, and finally put the prepared solution into the reaction kettle, heat the solvent at 220°C React for 48 hours, wash repeatedly with water for 5 times, wash with alcohol twice, filter, and dry at 105°C to obtain lithium manganese silicate material.

[0032] Earned Li 2 MnSiO 4 The X-ray diffraction pattern of the material is as figure 1 As shown, test conditions: Holland PHILIP company Panalytical X-pert powder diffractometer (CuKα ray ), the working voltage is 40kV, and the working current is 50mA; the test parameters are angle range(°): 5°-80°; Step size(°): 0.0167°; Time per step (s): 5s.

[0033] The X-ray diffraction patterns of the products in each time pe...

Embodiment 2

[0035] Take 9ml of ethanol and 1ml of water to prepare a mixed solution, add 1.500g of nano-scale silicon dioxide, stir well; add 4.950g of MnCl 2 .4H 2O, stir evenly; add 2.100g of LiOH to the solution prepared in the above steps, stir evenly; adjust the pH value to 12 with acetic acid and ethylenediamine, and finally put the prepared solution into the reaction kettle, heat the solvent at 220°C React for 48 hours, wash repeatedly with water for 5 times, wash with alcohol twice, filter, and dry at 105°C to obtain lithium manganese silicate material.

Embodiment 3

[0037] Take 9ml of ethanol and 1ml of water to prepare a mixed solution, add 5.200g of tetraethyl orthosilicate solution, stir well; add 6.700g of C 4 h 6 o 4 Mn, stir evenly; add 2.100g of LiOH to the solution prepared in the above steps, stir evenly; adjust the pH value to 9 with acetic acid and ethylenediamine, and finally put the prepared solution into the reaction kettle, heat the solvent at 220°C React for 48 hours, wash repeatedly with water for 5 times, wash with alcohol twice, filter, and dry at 105°C to obtain lithium manganese silicate material.

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Abstract

The invention relates to a lithium ion battery positive pole material, particularly a preparation method of a lithium manganese silicate (Li2MnSiO4) positive pole material for lithium ion batteries. The preparation method comprises the following steps: adding manganese salt, lithium salt and nano silicon dioxide or ethyl orthosilicate as a reactive silicon source into an organic solvent or a mixed solution of an organic solvent and water; adding organic acid or organic amine into the solution as a pH regulator; and carrying out solvothermal reaction on the solution, washing the product, filtering, and drying to obtain the lithium manganese silicate material. The method provided by the invention can be carried out under common hydrothermal reaction kettle conditions without pressurization, thereby enhancing the safety coefficient on the premise of greatly lowering the production cost, and being convenient for industrialized large-scale production.

Description

technical field [0001] The present invention relates to a kind of anode material of lithium ion battery, especially relate to a kind of manganese lithium silicate (Li 2 MnSiO 4 ) Preparation method of cathode material. Background technique [0002] Li 2 MnSiO 4 As a new lithium-ion battery cathode material, it has the advantages of high theoretical specific capacity, stable structure, excellent cycle performance, low price and environmental friendliness. It is considered to be a very competitive cathode material for lithium-ion batteries in the future and is expected to be widely used in lithium Ion power battery. Its traditional preparation methods mainly include high-temperature solid-phase method, sol-gel method and hydrothermal method, etc., but these methods have the problems of high synthesis temperature, long cycle, or low purity of materials and poor crystallinity. In 2010, T.Muraliganth et al. synthesized Li by microwave-solvothermal method at 300°C and 30bar p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58
CPCY02E60/10
Inventor 孙化雨史松君
Owner SUZHOU GCL ENERGY TECH DEV CO LTD