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Method for preparing nano lithium manganese phosphate material with uniform size

A lithium manganese phosphate, size technology, applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problem of large particle size distribution range, and achieve simple equipment, environmental friendliness, and low energy consumption Effect

Inactive Publication Date: 2014-08-20
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, LiMnPO prepared by traditional high-temperature solid-phase method, sol-gel method, hydrothermal method, etc. 4 The size of the material is relatively large, greater than or much greater than 40nm, and the particle size distribution range of the material is also large

Method used

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  • Method for preparing nano lithium manganese phosphate material with uniform size
  • Method for preparing nano lithium manganese phosphate material with uniform size
  • Method for preparing nano lithium manganese phosphate material with uniform size

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 0.08mol of H 3 PO4 is dissolved in a mixed solvent of PEG-400 and distilled water, the volume of PEG-400 is 80mL, the volume ratio of organic solvent to water is 1, H 3 PO 4 The concentration of oleic acid is 0.5mol / L, add LiOH until the pH value of the solution is 9.5, then add 0.032mol oleic acid and stir evenly, the concentration of oleic acid is 0.2mol / L, then add 0.08mol of MnSO 4 , MnSO 4 The concentration of the above solution is 0.5mol / L, transfer the above solution to the reaction kettle, conduct hydrothermal crystallization reaction at 210°C for 5h, open the kettle after cooling at room temperature, centrifuge, wash with deionized water and alcohol for 3 times respectively, at 50 The product was obtained by drying at ℃, and the prepared nano-LiMnPO 4 The scanning electron microscope photograph of the material is as figure 1 As shown, it shows that the prepared product has a uniform size smaller than 40nm.

Embodiment 2

[0019] 0.015mol of H 3 PO4 is dissolved in a mixed solvent of PEG-400 and distilled water, the volume of PEG-400 is 60mL, the volume ratio of organic solvent to water is 0.5, H 3 PO 4 The concentration of oleic acid is 0.08mol / L, add LiOH until the pH value of the solution is 12.5, then add 0.0075mol oleic acid and stir evenly, the concentration of oleic acid is 0.04mol / L, then add 0.015mol of MnSO 4 , MnSO 4 The concentration of the solution is 0.08mol / L, the above solution is transferred to the reaction kettle, and the hydrothermal crystallization reaction is carried out at 140°C for 12 hours. After cooling at room temperature, the kettle is opened, centrifuged, washed with deionized water and alcohol for 3 times, and at 70 The product was obtained by drying at ℃, and the prepared nano-LiMnPO 4 The X-ray diffraction pattern of the material is as figure 2 As shown, the description has a pure composition and a small particle size.

Embodiment 3

[0021] 0.018mol of H 3 PO4 is dissolved in a mixed solvent of PEG-400 and distilled water, the volume of PEG-400 is 100mL, the volume ratio of organic solvent to water is 0.2, H 3 PO 4 The concentration of oleic acid is 0.03mol / L, add LiOH until the pH value of the solution is 13, then add 0.012mol oleic acid and stir evenly, the concentration of oleic acid is 0.02mol / L, then add 0.018mol of MnSO 4 , MnSO 4 The concentration of the above solution is 0.03mol / L, the above solution is transferred to the reaction kettle, and the hydrothermal crystallization reaction is carried out at 90 ℃ for 30 hours. The product was obtained by drying at ℃, and the prepared nano-LiMnPO 4 The transmission electron microscope photographs of the material are as image 3 As shown, it shows that the prepared product has a uniform size smaller than 40nm.

[0022] It can also be clearly seen from the accompanying drawings of the above embodiments that the product prepared by the present invention ...

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Abstract

The invention provides a method for preparing a nano lithium manganese phosphate material with uniform size. The method comprises the steps of adding H3PO4 into a mixed solvent consisting of an organic solvent and water, wherein the organic solvent and the water are in volume ratio of (0.2-1) to 1; adding LiOH, and adjusting the pH value to be 9.5 to 13; adding oleic acid and uniformly stirring, wherein the concentration of oleic acid is 0.02 to 0.2mol / L; adding MnSO4, and maintaining the molar ratio of Mn elements and P elements to be 1 to 1; transferring the solution into a hydrothermal reaction kettle and reacting for 5h to 30h under the temperature of 90 to 210 DEG C; cooling at room temperature, then opening the hydrothermal reaction kettle, filtering the solution, separating the mixture, and drying a product at the temperature of 50 to 90 DEG C to obtain the nano lithium manganese phosphate material with uniform size. The size of the material is uniform and is smaller than 40nm, the device is simple, and the energy consumption is low; the method has the characteristics that raw materials are easily available and environmentally friendly.

Description

technical field [0001] The invention belongs to the field of synthesis of inorganic nanometer materials. More specifically, it relates to a method for preparing nano-manganese lithium phosphate materials with uniform and controllable shape and size by using a surfactant solvothermal method. Background technique [0002] Nano-lithium manganese phosphate (LiMnPO 4 ) is a positive electrode material used in lithium-ion batteries, and has gradually attracted attention due to its high stability and low cost of polyanionic phosphate. LiFePO in the same polyanionic lithium phosphate cathode material 4 The fastest growing, but relative to Li + The electrode potential of / Li is only 3.4V, which is increasingly unable to meet the needs of high-power discharge; LiCoPO 4 It has a high redox potential (4.8V), but the high price of raw materials and its own toxicity limit its application; LiNiPO 4 It is the oxidation-reduction potential is too high (5.2V), beyond the working voltage ...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M4/62B82Y30/00
CPCB82Y30/00B82Y40/00H01M4/5825H01M4/62H01M10/0525Y02E60/10
Inventor 孙晓红李家洪郑春明
Owner TIANJIN UNIV
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