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Nanorod assembled lithium manganese iron phosphate microspheres, composite material and preparation method thereof

A technology of lithium iron manganese phosphate and carbon composite material, applied in phosphorus compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of high energy consumption, long reaction time, etc. The effect of small diffusion distances

Active Publication Date: 2017-12-19
ADVANCED TECHNOLOGY & MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently, the synthetic LiMnPO 4 The main methods include high-temperature solid phase, high-energy ball milling, etc., with long reaction time and high energy consumption

Method used

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  • Nanorod assembled lithium manganese iron phosphate microspheres, composite material and preparation method thereof
  • Nanorod assembled lithium manganese iron phosphate microspheres, composite material and preparation method thereof
  • Nanorod assembled lithium manganese iron phosphate microspheres, composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Example 1LiMnFePO 4 Preparation of microspheres and their composites

[0049] Aqueous / solvothermal synthesis of LiMnFePO with a diameter of about 2 μm 4 microspheres, which were used to assemble LiMnFePO 4 The diameter of the primary structure LiMnFePO4 nanorod of the microsphere is 20-50 nanometers.

[0050] The preparation method is as follows:

[0051] (1) Measure ethylene glycol and deionized water, and mix the two to obtain a mixed solvent of ethylene glycol and water with a volume ratio of 1:1.

[0052] (2) Weigh 0.169g manganese sulfate (MnSO 4 ·H 2 O) and 0.417g ferrous sulfate (FeSO 4 ·7H 2 (2) was dissolved successively in a mixed solvent of ethylene glycol and water with a total volume of 20ml to obtain solution A (ie the first mixed solution).

[0053] (3) Weigh 0.48g lithium sulfate (Li 2 SO 4 ·H 2 O), 0.2875g ammonium dihydrogen phosphate ((NH 4 )H 2 PO 4 ) and 0.21g potassium hydroxide (KOH), were dissolved successively in another solvent wi...

Embodiment 2

[0061] Water / Solvothermal Synthesis of LiMnFePO 4 Nanorod assembled microspheres, the diameter of the microspheres is not more than 1.5 microns, and the primary structure of the microspheres is LiMnFePO 4 The diameter of the nanorods is not greater than 50 nanometers.

[0062] Except that the following process is different from Example 1, other process steps are the same as Example 1, the difference is: the volume ratio of ethylene glycol and water in the mixed solvent prepared in step (1) is 1:1.5; Take by weighing 0.38g manganese sulfate and 0.07g ferrous sulfate; Take by weighing 0.16g lithium sulfate and 0.383g ammonium dihydrogen phosphate and 0.28g potassium hydroxide in step (3); In step (5), water / solvothermal reaction temperature at 160° C., and keep warm for 24 hours; in step (6), the organic carbon source is selected as sucrose, and the inert atmosphere is nitrogen.

[0063] Figure 5 LiMnFePO prepared for this example 4 The X-ray diffraction (XRD) pattern of th...

Embodiment 3

[0066] Water / Solvothermal Synthesis of LiMnFePO 4 Nanorods assemble microspheres.

[0067] Except that the following process is different from Example 1, other process steps are the same as Example 1, the difference is: the volume ratio of ethylene glycol and water in the mixed solvent prepared in step (1) is 1:2; , the temperature of the water / solvothermal reaction is 240°C, and the temperature is kept for 8 hours.

[0068] LiMnFePO prepared from this example 4 The scanning electron microscope (SEM) picture of the microspheres shows that the LiMnFePO 4 The nanorod-assembled microspheres are 2 microns in diameter, and the primary structure of the microspheres is LiMnFePO 4 The diameter of the nanorod is 50 nanometers, the product has uniform appearance and good dispersion.

[0069] The charging and discharging performance test of the composite material prepared in this example: the lithium iron phosphate-carbon composite material prepared in this example is used as the pos...

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Abstract

The invention relates to a nanorod-assembled lithium iron manganese phosphate microsphere and a composite material and preparation methods thereof, belonging to the technical field of preparation of new-energy materials. The preparation method for the microsphere comprises the following steps: dissolving reaction materials consisting of lithium sulfate, ammonium biphosphate and potassium hydroxide in a mixed solvent composed of glycol and water; then dissolving manganese sulfate and ferrous sulphate in the mixed solvent composed of glycol and water; mixing the two obtained solutions under stirring and adding the obtained mixture into in an enclosed reaction vessel system for a hydro / solvothermal reaction; and then carrying out filtering, drying and the like to obtain LiMnFePO4 nanorod-assembled microsphere. The preparation method only needs one-step hydrothermal reaction to prepare the microsphere, is simple to operate and has low cost due to usage of common raw materials and reagents. The LiMnFePO4 microsphere with a diameter of no more than 3 [mu]m is prepared through assembling of the LiMnFePO4 nanorod with a diameter of no more than 50 nm. With such a structure, the electrochemical performance of the material can be perfectly improved.

Description

technical field [0001] The invention belongs to the technical field of preparation of new energy materials, and relates to lithium manganese iron phosphate microspheres, a positive electrode material of lithium batteries, and a preparation method thereof, in particular to nanorod-assembled lithium manganese iron phosphate microspheres, a composite material and a preparation method thereof. Background technique [0002] Energy is the most important material basis for human survival and development. The development of clean and renewable energy is one of the key technologies that will affect the future development of the world, and it is also a hot spot in the current social and scientific development. Among them, lithium-ion batteries have become the first choice for future energy storage and portable batteries due to their unique advantages such as large specific energy, high cell voltage, small self-discharge, no memory effect, and no pollution. Among them, the olivine stru...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/45H01M4/36H01M4/58
CPCY02E60/10
Inventor 周少雄曾宏武英况春江徐刚韩高荣
Owner ADVANCED TECHNOLOGY & MATERIALS CO LTD
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