Preparation method and product of flowerlike lithium manganese phosphate nano-particles

A technology of lithium manganese phosphate and nanoparticles, applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., to achieve the effects of no environmental pollution, easy control, and large specific surface area

Inactive Publication Date: 2015-02-04
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] At present, there are only reports on the synthesis of spindle, flake, bird's nest and amorphous particles at home and abroad, and different particle shapes will show different electrochemical properties. Therefore, it is necessary to develop more manganese phosphate with different shapes. Lithium has important application significance

Method used

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  • Preparation method and product of flowerlike lithium manganese phosphate nano-particles
  • Preparation method and product of flowerlike lithium manganese phosphate nano-particles
  • Preparation method and product of flowerlike lithium manganese phosphate nano-particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Flower-like LiMnPO with a diameter of about 1 μm assembled from nanorods with a diameter of about 100 nm synthesized by hydro / solvothermal method 4 Particles, flower-like LiMnPO was synthesized according to the following process steps 4 nanoparticles.

[0032] 1) Measure ethylene glycol and deionized water at a volume ratio of 1:1, and mix the two to obtain a mixed solvent with a volume ratio of ethylene glycol and water of 1:1.

[0033] 2) Weigh 0.0025mol (0.42g) manganese sulfate (MnSO 4 ·H 2 (2), it is dissolved in the step 1 of 20ml) in the mixed solvent of the preparation of ethylene glycol and water, and the manganese sulfate solution concentration that is formed is adjusted to be: 0.125mol / L (mole per liter).

[0034] 3) According to the molar ratio of lithium sulfate, ammonium dihydrogen phosphate and sodium hydroxide is 3:2:4, namely weigh 0.00375mol (0.48g) lithium sulfate (Li 2 SO 4 ·H 2 O) and 0.0025mol (0.287g) ammonium dihydrogen phosphate ((NH 4 )H...

Embodiment 2

[0038] Water / solvothermal synthesis of flower-like LiMnPO 4 particles.

[0039]Concrete processing step is identical with example 1, and difference is: the volume ratio of ethylene glycol and water in the mixed solvent of preparation in step 1) is: 1:1.5; Step 2) takes by weighing 0.002mol manganese sulfate, and the prepared manganese sulfate The solution concentration is: 0.1mol / L, correspondingly weigh 0.003mol lithium sulfate and 0.002mol ammonium dihydrogen phosphate and 0.004mol sodium hydroxide in step 2), and lithium sulfate concentration in the prepared solution is: 0.15mol / L; In step 4), the reaction precursor suspension in the final reactor accounts for 3 / 4 of the volume of the reactor; in step 5), the heat treatment temperature is 160° C., and the temperature is kept for 24 hours.

Embodiment 3

[0041] Water / solvothermal synthesis of flower-like LiMnPO 4 particles.

[0042] Concrete processing step is identical with example 1, and difference is: the volume ratio of ethylene glycol and water in the mixed solvent of preparation in step 1) is: 1:2; Step 2) takes by weighing 0.004mol manganese sulfate, and the prepared manganese sulfate The solution concentration is: 0.2mol / L, and correspondingly step 2) takes by weighing 0.006mol lithium sulfate and 0.004mol ammonium dihydrogen phosphate and 0.008mol sodium hydroxide, and lithium sulfate concentration in the prepared solution is: 0.3mol / L; In step 4), the reaction precursor suspension in the final reactor accounts for 4 / 5 of the volume of the reactor; in step 5), the heat treatment temperature is 240° C., and the temperature is kept for 8 hours.

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Abstract

The invention discloses a preparation method of flowerlike lithium manganese phosphate nano-particles. The preparation method comprises the following steps: mixing ethylene glycol with water in a volume ratio of 1 to (1-2) to obtain an ethylene glycol/water mixed solvent; taking one part of the ethylene glycol/water mixed solvent to mix with manganese sulfate to obtain a mixed solution I with concentration of 0.1-0.2mol/L; then, taking one part of the ethylene glycol/water mixed solvent to mix with lithium sulfate, ammonium dihydrogen phosphate and sodium hydroxide to obtain a mixed solution II, wherein the concentration of the lithium sulfate in the mixed solution II is 0.15-0.3mol/L; adding the mixed solution I into the mixed solution II, uniformly stirring to obtain a precursor solution, performing hydrothermal reaction for 8-24 hours at 160-240 DEG C, and then, performing post-treatment to obtain the flowerlike lithium manganese phosphate nano-particles. According to the preparation method disclosed by the invention, by precisely controlling the charging sequences and the reaction conditions, a method of preparing the flowerlike lithium manganese phosphate nano-particles is obtained, wherein the method is simple in process and easy to control.

Description

technical field [0001] The invention relates to the field of preparation of inorganic non-metallic materials, in particular to a preparation method and product of flower-shaped lithium manganese phosphate nanoparticles. Background technique [0002] Energy is the most important material basis for human survival and development. With the increasing shortage of traditional fossil energy and the increasing demand for energy, new energy, especially renewable energy, has become a hot spot in the current social and scientific development. Among them, lithium-ion batteries have become an important direction for the current development of new energy because of their advantages such as high energy density, long service life, and low pollution. Olivine structure material lithium manganese phosphate (LiMnPO 4 ), Mn 3+ / Mn 2+ The electrode potential relative to lithium is 4.1V, which is just in the stable chemical window of the existing electrolyte. Under the same specific discharge ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45B82Y30/00B82Y40/00
Inventor 徐刚鲍亮周少雄韩高荣武英曾宏李玲玲任召辉沈鸽
Owner ZHEJIANG UNIV
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