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Preparation of hollow Mn2O3 micro-spheres and application method thereof in lithium battery

An application method, the technology of microspheres, applied in the direction of lithium batteries, battery electrodes, non-aqueous electrolyte batteries, etc., can solve the problems of complex preparation methods of synthetic hollow structures, unfavorable commercial promotion, high cost, etc., to achieve commercial promotion, Good cycle stability, low cost effect

Active Publication Date: 2017-02-22
SHANGHAI HUIJUE NETWORK COMM EQUIP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the preparation methods for the synthesis of hollow structures reported so far are complicated and expensive, which is not conducive to commercialization.

Method used

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  • Preparation of hollow Mn2O3 micro-spheres and application method thereof in lithium battery
  • Preparation of hollow Mn2O3 micro-spheres and application method thereof in lithium battery
  • Preparation of hollow Mn2O3 micro-spheres and application method thereof in lithium battery

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: Preparation of Mn-BTC microspheres

[0029] At room temperature at 25°C, drop a mixed solution of 10 mL of ethanol containing 90 mg of trimesic acid and water (volume ratio of 1:1) into 10 mL of ethanol containing 49 mg of manganese acetate tetrahydrate and 0.3 g of polyvinylpyrrolidone and In a mixed solution of water (volume ratio 1:1), stir evenly, let stand for 24 hours, and centrifuge to obtain the precursor Mn-BTC (complex formed by manganese and trimesic acid) microspheres. X-ray diffraction of the precursor Figure such as figure 1 As shown, the appearance characteristics are as figure 2 shown.

[0030] figure 2 are scanning electron microscope (SEM) and transmission electron microscope (TEM) pictures of precursors at different magnifications. It can be seen from the figure that the precursor exists in the form of microspheres with a uniform shape, a particle size of about 2 μm, and a solid structure.

Embodiment 2

[0031] Example 2: Preparation of hollow Mn 2 o 3 microsphere

[0032] The precursor Mn-BTC microspheres obtained in Implementation 1 were placed in a muffle furnace, and the temperature was raised to 450° C. at a rate of 10° C. / min in an air atmosphere. Then calcined at this temperature for 2 hours, after natural cooling to room temperature, the hollow Mn 2 o 3 Microspheres (Mn 2 o 3 -10R). The chemical composition of the calcined product can be determined by X-ray diffraction to determine, such as image 3 shown. From image 3 It can be seen that the X-ray diffraction peak of the obtained product is consistent with the standard JCPDS card No.41-1442, indicating that the obtained sample is Mn 2 o 3 . In addition, through the scanning electron microscope and transmission electron microscope photographs of different magnifications of the product, Mn 2 o 3 The appearance characteristics of -10R were analyzed by nitrogen adsorption experiment. Such as Figure 4 As s...

Embodiment 3

[0033] Embodiment 3: the influence of heating rate on product

[0034] As with other conditions in Example 2, the precursor Mn-BTC microspheres were heated up to 450°C at a rate of 5°C / min and 2°C / min, respectively, and then calcined at this temperature for 2 hours to obtain the black product Mn 2 o 3 -5R and Mn 2 o 3 -2R. and the samples calcined at a rate of 10°C / min to 450°C (Mn 2 o 3 -10R), as in image 3 As shown, all obtained are Mn 2 o 3 . Figure 5 Corresponding to Mn in 2 o 3 -5R and Mn 2 o 3 -SEM pictures and TEM pictures at different magnifications of 2R. From Figure 5 It can be seen from the figure that when the heating rate is reduced from 5°C / min to 2°C / min, the product still maintains a spherical appearance, but the degree of damage of the hollow spheres is increasing. And, Mn 2 o 3 The hollow sphere structure of -10R is relatively Mn 2 o 3 -5R and Mn 2 o 3 -2R is relatively complete. Therefore, as the heating rate decreases, the degree of...

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Abstract

The invention discloses preparation of hollow Mn2O3 micro-spheres and an application method thereof in a lithium battery. Preparation includes the following steps that a mixed solution of ethyl alcohol containing trimesic acid and water is added dropwise into a mixed solution of ethyl alcohol containing manganese acetate tetrahydrate and polyvinylpyrrolidone and water, wherein the content of trimesic acid is 80-100 mg / 10 ml of ethyl alcohol, the content of manganese acetate tetrahydrate is 40-60 mg / 10 ml of ethyl alcohol, the content of polyvinylpyrrolidone is 0.2-0.5 g / 10 ml of ethyl alcohol, and the mixture solution is standing still after magnetic stirring and then centrifugally separated to obtain Mn-BTC micro-spheres; the obtained micro-spheres are placed in a muffle furnace and calcined in the air atmosphere, wherein the temperature rising speed is 2-10 DEG C / min, and the hollow Mn2O3 micro-spheres are obtained after calcination. The preparation has the advantages that the hollow Mn2O3 micro-spheres are simple in preparing process, uniform in morphology and large in specific surface and has great application potentiality in lithium ion batteries and electrochemistric energy storage; the method is simple, efficient, safe, easy to implement, short in period and capable of being popularized and industrially applied.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a hollow Mn 2 o 3 Preparation of microspheres and their application in lithium batteries. Background technique [0002] Due to their high energy density and power density, lithium batteries are widely used in mobile energy storage devices for electric vehicles and electronic products. Compared with graphite, the traditional lithium battery anode material, transition metal oxides have higher specific capacity. Among many transition metal oxides, manganese-based oxides (such as MnO, MnO 2 , Mn 2 o 3 and Mn 3 o 4 ) is abundant on the earth, cheap, and does not cause any harm to the environment. In addition, these manganese-based oxides have high output voltage and low operating voltage. [0003] In 2015, the British "Science Bulletin" magazine (Sci.Rep., 2014, Volume 5, page 14686) reported that Mn 2 o 3 Has a higher theoretical specific capacity (1018mAh...

Claims

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Application Information

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IPC IPC(8): C01G45/02H01M4/50H01M10/052
CPCC01G45/02C01P2002/74C01P2004/34C01P2004/61C01P2006/12C01P2006/14C01P2006/16H01M4/50H01M10/052Y02E60/10
Inventor 郑方才
Owner SHANGHAI HUIJUE NETWORK COMM EQUIP
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