Preparation method of lithium ion battery negative electrode material zinc manganate

A technology for zinc manganate and lithium-ion batteries, applied in battery electrodes, secondary batteries, manganate/permanganate, etc., can solve poor electrochemical performance, complicated preparation process, long preparation cycle, etc. problems, to achieve excellent specific capacity, high product purity, and shortened diffusion distance

Active Publication Date: 2018-02-23
NANJING UNIV OF SCI & TECH
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Problems solved by technology

Xiao et al. selected manganese nitrate and zinc nitrate as manganese source and zinc source respectively, and prepared pure phase ZnMn by hydrothermal method at 160 °C for 48 h. 2 o 4 , the preparation cycle is long, but the electrochemical performance is not good, the initial capacity is only 763mAh / g (Xiao L, et al.Low temperature synthesis of flower-like ZnMn 2 o 4 superstructures with enhanced electrochemical lithium storage[J].Journal ofPower Sources,2009)
Yang et al. used the electrospinning method to spray the precursor of zinc manganate onto the surface of Al foil by electrospray technology at a high voltage of 12kV, and obtained the ZnMn after the fibrous precursor was roasted at high temperature. 2 o 4 , electrochemical behavior tests show that it has good electrochemical stability, but the preparation process is more complicated and requires higher equipment (Yang G, et al. Facile synthesis of interwoven ZnMn 2 o 4 nanofibers by electrospinning and their performance in Li-ion batteries[J].Materials Letters,2014)
At present, ZnMn is prepared by co-precipitation method. 2 o 4 Powder as an electrode material has not yet been reported

Method used

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  • Preparation method of lithium ion battery negative electrode material zinc manganate
  • Preparation method of lithium ion battery negative electrode material zinc manganate
  • Preparation method of lithium ion battery negative electrode material zinc manganate

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Embodiment 1

[0026] (1) Solution preparation: When preparing the solution, weigh 0.01mol of zinc acetate and 0.02mol of manganese sulfate and dissolve them in 100mL of deionized water, weigh 0.15mol of oxalic acid and dissolve them in 100mL of absolute ethanol, and stir until completely dissolved.

[0027] (2) Solution mixing: under vigorous magnetic stirring, the aqueous solution of zinc acetate and manganese sulfate is slowly added dropwise to the ethanol solution of oxalic acid at a rate of 5 mL / min, centrifuged, washed with water and alcohol, and the precipitate is vacuum-dried. get the precursor;

[0028] (3) High temperature sintering: calcining the precursor at 600°C for 3 hours to obtain zinc manganate.

[0029] figure 1 It is the XRD pattern of zinc manganate obtained by sintering the precursor at different temperatures from 300 to 700°C. It can be seen that as the temperature continues to rise, the crystallinity increases and the average particle size increases. The degree of c...

Embodiment 2

[0036] This embodiment is basically the same as Embodiment 1, the only difference is that the rate of addition is 3mL / min. Since manganese sulfate is completely soluble in water and insoluble in ethanol, when the mixed aqueous solution of zinc acetate and manganese sulfate is added to the ethanol solution of ultra-high concentration oxalic acid, in the local area, manganese sulfate and oxalic acid complex, and this complex is easy Mature and grow up. Therefore, when the dropping rate slows down, due to the generation of by-products, the yield of the precursor decreases, resulting in a decrease in the yield of zinc manganate.

Embodiment 3

[0038] This embodiment is basically the same as Embodiment 1, the only difference is that the sintering is carried out at 300, 400, 500, 600, 700, 1000°C. figure 1 It can be seen that with the continuous increase of sintering temperature, ZnMn 2 o 4 The sharper the diffraction characteristic peak of the powder, it shows that the crystallinity is increasing continuously, but at the same time, with the increase of calcination temperature, the broadening phenomenon of the diffraction characteristic peak is weakened, indicating that high temperature sintering leads to the increase of ZnMn 2 o 4 The powder agglomeration phenomenon is aggravated, and the average particle size increases. For the screening of materials, it is necessary to comprehensively consider the influence of crystallinity and agglomeration factors, figure 1 Among them, when the calcination temperature is 600°C and 700°C, there is little difference in the diffraction characteristic peaks between the two, that i...

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Abstract

The invention discloses a preparation method of a lithium ion battery negative electrode material zinc manganate. The method is characterized in that the zinc manganate is prepared through a co-precipitation technology by using oxalic acid as a precipitating agent. The method concretely comprises the following steps: slowly dropwise adding an aqueous solution of a manganese salt and a zinc salt into an ethanol solution of oxalic acid, performing centrifuging, water washing, alcohol washing and vacuum drying to obtain a precursor, and carrying out high temperature calcination on the precursor to obtain the zinc manganate. The method has the advantages of simple process, low cost, large output, easiness in control, short cycle, and convenience in industrial production. The prepared zinc manganate has a meso-porous structure, has excellent specific capacity, cycle performances, rate performances and safety, and has an extremely wide application prospect as a lithium ion battery negative electrode material.

Description

technical field [0001] The invention relates to a preparation method of zinc manganate, a lithium ion negative electrode material, in particular to a method for synthesizing lithium ion negative electrode material zinc manganate by coprecipitation, and belongs to the technical field of inorganic nanometer materials and chemical power sources. Background technique [0002] Lithium-ion batteries are widely used in electronic products, vehicles, military equipment and other fields due to their high specific capacity, long cycle life, good safety performance, and environmental friendliness. In order to pursue higher specific capacity, longer cycle life, and better safety performance of lithium-ion batteries, it is necessary to develop electrode materials with better performance. Nowadays, the anode materials of industrially produced lithium-ion batteries are mostly various carbon materials, but the theoretical specific capacity of carbon materials as the anode is only 372mAh g ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/12H01M4/485H01M4/505H01M10/0525
CPCC01G45/12C01P2002/72C01P2004/03C01P2004/61H01M4/485H01M4/505H01M10/0525Y02E60/10
Inventor 卑凤利于洪珺张玉环刘家伟
Owner NANJING UNIV OF SCI & TECH
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