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Preparation method of zinc-based negative electrode material, prepared negative electrode material, negative-electrode plate and lithium battery

A technology of negative electrode material and negative electrode sheet is applied in the field of preparation of zinc-based negative electrode material, which can solve the problems of low lithium ion diffusion rate, restrict the application of lithium titanate, and wide range of powder particle size, and achieve uniform distribution of titanium source, Improved reproducibility and controllability, particle size and composition uniformity

Active Publication Date: 2019-12-17
东北大学秦皇岛分校
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Problems solved by technology

CN106848285A discloses a lithium-poor lithium titanate negative electrode material with a uniform surface. The material obtains a lithium titanate material with a uniform surface by doping other metals other than lithium and titanium in the basic structure lithium titanate material, which is stable However, the relatively low lithium ion diffusion rate, low conductivity and low theoretical capacity restrict the wider application of lithium titanate; therefore, it is necessary to develop a reliable new type of lithium titanate with a lower potential platform Titanate anode material
[0006] CN102583519A discloses a preparation method of zinc titanate-based micro-nano crystal powder, by ball milling, drying and grinding the main raw material and molten salt raw material according to the mass ratio of 1:3-8, and drying again after washing Zinc titanate-based micro-nanocrystalline powder is obtained. The preparation process of the method is simple, but the prepared powder has a wide particle size range, large particle size and uneven distribution
[0007] CN106410264A discloses a method for preparing molten salt of zinc titanate. After mixing nanotube titanic acid, zinc acetylacetonate and molten salt, the zinc titanate material is prepared by ball milling, drying, washing and re-drying. The reaction temperature of the method is Relatively low, the prepared negative electrode material has high capacity and good cycle performance, but the crucible and utensils in the molten salt method will pollute the molten salt, which will easily affect the quality of the product, and the crystallinity is low
[0008] In summary, the existing preparation process of zinc titanate materials still has problems such as uneven particle size, many impurity phases and low crystallinity in the product. Therefore, a new titanic acid with uniform particle size, good dispersion performance and high electrochemical performance has been developed. The preparation process of zinc anode materials is the key to further improving the application prospects of zinc titanate anode materials in the field of lithium batteries

Method used

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  • Preparation method of zinc-based negative electrode material, prepared negative electrode material, negative-electrode plate and lithium battery
  • Preparation method of zinc-based negative electrode material, prepared negative electrode material, negative-electrode plate and lithium battery
  • Preparation method of zinc-based negative electrode material, prepared negative electrode material, negative-electrode plate and lithium battery

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Embodiment 1

[0098] This embodiment provides a method for preparing a zinc-based negative electrode material, the method comprising the following steps:

[0099] (1) Add 0.01mol of zinc citrate under stirring conditions to 110mL mixed solution composed of ethanol, ethylene glycol, formamide and acetonitrile in a volume ratio of 10:10:1:1 to obtain solution A; Tetrabutyl titanate was added to a 30mL mixed solution composed of ethanol and benzyl alcohol in a volume ratio of 2:1 to obtain solution B;

[0100] (2) Add the solution B to the continuously stirring solution A, and simultaneously add 0.01 g of a mixture of sodium stearate and sodium dodecylsulfonate in a mass ratio of 1:8 and 0.01 g of 1-ene Propyl-3-methylimidazolium chloride salt to obtain solution C, and continue to stir vigorously for 10 minutes to make the solution C mix uniformly;

[0101] (3) Heat the solution C in a polytetrafluoroethylene reactor at 180° C. for 6 hours to obtain a mixed solution. The mixed solution is coo...

Embodiment 2

[0108] This embodiment provides a method for preparing a zinc-based negative electrode material, the method comprising the following steps:

[0109] (1) Add 0.01mol zinc citrate to a 110mL mixed solution composed of ethanol and ethylene glycol at a volume ratio of 1:1 under stirring conditions to obtain solution A; add 0.01mol tetrabutyl titanate to ethanol and ethylene glycol Benzyl alcohol is in the 30mL mixed solution that forms by volume ratio 2:1, obtains solution B;

[0110] (2) Add the solution B to the continuously stirring solution A, and simultaneously add 0.01 g of a mixture of sodium stearate and sodium dodecylsulfonate in a mass ratio of 1:8 and 0.01 g of 1-ene Propyl-3-methylimidazolium chloride salt to obtain solution C, and continue to stir vigorously for 10 minutes to make the solution C mix uniformly;

[0111] (3) Heat the solution C in a polytetrafluoroethylene reactor at 180° C. for 6 hours to obtain a mixed solution. The mixed solution is cooled to room t...

Embodiment 3

[0115] This embodiment provides a method for preparing a zinc-based negative electrode material, the method comprising the following steps:

[0116] (1) Add 0.01mol of zinc citrate under stirring conditions to 110mL mixed solution composed of ethanol, ethylene glycol, formamide and acetonitrile in a volume ratio of 10:10:1:1 to obtain solution A; Tetrabutyl titanate was added to 30 mL of benzyl alcohol solution to obtain solution B;

[0117] (2) Add the solution B to the continuously stirring solution A, and simultaneously add 0.01 g of a mixture of sodium stearate and sodium dodecylsulfonate in a mass ratio of 1:8 and 0.01 g of 1-ene Propyl-3-methylimidazolium chloride salt to obtain solution C, and continue to stir vigorously for 10 minutes to make the solution C mix uniformly;

[0118] (3) Heat the solution C in a polytetrafluoroethylene reactor at 180° C. for 6 hours to obtain a mixed solution. The mixed solution is cooled to room temperature and then filtered to obtain a...

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Abstract

The invention provides a preparation method of a zinc-based negative electrode material, the prepared negative electrode material, a negative-electrode plate and a lithium battery. The preparation method comprises the following steps: respectively dissolving a zinc source and a titanium source in an organic solvent; and carrying out mixing, heating, ball milling and sintering to realize uniform mixing of the zinc source and a titanium source. According to the invention, long-time high-energy-consumption high-temperature sintering process is avoided; the problems of easy agglomeration of powder, large granularity and difficulty in acquiring high-purity micropowder in the prior art are overcome; the preparation method has the advantages of simple operation and high reproducibility; and the negative electrode material prepared by using the preparation method has excellent rate capability and stable cycle life, is high in practical use value, and can effectively meet the practical requirements of various application occasions of the lithium ion battery.

Description

technical field [0001] The invention relates to the technical field of lithium ion batteries, in particular to a preparation method of a zinc-based negative electrode material, a negative electrode material, a negative electrode sheet and a lithium battery prepared therefrom. Background technique [0002] With the development of various electronic devices as well as electric vehicles and hybrid vehicles, higher requirements are placed on the batteries that provide energy for them. Among them, lithium-ion batteries have higher capacity density and energy density and are recognized as the most promising. power battery. At present, the anode materials of commercial lithium-ion batteries mostly use various lithium intercalation carbon / graphite materials. However, the lithium intercalation potential (0-0.26V) of carbon materials is very close to the deposition potential of metal lithium. When the battery is overcharged, metal lithium may It will precipitate on the surface of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00H01M4/131H01M4/48H01M10/0525
CPCC01G23/003H01M4/48H01M4/131H01M10/0525C01P2002/72C01P2004/03C01P2006/40Y02E60/10
Inventor 伊廷锋仇立英齐思雨韩梦成刘延国
Owner 东北大学秦皇岛分校
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