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Pre-lithiation material and preparation method thereof

A pre-lithium and precursor technology, applied in chemical instruments and methods, inorganic chemistry, nickel compounds, etc., can solve the problems of easy agglomeration and segregation of NiO, high activity, complex preparation process, etc.

Active Publication Date: 2021-09-07
XTC NEW ENERGY MATERIALS(XIAMEN) LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Research on pre-lithium materials has been a research hotspot in the field of lithium batteries in recent years. Patent CN 107221650 B mentions a lithium supplement additive and its preparation method. It is completed by mixing various substances in a certain proportion and multi-step sintering, but the active ingredients The purity is low, and the small activity of some product particles makes it difficult to store, and passivation treatment is required, and the process is complicated
Patent CN107819113A discloses a lithium-supplementing additive and its preparation method and application. The lithium-supplementing additive is a core-shell structure, the core material is a conductive carbon material, and the shell material is lithium oxide; lithium oxide is deposited on the surface of the conductive carbon material. Nano-sized lithium oxide particles form nano-layer shells, and the preparation process is complex and difficult
[0006] In existing patents and research, the synthesis of Li 2 NiO 2 The raw materials and methods are mainly to choose Li 2 O / LiOH and the corresponding nickel salt, and adding additives for solid-phase synthesis, but found in the actual synthesis process, although it is possible to synthesize Li 2 NiO 2 sample, but its impurity components are large and the content is low, the main reason is that NiO is easy to agglomerate and segregate during the synthesis process, and the reproducibility is poor

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  • Pre-lithiation material and preparation method thereof

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Embodiment approach

[0040] One embodiment of the present invention provides a method for preparing a pre-lithium material, the main steps of which include:

[0041] S1 selects nickel salt and additives, and uses chemical co-precipitation method to prepare precursor 1;

[0042] S2 calcines precursor 1 under an inert atmosphere to prepare precursor 2;

[0043]S3 performs an induction operation on the precursor 2 to induce a crack structure, and prepares the precursor 3;

[0044] S4 mixes precursor 3 with an equimolar ratio of Li 2 O mixed, sintered and pulverized under an inert atmosphere to prepare a pre-lithium material.

[0045] In one embodiment of the present invention, the nickel salt includes one or more of nickel sulfate, nickel nitrate, nickel chloride, and nickel bromide.

[0046] In one embodiment of the present invention, the additive includes one or a mixture of two or more compounds containing Sr, Y, Nb, Ce, Ta, Mo, W. The compounds of Sr include SrCO 3 , SrO or SrSO 4 , compoun...

Embodiment 1

[0057] Take 10kg of analytically pure nickel sulfate and 0.01g of analytically pure cerium sulfate as raw materials, configure it into a 1mol / L sulfate solution, and mix 5L of sulfate solution with 8L of 1mol / L sodium hydroxide solution and 0.2L of The ratio of 10mol / L ammonia water is added to the reaction vessel for reaction, and the precipitate is filtered, washed and dried to prepare precursor 1, which is denoted as Ni (1-x) Me x (OH) 2 , where Me is Ce, x is 10 -5 ; Sintering under a nitrogen atmosphere, the sintering pressure is 30bar, the sintering temperature is 750 ℃, the sintering time is 60min, and the precursor 2 is prepared, which is recorded as Ni (1-x) Me x O, where Me is Ce and x is 10 -5 ;Add 0.005g of the inducing chemical substance cerium sulfate to the precursor 2, mix evenly, place it in a liquid nitrogen -196°C environment for 60min, and cause the crystal structure to be mutagenized under the cooperation of the low temperature environment and the indu...

Embodiment 2

[0059] Get 10kg of analytically pure nickel chloride and 0.1g of analytically pure niobium pentachloride as raw materials, configure it into a 1mol / L sulfate solution, and mix 5L of sulfate solution with 8L of 1mol / L sodium hydroxide solution and 0.2L of 10mol / L ammonia water is added into the reaction vessel for reaction, and the precipitate is filtered, washed and dried to prepare precursor 1, denoted as Ni (1-x) Me x (OH) 2 , where Me is Nb, x is 10 -3 ; Sintering under a nitrogen atmosphere, the sintering pressure is 30bar, the sintering temperature is 750 ℃, the sintering time is 60min, and the precursor 2 is prepared, which is recorded as Ni (1-x) Me x O, where Me is Nb and x is 10 -3 ;Add 0.02g of induced chemical substance niobium pentachloride to the precursor 2 and mix evenly, then place it in an isostatic pressure environment, press to 150bar, pressurize for 30min, heat to 500°C after decompressing, and heat for 60min , the liquid nitrogen is extremely cooled t...

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Abstract

The invention discloses a pre-lithiation material and a preparation method thereof. The chemical formula of the pre-lithiation material is LiNi (1-x) MexO, x is 10 <-6 >-10 <-1 >, Me is a third metal except Li and Ni; and the pre-lithiation material has the characteristics of high purity, high density, high lithium removal capacity and the like. The invention further discloses a preparation method of the pre-lithiation material; a nickel salt and additives are selected, a crack structure is induced by adopting a chemical coprecipitation method, calcination, an induction environment, an induction chemical substance and a combination of the chemical coprecipitation method, calcination, induction environment and induction chemical substance, a precursor is obtained; and the precursor is mixed with Li2O, the mixture is sintered and smashed, so that the pre-lithiation material can be obtained. According to the method, through the induction effect of the induction environment or the induction chemical substance, a crystal structure is changed, and the unit cell volume is further enlarged, so that lithium ions can fully react with NiO, segregation is reduced, the purity and density of the pre-lithiation material are improved, the lithium removal capacity is further improved, and improvement of the overall electric capacity of a lithium ion battery is promoted.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, in particular to a pre-lithium material, in particular to a high-purity pre-lithium material and a preparation method thereof. Background technique [0002] In order to improve the energy density of lithium-ion batteries, silicon anode materials with high specific capacity are gradually becoming the choice of battery companies and material suppliers, and become one of the most potential anode materials for next-generation lithium-ion batteries. However, the large volume expansion and low first-time Coulombic efficiency of silicon anode limit its practical application. Since the Coulombic efficiency of the positive electrode material is much higher than that of the negative electrode, the capacity of the positive electrode material cannot be fully utilized, resulting in waste of positive electrode materials and a decrease in battery capacity. This is mainly because a solid electroly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00H01M4/485H01M4/525H01M10/0525
CPCC01G53/70C01G53/42C01G53/68H01M4/525H01M10/0525H01M2004/028C01P2004/03H01M4/628Y02E60/10
Inventor 姜龙余柏烈魏国祯林振曾雷英谢能建
Owner XTC NEW ENERGY MATERIALS(XIAMEN) LTD
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