A kind of preparation method of single crystal large particle of ternary material

A ternary material, large particle technology, applied in electrical components, electrode manufacturing, structural parts, etc., can solve the problems of incomplete combination of main metal elements released by carbonate, large amount of additives, waste, etc., to prevent particle growth. Uniform phenomenon, the effect of preventing uneven distribution of flux

Active Publication Date: 2021-08-31
RISESUN MENGGULI NEW ENERGY SCIENCE & TECHNOLOGY CO LTD
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Problems solved by technology

Patent application CN108232186A discloses that in the synthesis of single crystal particles, an expanded precursor is prepared by a polymer template, and then the powder with volume expansion after thermal polymerization is sintered to obtain the required single crystal positive electrode material, but this method is in the process of preparing The introduction of strong acids such as nitric acid and sulfuric acid in the process of precursors in order to improve solubility and achieve uniform mixing will pollute the environment
Patent application CN106159251A discloses the method of adding flux to reduce the melting point of the material, which reduces the number of sintering times and sintering time in the current single crystal material synthesis process, but the flux, precursor and lithium source are mixed by mechanical mixing. Uniformity of mixing and consistency of single crystal growth rate cannot be guaranteed
At the same time, the literature "Zhong Weipan et al." different precipitants have different effects on the prepared LiNi(0.8)Co(0.1)Mn(0.1)O 2 A study on the influence of positive electrode materials on the performance of "[J]. Functional Materials, 2012, 43(11): 1425-1430." Ionic compounds NaOH and NaOH were used in 2 CO 3 As a precipitating agent for the reaction, since the precipitating agent used is an ionic compound, the carbonate group is released quickly when it meets water, and the combination with the main metal element is not complete, so the amount of the auxiliary agent required is large, which is prone to pollution and waste.

Method used

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  • A kind of preparation method of single crystal large particle of ternary material
  • A kind of preparation method of single crystal large particle of ternary material
  • A kind of preparation method of single crystal large particle of ternary material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The reaction mechanism for preparing NCM523 precursor is as follows:

[0047] NH 2 CONH 2 +H 2 O→2NH 3 +CO 2 (1)

[0048] NH 3 +H 2 O→NH 4 + +OH- (2)

[0049] CO 2 +OH - →CO 3 2- +H 2 O (3)

[0050] 0.5Ni 2+ +0.2Co 2+ +0.3Mn 2+ +CO 3 2- →Ni 0.5 co 0.2 mn 0.3 CO 3 (4)

[0051] Ni 0.5 co 0.2 mn 0.3 CO 3 +Li + +1 / 2O 2 →LiNi 0.5 co 0.2 mn 0.3 o 2 +CO 2 (5)

[0052] Table 1. NCM523 (LiNi 0.5 co 0.2 mn 0.3 o 2 ) Experimental scheme for the preparation of large single crystal particles

[0053]

[0054] Experimental steps:

[0055] (1) Prepare 4 beakers marked as 1#, 2#, 3#, 4#, and weigh 100mL deionized water respectively;

[0056] (2) template agent 1 and 2 of experimental scheme in table 1, fluxing agent are dissolved in 1#, 2#, 3#, 4# beaker according to scheme respectively to obtain mixed solution;

[0057] (3) then take cobalt source, nickel source and manganese source respectively according to the amount calculated in ta...

Embodiment 2

[0062] Table 2. NCM622 (LiNi 0.6 co 0.2 mn 0.2 o 2 ) Experimental scheme for the preparation of large single crystal particles

[0063]

[0064] Experimental steps:

[0065] (1) Prepare 4 beakers marked as 1#, 2#, 3#, 4#, and weigh 200mL deionized water respectively;

[0066] (2) template agent 1 and 2 of experimental scheme in table 1, fluxing agent are dissolved in 1#, 2#, 3#, 4# beaker according to scheme respectively to obtain mixed solution;

[0067] (3) then take cobalt source, nickel source and manganese source respectively according to the amount calculated in table 1 and be respectively placed in 1#, 2#, 3#, 4# beakers and fully dissolve to obtain metal mixed solution;

[0068] (4) Finally, put the urea calculated in Table 1 into the mixed metal solution, fully dissolve it, transfer it to a hydrothermal reaction kettle, and place the sealed reaction kettle in an oven at 200°C for 16 hours to obtain the NCM622 precursor solution;

[0069] (5) After filtering, ...

Embodiment 3

[0072] Table 3. NCM811 (LiNi 0.8 co 0.1 mn 0.1 o 2 ) Experimental scheme for the preparation of large single crystal particles:

[0073]

[0074] Experimental steps:

[0075] (1) Prepare 4 beakers marked as 1#, 2#, 3#, 4#, and weigh 180mL deionized water respectively;

[0076] (2) template agent 1 and 2 of experimental scheme in table 1, fluxing agent are dissolved in 1#, 2#, 3#, 4# beaker according to scheme respectively to obtain mixed solution;

[0077] (3) then take cobalt source, nickel source and manganese source respectively according to the amount calculated in table 1 and be respectively placed in 1#, 2#, 3#, 4# beakers and fully dissolve to obtain metal mixed solution;

[0078] (4) Finally, put the urea calculated in Table 1 into the mixed metal solution, fully dissolve it, transfer it to a hydrothermal reactor, and place the sealed reactor in an oven at 180°C for 12 hours to obtain the NCM811 precursor solution;

[0079] (5) After the precursor solution syn...

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Abstract

The invention provides a method for preparing large single crystal particles of ternary materials, which belongs to the field of lithium ion batteries. The preparation method mainly includes the following steps: (1) mixing the main element raw materials of the ternary material, a uniform precipitant, a templating agent, and a fluxing agent in deionized water according to a certain stoichiometric ratio to obtain a mixed solution; (2) mixing the mixed solution Transfer to the reaction kettle, keep it at a certain temperature for a period of time to carry out hydrothermal reaction to obtain the corresponding uniform ternary material precursor; (3) the precursor is added to the lithium source and then calcined at a high temperature to obtain single crystal particles. The present invention uses urea as a uniform precipitant, which can slowly and uniformly release CO in the solution 3 2‑ The ion overcomes the uneven local distribution caused by directly adding the precipitating agent from the outside; the template agent and the soluble flux are uniformly added to the precursor by the hydrothermal method, which can effectively prevent agglomeration.

Description

technical field [0001] The invention belongs to the field of lithium ion battery materials, and in particular relates to a method for preparing large single crystal particles of ternary materials. Background technique [0002] With the innovation of new energy material research and development technology, lithium-ion batteries with advantages such as low-carbon environmental protection, high energy density, and wide operating temperature range have received widespread attention. At present, LiFeO with good safety is mostly used as the positive electrode material of lithium ion battery on the market. 4 , but LiFeO 4 Low capacity is not enough to meet the increasing demand for high energy density batteries, so ternary materials have become a research hotspot due to their high energy density. Ternary materials are mostly spherical, and the primary particle size is generally around several hundred nanometers. Side reactions between surface particles and electrolyte are prone t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/485H01M4/505H01M4/525H01M10/0525H01M4/04
CPCH01M4/0402H01M4/485H01M4/505H01M4/525H01M10/0525Y02E60/10
Inventor 刘建红刘贵娟王伟臣王兴勤
Owner RISESUN MENGGULI NEW ENERGY SCIENCE & TECHNOLOGY CO LTD
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