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Preparation method of nano-spinel nickel cobalt lithium manganate

A nano spinel, nickel cobalt lithium manganate technology, applied in chemical instruments and methods, nickel compounds, inorganic chemistry, etc., can solve the problems of poor product batch repeatability, difficult to control particle morphology, and unfavorable industrial production, etc. To achieve the effect of simple and easy process, narrow particle size distribution and short production cycle

Active Publication Date: 2016-12-21
XIANGTAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) High-temperature solid-phase sintering method, which is simple to operate, easy to control the preparation conditions, and easy to carry out industrial production, but the energy consumption is large, the prepared product particles are large, the particle shape is difficult to control, and the product batch repeatability is poor
[0005] (2) Spray pyrolysis method, this method has high powder purity, good shape, uniform particle size distribution, simple process, continuous production, large output, but large particles
[0006] (3) Sol-gel method, etc., this method has a long production cycle and is not conducive to industrial production
However, the particles are large and the process is complicated

Method used

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  • Preparation method of nano-spinel nickel cobalt lithium manganate
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  • Preparation method of nano-spinel nickel cobalt lithium manganate

Examples

Experimental program
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Effect test

Embodiment 1

[0041] A kind of nano-spinel type nickel-cobalt lithium manganese oxide (LiNi 0.5 co 0.05 mn 1.45 o 4 ) preparation method, comprising the following steps:

[0042] The first step, preparation of nano-scale Ni 0.5 co 0.05 mn 1.45 (OH) 2 Precursors, specifically:

[0043] Mix nickel salt, cobalt salt, and manganese salt according to the ratio to form a mixed solution with a total cation concentration of 0.2mol / L; use a spiral channel type rotating bed high-gravity reactor to generate a high-gravity field, and control the high-gravity reactor The rotor speed is 1000rpm, the slurry mixture is placed in the supergravity field for reaction and circulation, and the mixed alkali solution composed of sodium hydroxide and ammonia water is added dropwise to the supergravity field reactor according to the proportioning ratio, and the post-reaction solution ( The pH value is 11.0); the solution after the reaction is filtered, washed with distilled water and dried to obtain nanosca...

Embodiment 2

[0050] Embodiment 2-Example 3 differs from Example 1 in that: the temperature and time of roasting in a microwave muffle furnace have: in Example 2, the roasting temperature is 780 ° C, and the roasting time is 10h; in Example 3 The calcination temperature is 950°C, and the calcination time is 14h.

[0051] Embodiment 2 and embodiment 3 gained nano spinel type LiNi 0.5 co 0.05 mn 1.45 o 4 The XRD test results are detailed in Figure 4 , in combination with Examples 1-3, from Figure 4 It can be seen that under the microwave calcination conditions of 750°C and 950°C, other impurity phases will be produced, and the diffraction peaks of impurities are more obvious. However, under the calcination condition of 880°C, the crystal form is good, and there is no impurity peak. It can be seen that the calcination temperature has a great influence on the crystal form, and it is better to control the calcination temperature at about 880°C in order to obtain nano-nickel cobalt lithiu...

Embodiment 4

[0053] Embodiment 4-Example 5 differs from Example 1 only in the concentration of total cations, specifically: the concentration of total cations in Example 4 is 0.1mol / L, and the concentration of total cations in Example 5 is 0.25mol / L L.

[0054] Embodiment 4-embodiment 5 gained nano spinel type LiNi 0.5 co 0.05 mn 1.45 o 4 The XRD test results are detailed in Figure 5 . In conjunction with embodiment 1, embodiment 4 and embodiment 5 (see Figure 5 ) shows that: when the concentration of total cations is about 0.20mol / L, the crystallinity of the prepared sample is high, and no impurities are produced.

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Abstract

The invention provides a preparation method of nano-spinel nickel cobalt lithium manganate. The method comprises the following steps: 1. preparation of nano nickel cobalt lithium manganate precursor: uniformly mixing a nickel salt, a cobalt salt and a manganese salt to obtain a mixed solution, adding into a hypergravity field reactor, reacting, and sequentially carrying out filtration, washing and filtration on the reaction solution to obtain the nano precursor; and 2. uniformly mixing the nano precursor obtained in the step 1 with a lithium salt, and sequentially carrying out presintering, roasting and annealing to obtain the nano-spinel nickel cobalt lithium manganate. The method has the advantages of simple technique and low cost, is easy to operate, and can implement quick mass production. The prepared nickel cobalt lithium manganate has the advantages of controllable particle size (the average particle size is 200nm or so), narrow particle size distribution, no aggregation, high crystallinity and complete crystal form.

Description

technical field [0001] The invention relates to the technical field of preparation of lithium-ion battery materials, in particular to a nano-spinel type nickel-cobalt lithium manganese oxide LiNi 0.5 co 0.05 mn 1.45 o 4 method of preparation. Background technique [0002] Lithium-ion battery cathode material is the key and core technology for the development of lithium-ion batteries, and it is also the main direction and hotspot of lithium-ion battery research. Integrated LiCoO 2 , LiNiO 2 , LiMnO 2 Advantages of the three classes of materials to form LiCoO 2 / LiNiO 2 / LiMnO 2 The eutectic system can be combined into a new type of transition metal lithium intercalation oxide composite material containing nickel, cobalt and manganese, whose general formula is LiCo x mn y Ni (1-x-y) o 2 (0<x<0.5, 0<y<0.5), its comprehensive performance is better than any single combination compound, and there is an obvious ternary synergistic effect: the main working r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00
CPCC01G53/006C01P2002/72C01P2004/03C01P2004/04C01P2004/62
Inventor 周继承张祖喜隗小山
Owner XIANGTAN UNIV
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