Preparation method of magnesium-doped lithium nickel cobalt oxide anode material for lithium ion battery

A technology for lithium-magnesium-nickel-cobaltate and lithium-ion batteries, which is applied in the field of preparation of high-density magnesium-nickel-nickel-cobaltate positive electrode materials for lithium-ion batteries, can solve the problems of complex process, high difficulty in industrialization, and large crystal size, and achieve The effect of simple process and low cost

Active Publication Date: 2012-04-11

HENGDIAN GRP DMEGC MAGNETICS CO LTD

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Problems solved by technology

Chinese patent document CN03112435.6 announced "the method for preparing lithium cobaltate lithium ion battery anode material with nano-cobalt tetroxide as raw material". This method is a traditional high-temperature solid-phase synthesis method. The material has a wide particle size distribution range, large crystal size, and poor electrochemical performance.

The Chinese patent document CN200810052730 announced "the preparation method of doped and surface-coated lithium nickel cobalt oxide...

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Abstract

The invention belongs to the technical field of battery material preparation, and in particular relates to a preparation method of a magnesium-doped lithium nickel cobalt oxide anode material for a lithium ion battery. The preparation method comprises the following steps: proportionally preparing a Li source, a Ni source, a Co source and a Mg source, and mixing the materials by wet ball-milling to obtain blended slurry; spray-drying the blended slurry; preheating the dried material in a heat treatment atmosphere to obtain a pre-sintering material; pulverizing the pre-sintered material, adding a PVA (polyvinyl alcohol) binder, and compacting to obtain a dense block; heating the compacted block and performing heat preservation in the heat treatment atmosphere to obtain a sintered material; and finally cooling, pulverizing, and screening the sintered material to obtain the magnesium-doped lithium nickel cobalt oxide anode material. The magnesium-doped lithium nickel cobalt oxide anode material prepared by the method has the characteristics of uniform particle distribution, high capacity and high tap density. The preparation method has the advantages of simple process and low cost, thus being applicable to industrial production.

Application Domain

Cell electrodes

Technology Topic

Cobalt oxideLithium electrode +7

Image

Examples

Experimental program(2)

Example Embodiment

[0031] Example 1

[0032] (1) According to the molar ratio of Li:Ni:Co:Mg of 1.01:0.8:0.15:0.05, weigh the reactant material LiOH·H with higher purity 2 O, Ni(OH) 2 , Co 3 O 4 , MgO;

[0033] (2) The prepared raw materials are proportioned as material: alcohol: water: zirconium balls=1:0.05:2:4 (wt%), and perform wet ball milling and mixing for 10 hours. The particle size of the mixed slurry is 0.5 ~1.5μm;

[0034] (3) Spray drying the mixed slurry;

[0035] (4) Put the dry material into a ceramic bowl, put it in a tube furnace and heat it up in an oxygen atmosphere of 1.5 atmospheres of oxygen pressure for pre-heat treatment, the heating rate is 15℃/min, and the temperature is kept at 400℃ Pre-fired for 2 hours to obtain the pre-fired material;

[0036] (5) Crush the pre-fired material to a particle size of 2 ~ 5μm, add 0.5wt% PVA binder to the pre-fired material, at 1800kg/cm 3 Under pressure, press into a compact block;

[0037] (6) Put the compacted block into a ceramic bowl in a tube furnace, heat it up and keep it warm at an oxygen pressure of 2 atmospheres, at a temperature rising rate of 10℃/min, calcine at 750℃, and keep it warm for 15 hours to obtain a sintered material;

[0038] (7) Cool the ceramic bowl containing the fully reacted sintering material at a rate of 10°C/min. After the temperature is lowered to room temperature, pour the sintered material out and pulverize and sieving together. Airflow crushing, sieving, and classification Obtained grain diameter is 8μm, tap density is 2.5g/cm 3 The chemical formula is LiNi 0.8 Co 0.15 Mg 0.05 O 2 The high-density magnesium-doped lithium nickel cobalt oxide cathode material.

[0039] After inspection, the particles of the magnesium-doped lithium nickel cobalt oxide cathode material are uniformly distributed, and the average primary grain size is 0.5μm (see figure 1 ); 0.5C discharge capacity up to 180mAh/g (see figure 2 ); 1C cycle 100 times capacity attenuation is 4.5% (see image 3 ).

Example Embodiment

[0040] Example 2

[0041] (1) According to the molar ratio of Li:Ni:Co:Mg of 1.01:0.8:0.15:0.05, weigh the reactant materials with higher purity: lithium carbonate, nickel carbonate, cobalt carbonate, and magnesium carbonate;

[0042] (2) The prepared raw materials are proportioned as material: alcohol: zirconium balls=1:0.05:2.5:4 (wt%), and wet ball milling is carried out for 12 hours, and the particle size of the mixed slurry is 0.5-1.5 μm;

[0043] (3) Spray drying the mixed slurry;

[0044] (4) Put the dry material into a ceramic bowl, heat it in a tube furnace, heat up in an oxygen atmosphere of 1.5 atmospheres of oxygen pressure for pre-heat treatment, the heating rate is 10℃/min, and keep it at 450℃ Pre-fired for 2 hours to obtain the pre-fired material;

[0045] (5) Crush the pre-fired material to a particle size of 2 ~ 5μm, add 0.5wt% PVA binder to the pre-fired material, at 1800kg/cm 3 Under pressure, press into a compact block;

[0046] (6) Put the compacted block into a ceramic bowl in a tube furnace, and heat it up and heat it under an oxygen pressure of 2 atmospheres at a rate of 10°C/min, calcine at 800°C, and keep it for 10 hours to obtain a sintered material;

[0047] (7) Cool the ceramic bowl containing the fully reacted sintering material at a cooling rate of 20°C/min. After the temperature is lowered to room temperature, the sintering material is poured out, crushed and sieved together, and crushed and sieved by airflow. The obtained grain diameter is 10μm and the tap density is 2.6g/cm 3 The chemical formula is LiNi 0.8 Co 0.15 Mg 0.05 O 2 High-density magnesium-doped lithium nickel cobalt oxide cathode material.

[0048] Upon inspection, the particles of the magnesium-doped lithium nickel cobalt oxide cathode material are uniformly distributed, with an average primary crystal size of 0.6 μm; a discharge capacity of 175 mAh/g at 0.5C; and a capacity decay of 5% after 100 cycles of 1C.

[0049] Experimental research shows that, except for the above-mentioned optimal implementation, the main process parameters of the present invention are controlled within the scope disclosed in the content of the invention: as in step (1): the mole ratio of Li:Ni:Co:Mg is 1:0.7~0.9 :0.1~0.2: 0~0.1 and ≠0, lithium salt is nitrate, nickel salt, cobalt salt or magnesium salt is oxalate, nitrate; in step (4): the heating rate is 5-30°C/min, The heat preservation range is 350~500℃, and the heat preservation time is 0.5~3 hours; in step (5): the amount of PVA binder added is 0.2~0.8 wt% based on the pre-fired material; in step (6): the heating rate is 5~20℃/min, heat preservation range is 750~850℃, heat preservation time is 5~20 hours. The average primary grain size is 0.5~1μm, the 0.5C discharge capacity range is 170~180mAh/g, and the tap density is 2.5~2.8g/cm. 3 , The nucleus whose capacity is decayed within 5% after 100 cycles of 1C is LiNixCoyMgzO 2 The particle size of the composite particles is 5-15 μm, and the inventor will not repeat them here.

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PUM

Property	Measurement	Unit
Granularity	0.5 ~ 1.5	µm
Particle size	2.0 ~ 5.0	µm
Tap density	0.0 ~ 2.8	g/cm³
tensile		MPa
Particle size		Pa
strength	10

Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

Uniform particle distribution
Increase capacity

Preparation method of magnesium-doped lithium nickel cobalt oxide anode material for lithium ion battery

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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