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Preparation method of layered manganese-based cathode material for raising initial charge/discharge efficiency

A technology of charge-discharge efficiency and positive electrode material is applied in the field of preparation of positive electrode active materials for lithium-ion batteries, which can solve the problems of phase composition control of transition metal ions, deviation of transition metal ion ratio from stoichiometry, waste of raw materials, etc., so as to improve the first charge-discharge efficiency. , Precise control of chemical composition, improved charge-discharge efficiency and cycle stability

Inactive Publication Date: 2012-05-09
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, transition metal ions are lost to varying degrees during washing, resulting in waste of raw materials. The most serious is that the ratio of transition metal ions deviates from stoichiometry, so that the concentration of transition metal ions and the phase composition of the final synthesis product cannot be controlled.

Method used

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  • Preparation method of layered manganese-based cathode material for raising initial charge/discharge efficiency
  • Preparation method of layered manganese-based cathode material for raising initial charge/discharge efficiency
  • Preparation method of layered manganese-based cathode material for raising initial charge/discharge efficiency

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Weigh nickel nitrate and manganese nitrate with a molar ratio of 0.75:1.25 to prepare a 1mol / l mixed solution, use ammonium bicarbonate as a precipitant, and add ammonia water dropwise at the same time to control the pH value to 8, and coprecipitate for 10 hours.

[0029] 2) Filter out the co-precipitation product, add deionized water to prepare a slurry with a concentration of 180g / l, and spray dry the slurry at 115°C to obtain nickel-manganese carbonate powder;

[0030] 3) Grinding the nickel-manganese carbonate powder, incubating at 300°C for 5.5 hours, then raising the temperature to 450°C for 2 hours to obtain the precursor powder;

[0031] 4) Weigh lithium hydroxide monohydrate with a molar number of 1.02 (K[1+x / (2+x)], where K=0.92), grind and mix with the precursor powder obtained above, and roast at 800°C for 8 hour, synthesize 0.25Li 2 MnO 3 0.75LiNi 1 / 2 mn 1 / 2 o 2 (xLi 2 MnO 3 ·(1-x)LiNi 1 / 2 mn 1 / 2 o 2 , where x=0.25) powder;

[0032] 5) 0.25Li...

Embodiment 2

[0035] 1) Weigh nickel nitrate and manganese nitrate with a molar ratio of 0.6:1.4 to prepare a 1.5mol / l mixed solution, use ammonium bicarbonate as a precipitant, and add ammonia water dropwise at the same time, control the pH value to 9, and co-precipitate for 8 hours.

[0036] 2) Filter out the co-precipitation product, add deionized water to prepare a slurry with a concentration of 150g / l, and spray dry the slurry at 120°C to obtain nickel-manganese carbonate powder;

[0037] 3) Grinding the nickel-manganese carbonate powder, incubating at 320°C for 4 hours, then raising the temperature to 500°C for 3 hours to obtain the precursor powder;

[0038] 4) Weigh lithium hydroxide monohydrate with a molar number of 1.11 (K[1+x / (2+x)], where K=0.95), grind and mix with the precursor powder obtained above, and roast at 850°C for 10 hour, synthesize 0.4Li 2 MnO 3 0.6LiNi 1 / 2 mn 1 / 2 o 2 (xLi 2 MnO 3 ·(1-x)LiNi 1 / 2 mn 1 / 2 o 2 , where x=0.4) powder;

[0039] 5) 0.4Li 2 MnO...

Embodiment 3

[0041] 1) Weigh nickel nitrate and manganese nitrate with a molar ratio of 0.7:1.3 to prepare a 1.2mol / l mixed solution, use ammonium bicarbonate as a precipitant, and add ammonia water dropwise at the same time, control the pH value to 8.5, and co-precipitate for 12 hours.

[0042] 2) Filter out the co-precipitation product, add deionized water to prepare a slurry with a concentration of 200g / l, and spray dry the slurry at 110°C to obtain nickel-manganese carbonate powder;

[0043] 3) Grinding nickel-manganese carbonate powder, incubating at 300°C for 4 hours, then raising the temperature to 480°C for 2 hours to obtain precursor powder;

[0044] 4) Weigh lithium hydroxide monohydrate with a molar number of 1.03 (K[1+x / (2+x)], where K=0.91), grind and mix with the precursor powder obtained above, and roast at 850°C for 10 hour, synthesize 0.3Li 2 MnO 3 0.7LiNi 1 / 2 mn 1 / 2 o 2 (xLi 2 MnO 3 ·(1-x)LiNi 1 / 2 mn 1 / 2 o 2 , where x=0.3) powder;

[0045] 5) 0.3Li 2 MnO 3 0...

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Abstract

A preparation method of a layered manganese-based cathode material for raising initial charge / discharge efficiency comprises the following steps of: using ammonium bicarbonate as a precipitating agent, simultaneously adding ammoniacal liquor in a dropwise manner so as to control coprecipitation reaction pH value to 8-9, continuing for 8-12 hours, precipitating a coprecipitation product, adding deionized water to prepare a slurry with the concentration of 150-200g / l, carrying out spray drying on the slurry at the temperature of 100-120 DEG C to prepare a Ni-Mn carbonate powder, insulating at the temperature of 300-350 DEG C for 4-6 hours, heating up to 450-500 DEG C and insulating for 2-4 hours to obtain a precursor powder, weighing lithium hydroxide monohydrate with its mole number being K[1+x / (2+x)], grinding the prepared xLi2MnO3.(1-x)LiNi1 / 2Mn1 / 2O2 powder, roasting at the temperature of 600-650 DEG C for 1-6 hours, and annealing. According to the invention, the initial charge / discharge efficiency of the layered manganese-based cathode material is substantially raised, and the cycle stability is obviously improved.

Description

[0001] technical field [0002] The invention belongs to the technical field of preparation of positive electrode active materials for lithium ion batteries, and in particular relates to a preparation method of a positive electrode material which improves the first charge and discharge efficiency and cycle stability of a layered manganese-based positive electrode material. Background technique [0003] In view of the different performance requirements of different types of new energy vehicles (EV, HEV and PHEV, etc.) that have been booming in recent years, the technical research on the large-scale industrialization of power batteries has been further refined into energy-type power battery modules and power with both energy and power. Development of battery systems. Layered manganese-based cathode material xLi 2 MnO 3 ·(1-x)LiNi 1 / 2 mn 1 / 2 o 2 , where 0￡ x ￡0.5 is calculated according to the standard that an electron undergoes a charge-discharge reaction, and its theoret...

Claims

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Application Information

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IPC IPC(8): H01M4/505H01M4/525
CPCY02E60/122Y02E60/10
Inventor 连芳高敏
Owner UNIV OF SCI & TECH BEIJING
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