Aluminum-doped spinel manganese-based material and preparation method thereof

A spar manganese-based, aluminum-doped technology, used in electrical components, battery electrodes, circuits, etc., can solve the problems of inability to achieve uniform mixing of doping elements and uneven precipitation, and achieve excellent electrochemical performance and good repeatability. , the effect of increasing the doping ratio

Active Publication Date: 2015-04-01
SHANGHAI INST OF SPACE POWER SOURCES
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, for Al-doped lithium manganese oxide materials, when the precursor is synthesized by the co-precipitation method, due to the Al(OH) 3 The solubility product is much smaller than that of MnCO 3 The solubility product and the huge difference in precipitation speed can easily cause uneven precipitation, so that the purpose of uniform mixing of doping elements cannot be achieved.

Method used

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  • Aluminum-doped spinel manganese-based material and preparation method thereof
  • Aluminum-doped spinel manganese-based material and preparation method thereof
  • Aluminum-doped spinel manganese-based material and preparation method thereof

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Embodiment 1

[0030] MnSO 4 ·H 2 O was dissolved in deionized water to make a 2mol / L solution. with anhydrous Na 2 CO 3 As a precipitating agent, it can be dissolved in deionized water to form a 2mol / L solution. Using a peristaltic pump, the MnSO 4 solution and Na 2 CO 3 The solution was poured into the reactor at a flow rate of 0.5mol / L. Weigh a certain amount of aluminum isopropoxide in proportion, dissolve aluminum isopropoxide and acetylacetone in ethanol according to the molar ratio of 1:1, the concentration is 0.8mol / L, and dissolve the above aluminum isopropoxide solution at a certain dropwise into the reactor. The pH of the control system is ≈8, the temperature of the system is 50°C, the stirring speed is 600r / min, and the (Mn0.925 al 0.075 )CO 3 precipitation. After the precipitate was filtered and dried, it was calcined at 850 °C for 5 h to obtain M 2 o 3 (M=Mn, Al) oxide. After fully mixing the oxide and lithium carbonate with an amount of 1.05 times the stoichiomet...

Embodiment 2

[0035] Weigh 0.1mol nickel sulfate and 0.3mol manganese sulfate according to the molar ratio of 1:3, and dissolve them in deionized water to prepare a mixed solution of 2mol / L. Weigh 0.4mol sodium carbonate and prepare a 2mol / L solution as a precipitant. The manganese sulfate solution, nickel sulfate solution and sodium carbonate solution were pumped into the reactor at a flow rate of 0.5 mol / L by a peristaltic pump. Weigh a certain amount of aluminum isopropoxide in proportion, dissolve aluminum isopropoxide and acetylacetone in ethanol according to the molar ratio of 1:1, the concentration is 0.8mol / L, and drop the aluminum salt solution at a certain speed added to the reactor. The pH value is controlled at 8.3, the temperature is 50°C, the stirring speed is 400r / min, and the reaction time is 20h. After several times of filtration, washing, and drying, a carbonate precipitate is obtained. The precipitate was heat-treated at 600°C for 5h to obtain the oxide. Fully grind th...

Embodiment 3

[0038] Dissolve manganese sulfate in deionized water to make a 1mol / L solution. Ammonium bicarbonate was used as a precipitating agent, dissolved in deionized water to form a 1mol / L solution. The manganese sulfate solution and the ammonium bicarbonate solution were pumped into the reactor at a flow rate of 0.5 mol / L by a peristaltic pump. Weigh a certain amount of aluminum isopropoxide in proportion, dissolve aluminum isopropoxide and acetylacetone in ethanol according to the molar ratio of 1:1, the concentration is 0.8mol / L, and drop the aluminum salt solution at a certain speed added to the reactor. The pH of the control system is ≈7.5, the temperature of the system is 50°C, the stirring speed is 600r / min, and the (Mn 0.925 al 0.075 )CO 3 precipitation. After the precipitate was filtered and dried, it was calcined at 800 °C for 5 h to obtain M 2 o 3 (M=Mn, Al) oxide. After fully mixing the oxide and lithium carbonate with an amount of 1.01 times the stoichiometric ra...

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Abstract

The invention discloses an aluminum-doped spinel manganese-based material and a preparation method thereof. The method comprises the steps of respectively putting configured manganese source compound solution, or a nickel source compound, aluminum salt compound solution and a precipitator solution into a reactor according to the flow rate being 0.5-2L / h, stirring to control the pH value of a system to be 7-8.5 and the heating temperature of the system to be 30 DEG C-60 DEG C, heating and then curing for 10h-20h to obtain a spherical precipitate precursor, washing and drying the spherical precipitate precursor; forging the dried precipitate for 5-20h under the temperature being 600-900 DEG C; and sufficiently mixing oxidizing materials and a lithium source compound according to a proportion that the stoichiometric ratio exceeds the lithium source compound by 1-10%, and forging for 5-20h under the temperature being 600-900 DEG C to obtain the modified spinel manganese-based material. According to the method disclosed by the invention, the feature of the precursor and the distribution uniformity of an Al element can be improved effectively; due to the reasonable high forging temperature and doping proportion, the structure stability of the aluminum-doped spinel manganese-based material can be improved greatly, and the circulation performance and high-temperature and low-temperature performances of the material can be improved; and the process is simple, and the repeatability is good.

Description

technical field [0001] The invention belongs to the field of lithium ion batteries, and relates to a lithium ion positive electrode material, in particular to a method for preparing an aluminum-doped spinel manganese-based material. Background technique [0002] Li-Mn-O spinel manganese-based materials are considered to be positive electrode materials for lithium-ion batteries with good application prospects due to their three-dimensional lithium ion channels and stable thermodynamic properties. And its derived LiM x mn 2-x o 4 (M=Cr, Co, Fe, Ni, etc.) materials have a high-voltage platform above 4.5V and have higher energy density, which has also attracted widespread attention. Among them, Li-Ni-Mn-O spinel manganese-based materials have become a hot spot in the research of high-voltage materials due to their high discharge specific capacity due to their 4.7V voltage platform. However, spinel manganese-based materials such as Li-Mn-O and Li-Ni-Mn-O have certain limitati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/505H01M4/525
CPCY02E60/122Y02E60/10
Inventor 罗英解晶莹冯毅顾海涛汤卫平
Owner SHANGHAI INST OF SPACE POWER SOURCES
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