Lithium-titanium complex oxide, and battery electrode and lithium ion secondary battery containing same

A composite oxide, battery technology, applied in battery electrodes, circuits, titanate and other directions, can solve the problem of battery performance degradation, and achieve the effect of inhibiting reaction, excellent stability over time, and improving stability over time

Inactive Publication Date: 2013-06-26
TAIYO YUDEN KK
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In Patent Document 3, it is described that when the pH value is increased to a level greater than 11.2 due to the exposure of unreacted Li components such as hydroxides or carbonates that have not been absorbed into lithium titanate on the surface, battery performance tends to decrease.

Method used

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  • Lithium-titanium complex oxide, and battery electrode and lithium ion secondary battery containing same
  • Lithium-titanium complex oxide, and battery electrode and lithium ion secondary battery containing same
  • Lithium-titanium complex oxide, and battery electrode and lithium ion secondary battery containing same

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Embodiment ）

[0076] Next, the present invention will be described more specifically based on examples. However, the present invention is not limited to the aspects described in these Examples. First, analysis and evaluation methods of the samples obtained in the respective examples and comparative examples will be described.

[0077] (Elemental analysis)

[0078] Quantitative analysis of contained elements is carried out by atomic absorption spectrometry or ICP emission spectrometry after the sample of titanium-lithium composite oxide is subjected to pressurized acid decomposition. The ratios (% by mass) of potassium, phosphorus, and sulfur were calculated relative to the weight of 100% of the titanium-lithium composite oxide. For lithium, the value quantified by ICP emission spectroscopic analysis was used. For titanium, the Li / Ti molar ratio was calculated using a value obtained by subtracting the value of the intense heat loss up to 900° C. and the mass of all the elements quantifie...

Embodiment 1）

[0091] The feed Li / Ti atomic ratio was set to 0.805. The Li source is lithium carbonate (a high-purity commercially available reagent with a purity of 99%), and the titanium oxide is a high-purity product with a purity of 99.9% and a specific surface area of ​​10±1m 2 / g of titanium oxide. The pure water of the dispersion medium was added so that the solid content concentration was 52% by mass, potassium hydroxide was added as a potassium source, and ammonium dihydrogen phosphate was added as a phosphorus source to obtain a slurry.

[0092] The resulting slurry was mixed with a bead mill. Then, the dispersion medium was removed with a spray dryer, and heat-treated at 820° C. for 3 hours in the air. Then, use pure water and a bead mill for crushing, and dry the filter cake after filtration and punching. After dry crushing, it will not contain CO 2 (less than 1ppm) of 20%O 2 -80%N 2 In an atmosphere of mixed gas (dew point -70°C), heat-treat at 500°C for 1 hour, and cool to...

Embodiment 2）

[0095] The feed Li / Ti atomic ratio was set to 0.805. The Li source is lithium carbonate (a high-purity commercially available reagent with a purity of 99%), and the titanium oxide is a high-purity product with a purity of 99.9% and a specific surface area of ​​10±1m 2 / g of titanium oxide. Potassium hydroxide was added as a K source, and ammonium dihydrogen phosphate was added as a phosphorus source. currently using The balls were dry-mixed with a planetary ball mill for 2 hours, and heat-treated at 820° C. for 3 hours in the atmosphere. Then, by using pure water and a bead mill for pulverization, the filter cake after filtration and punching is dried for dry crushing so as not to contain CO 2 (less than 1ppm) of 20%O 2 -80%N 2 Atmosphere of mixed gas (dew point -70°C), heat treatment at 400°C for 1 hour, and cool to room temperature without exposure to the atmosphere. The value calculated by the above formula (2) is 0.0010.

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Abstract

The invention provides a lithium-titanium complex oxide which is manufactured by a solid phase method, is useful for manufacture of high-capacity batteries, and is excellent in storage stability, and a battery electrode and a lithium ion secondary battery containing the same. The lithium-titanium complex oxide in a particulate form whose main ingredient is Li4Ti5O12 contains potassium (K), wherein (SSK / SSTi) / (Ck) is 12 or less and preferably (SSK / SSTi)-(SIK / SITi) is 0.01 or less, where SSK is the K2p peak area of potassium (K) and SSTi is the Ti2p peak area of titanium (Ti) based on X-ray photoelectron spectral measurement of the particle surface, Ck is the content ratio (percent by mass) of potassium (K), SIK is the K2p peak area of potassium (K) and SITi is the Ti2p peak area of titanium (Ti) based on X-ray photoelectron spectral measurement in the interior of the particle.

Description

technical field [0001] The invention relates to a lithium-ion secondary battery, its electrode and a lithium-titanium composite oxide suitable as an electrode material. Background technique [0002] Li 4 Ti 5 o 12 Lithium titanate having a spinel structure has almost no volume change and is highly safe. Lithium-ion secondary batteries using it as a negative electrode have begun to be used in automobiles and infrastructure. However, the market is demanding a significant reduction in the price of batteries. Carbon materials are generally used as the negative electrode material, and although there are problems in safety compared with lithium titanate, the capacity is high and the price is much lower. Therefore, it is important to maintain the performance of lithium titanate high and to increase the efficiency of the production process. As the performance (electrochemical performance) of lithium titanate, high capacity, high rate characteristics (high-speed charge and disc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/485
CPCH01M4/131C01G23/005C01P2002/32C01P2002/52C01P2002/54C01P2002/74C01P2002/85C01P2006/12C01P2006/80H01M4/485Y02E60/10
Inventor 川村知荣持木雅希伊藤大悟和川明俊小形曜一郎落合俊幸铃木利昌
Owner TAIYO YUDEN KK
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