Negative electrode material for lithium ion batteries containing surface-fluorinated b-type titanium oxide powder, method for producing same, and lithium ion battery using same

A technology for lithium ion batteries and negative electrode materials, which is applied in battery electrodes, titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of limited and ineffective charging characteristics, and achieve the effect of increasing charging capacity and high discharging capacity.

Inactive Publication Date: 2014-05-07
DOSHISHA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the conditions under which a good effect can be obtained by fluorination treatment are limited. For example, the effect cannot be obtained by fluorination treatment at 25°C, and only high current densities (300mA / g, 600mA / g) can be seen to improve charging characteristics. situation, etc.

Method used

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  • Negative electrode material for lithium ion batteries containing surface-fluorinated b-type titanium oxide powder, method for producing same, and lithium ion battery using same
  • Negative electrode material for lithium ion batteries containing surface-fluorinated b-type titanium oxide powder, method for producing same, and lithium ion battery using same
  • Negative electrode material for lithium ion batteries containing surface-fluorinated b-type titanium oxide powder, method for producing same, and lithium ion battery using same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Manufacture of Fluorinated Type B Titanium Oxide Powder

[0054] As a starting material, TiO with an average particle size of 100nm was used 2 Anatase (manufactured by Aldrich, with a purity of over 99%) and K 2 CO 3 (Manufactured by Wako Pure Chemical Industries, Ltd., purity 99.8%). First, weigh the TiO 2 Anatase and K 2 CO 3 The molar ratio was set to 4:1, and mixing was performed at 400 rpm for 1 hour using a planetary ball mill, so that the samples were uniformly mixed. Next, the sample was put into an alumina crucible, and fired at 1000° C. in air twice for 24 hours. The obtained samples were each ion-exchanged in 1M HCl at room temperature for 72 hours. After performing ion exchange, washing and filtering were performed, and drying was performed at 80° C. for 24 hours in a vacuum dryer. After drying, dehydration was performed by heat-treating the sample at 500° C. for 30 minutes to synthesize B-type titanium oxide. Then, the synthesized B-type titanium...

Embodiment 2

[0059] Analysis of the crystal structure of the powder

[0060] Regarding the B-type titanium oxide powders obtained in Example 1 and Comparative Example 1, the crystal structure of the bulk was analyzed by powder X-ray diffraction (XRD). As a powder X-ray diffractometer, Rint2500 (manufactured by Rigaku Corporation) was used. CuKα was used as the X-ray source, and the measurement was carried out under the conditions of tube voltage 40kV, tube current 200mA, measurement range 5°≤2θ≤60°, light receiving slit 0.3mm, divergence slit 1°, and scattering slit 1°.

[0061] The results of the analysis are as figure 1 As shown, in Example 1 and Comparative Example 1, no change in XRD peak shape or peak shift was observed, and it was confirmed that the main structure of the B-type titanium oxide powder was not changed by the fluorination treatment.

Embodiment 3

[0063] Observation of the surface morphology of the powder

[0064] The surface morphology of the B-type titanium oxide powders obtained in Example 1 and Comparative Example 1 was observed using a field emission scanning electron microscope (FE-SEM). As the electron microscope, JSM7001FD manufactured by JEOL Ltd. was used. Since the electron conductivity of the sample was low, after performing gold sputtering, surface observation was performed at an acceleration voltage of 15 kV.

[0065] The observed results are as figure 2 As shown in (a), no significant change in surface morphology was observed in Example 1 and Comparative Example 1 in 5000-magnification observation. Additionally, if figure 2 As shown in (b), it was confirmed that the surface of the powder of Example 1 was slightly smoother than the surface of the powder of Comparative Example 1 in observation at 30000 magnification.

[0066] In addition, the specific surface area of ​​the B-type titanium oxide powd...

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Abstract

The present invention addresses the problem of providing a B-type titanium oxide (TiO2(B)) powder which can be suitable for use as a negative electrode material for lithium ion batteries by improving the charge and discharge characteristics and the rate characteristics of the B-type titanium oxide powder by a simple treatment. A surface-fluorinated B-type titanium oxide powder is obtained by reacting a B-type titanium oxide powder in a fluorine-containing gas atmosphere at 0-200 DEG C for 1 minute to 10 days. The fluorination treatment is preferably carried out at 0.01-2 atm. It is preferable to use, as the fluorine-containing gas, a gas that contains a fluorine compound, said gas being selected from among a fluorine (F2) gas, a nitrogen trifluoride (NF3) gas, a perfluorotrimethylamine (N(CF3)3) gas, a chlorine trifluoride (ClF3) gas and the like.

Description

technical field [0001] The present invention relates to a titanium oxide-based negative electrode material that can be used as a negative electrode of a lithium ion battery. In more detail, B-type titanium oxide (TiO 2 (B) Negative electrode material, method of manufacturing the same, and lithium ion battery using the same. Background technique [0002] In recent years, from the viewpoint of energy and environmental issues, lithium ion batteries have been expected to increase in size as power sources for electric vehicles or as large secondary batteries for power load balancing. However, it is considered that the cost, safety, and lifetime need to be greatly improved in order to be practically used as a large-scale secondary battery. [0003] In order to increase the output, cost, safety, and life of lithium-ion batteries, it is a solution to use a high-potential negative electrode that performs a charge-discharge reaction at a potential of 1.0 V or higher. As one of such...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/48
CPCC01G23/047C01P2002/52C01P2002/72C01P2002/85C01P2004/03C01P2006/12H01M4/1315H01M4/485H01M2004/021H01M10/0525H01M2004/027Y02E60/10H01M4/362
Inventor 稻叶稔田坂明政斋藤守弘高木干大竹林仁初代善夫
Owner DOSHISHA CO LTD
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