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Process for producing lithium borate compound

A compound, lithium borate technology, applied in the direction of boron compounds, boron oxide compounds, chemical instruments and methods, etc., can solve the problems of slow ion diffusion, lithium-deficient borate compounds, high resistance, etc., to achieve high capacity and good cycle characteristics, effect of inhibiting grain growth

Inactive Publication Date: 2012-02-08
NAT INST OF ADVANCED IND SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the solid-state reaction method requires a long-term reaction at a high temperature of 600°C or higher, and although the dopant element can be solid-dissolved, it involves problems such as crystal grain growth to 10 μm or larger and slow diffusion of ions.
Furthermore, since the reaction proceeds at a high temperature, there is a problem that doping elements that are not completely dissolved in the cooling process precipitate to generate impurities and increase the resistance.
Furthermore, due to heating to a high temperature, there is also a borate-based compound in which lithium deficiency and oxygen deficiency occur, and it is difficult to increase the capacity and improve the cycle characteristics.

Method used

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  • Process for producing lithium borate compound
  • Process for producing lithium borate compound
  • Process for producing lithium borate compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] Synthesis of lithium-excess borate-based compounds and charge-discharge characteristics of batteries using the compounds

[0080] As a raw material, iron oxalate FeC is used 2 o 4 2H 2 O (manufactured by SIGMA-ALDRICH, purity 99.99%), lithium hydroxide (anhydrous) LiOH (KISHIDA chemical, 98%), boric acid H 3 BO 3 (KISHIDA Chemical, 99.5%) each 0.005 mole, they are mixed with carbonate mixture (lithium carbonate (KISHIDA Chemical, passivation 99.9%), sodium carbonate (KISHIDA Chemical, purity 99.5%) and potassium carbonate (KISHIDA Chemical system, purity 99.5%)) mixed at a molar ratio of 0.435:0.315:0.25) were mixed. The mixing ratio is such that the total amount of iron oxalate, lithium hydroxide, and boric acid is 225 parts by weight relative to 100 parts by weight of the carbonate mixture.

[0081] 20 mL of acetone was added thereto, mixed with a zirconia ball mill at 500 rpm for 60 minutes, and dried. Then, the obtained powder was heated in a gold crucible, a...

Embodiment 2

[0095]Use the ferric oxalate used in the method of embodiment 1 and the metal component corresponding to the target composition shown in following table 2, except that, carry out the operation identical with embodiment 1 and synthesize by composition formula: Li 1+a-b A b m 1-x M' x BO 3+c (In the formula, A is at least one element selected from Na, K, Rb and Cs, M is at least one element selected from Fe and Mn, M' is selected from Mg, Ca, Co, Al, Ni , Nb, Mo, W, Ti and Zr. Each subscript is as follows: 0≤x≤0.5, 0 b) Lithium-excess borate-based compound represented. In addition, instead of the iron oxalate used in the method of Example 1, a metal component corresponding to the target composition shown in Table 3 below was used, and the same operation as in Example 1 was performed to synthesize the compound represented by the above composition formula. A lithium-excess borate-based compound.

[0096] It should be noted that the use of iron oxalate FeC 2 o 4 2H 2 O (ma...

Embodiment 3

[0112]

[0113] Add 50 parts by weight of acetylene black (hereinafter referred to as AB) and 20 parts by weight of LiF to 100 parts by weight of the product (lithium borate-based compound) after removing water-soluble substances such as carbonates in Example 2, and use a planetary ball mill (5mm Zirconia balls) were ground at 450rpm for 5 hours, in the mixed gas of carbon dioxide and hydrogen ((CO 2 :H 2 Heat treatment was performed at 700° C. for 2 hours in an atmosphere of (molar ratio)=100:3). The XRD pattern of the product after the heat treatment was very consistent with that of the sample before the heat treatment, and it was confirmed that the lithium-excess borate-based compound was not decomposed and the crystal structure was maintained. In addition, the elemental analysis results (element molar ratios) obtained by the ICP method are shown in Tables 6 and 7 below. From these tables, it was confirmed that the products were all lithium-excess fluorine-containing li...

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Abstract

A process for producing, by a relatively simple means, a lithium borate material which is useful as a positive-electrode material for lithium-ion secondary batteries, etc. and has improved cycle characteristics, capacity, etc., and excellent performances. The process is characterized by reacting one or more divalent-metal compounds comprising at least one compound selected from a group consisting of compounds of divalent iron and compounds of divalent manganese with boric acid and lithium hydroxide in a reducing atmosphere at 400-650 DEG C in the melt of a carbonate mixture comprising lithium carbonate and at least one alkali metal carbonate selected from a group consisting of potassium carbonate, sodium carbonate, rubidium carbonate, and cesium carbonate.

Description

technical field [0001] The present invention relates to a method for preparing a lithium borate-based compound useful as a positive electrode active material of a lithium-ion battery, and an application of the lithium borate-based compound obtained by the method. Background technique [0002] Lithium secondary batteries are small and have high energy density, and are widely used as power sources for portable electronic devices. As the positive electrode active material, LiCoO is mainly used 2 and other layered compounds. However, these compounds have the disadvantage that oxygen is easily desorbed at about 150° C. in a fully charged state, and in this case, an oxidative exothermic reaction of the non-aqueous electrolyte is likely to occur. [0003] In recent years, olivine phosphate compound LiMPO has been proposed as a positive electrode active material. 4 (LiMnPO 4 、LiFePO 4 、LiCoPO 4 Wait). The system is replaced by LiCoO 2 This kind of oxide is used as the 3-valen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/12H01M4/58H01M4/36
CPCB82Y30/00C01B35/128C01P2002/72C01P2004/03C01P2004/64H01M4/136H01M4/5825H01M10/0525Y02E60/10C01B35/12H01M4/1397H01M4/58
Inventor 小岛敏胜境哲男幸琢宽小岛晶丹羽淳一村濑仁俊
Owner NAT INST OF ADVANCED IND SCI & TECH
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