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Process for production of phosphoric acid compound, and process for production of secondary battery

A technology of phosphoric acid compound and manufacturing method, which is applied to phosphorous compounds, chemical instruments and methods, battery electrodes, etc., can solve the problems of narrow vitrification range, difficult control of LiMPO4 particle composition, etc., and achieves excellent reliability, low cost and simple manufacturing characteristics Effect

Inactive Publication Date: 2012-09-12
ASAHI GLASS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the composition of the precursor glass has a narrow vitrification range, making it difficult to perform LiMPO 4 Particle Composition Control

Method used

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  • Process for production of phosphoric acid compound, and process for production of secondary battery
  • Process for production of phosphoric acid compound, and process for production of secondary battery
  • Process for production of phosphoric acid compound, and process for production of secondary battery

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0085] (Preparation of solid particles of compound (Y))

[0086] The solid particles of compound (Y) are obtained as follows: a compound containing element A, a compound containing element M, and a compound containing P are prepared to form a compound having the composition represented by the aforementioned formula (4) to form a raw material mixture. The raw material mixture is obtained by heating the above-mentioned raw material compound to react. The crystalline particles are preferably produced by mixing a compound containing element A, a compound containing element M, and a compound containing P while being pulverized, and reacting them in a solid phase reaction. In addition, the crystalline particles can also be obtained by a method of slowly cooling and crystallizing a raw material mixture after melting, or a method of heating and crystallizing an amorphous substance of the compound (Y). Amorphous particles are preferably produced by mixing a compound containing element A,...

Embodiment 1）

[0155] Weigh lithium carbonate (Li 2 CO 3 ), iron trioxide (Fe 2 O 3 ) And ammonium dihydrogen phosphate (NH 4 H 2 PO 4 ) To make it Li 3 Fe 2 P 3 O 12 The composition shown is such that the molar ratio of each raw material is 3:2:6, and ethanol is used as a medium for wet grinding and mixing. After heating the mixture in air at 350°C for 2 hours, it was cooled to room temperature and crushed by a dry method. The resulting crushed material was heated in the air at 700°C for 8 hours to obtain Li 3 Fe 2 P 3 O 12 Powder of the compound shown in composition. The mineral phase of the obtained compound was identified with an X-ray diffraction device, and the result was compared with the existing Li 3 Fe 2 (PO 4 ) 3 (PDF No. 01-078-1106) The diffraction pattern is similar to the diffraction pattern.

[0156] Next, mix with Li 3 Fe 2 P 3 O 12 The crystalline compound of the composition shown is combined with iron trioxide (Fe 2 O 3 ) To make 2:1 based on the molar ratio of the oxide, and...

Embodiment 2）

[0159] The compound obtained in Example 1 has Li 3 Fe 2 P 3 O 12 The compound of the shown composition and iron trioxide (Fe 2 O 3 ) So that the molar ratio based on the oxide is 2:1, and carbon black and glucose are further added to the formulation, so that the mass ratio of the formulation to carbon black to glucose is 90:5:5. They are crushed and mixed by wet method using water as the medium. After the resulting mixture was dried at 110°C, it was heated under the same conditions as in Example 1 to obtain a carbon-containing LiFePO 4 Particles of phosphoric acid compound of the composition shown. The diffraction pattern of the obtained particles is similar to the existing LiFePO 4 The diffraction pattern of (PDF No. 01-083-2092) is similar, and it can be confirmed that they are crystalline particles.

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Abstract

Disclosed is a process for producing a phosphoric acid compound, which enables the production of olivine-type crystalline particles of a phosphoric acid compound having excellent properties and excellent reliability at low cost and in a simple manner. Particularly disclosed is a process for producing a phosphoric acid compound useful as a positive electrode material for a secondary battery. Solid particles of a compound (Y) having a chemical composition represented by the formula AxMyP3Oz (wherein element A represents at least one element selected from the group consisting of Li and Na; element M represents at least one element selected from the group consisting of Fe, Mn, Co and Ni; and N which represents the valency the element M, x and y respectively fulfill the requirements represented by the formulae +2<N<=+4, 0<x<4 and 0<y<3) and a compound (Z) containing the element M are mixed together so that the resulting product has a chemical composition represented by the formula AaMbPOw (wherein 0<a<2 and 0.8<b<1.2), and the resulting product is agitated while grinding and heated in an inert gas or a reducing gas to cause a solid-phase reaction. In this manner, particles of a phosphoric acid compound (X) having a chemical composition represented by the formula AaMbPOw (wherein A is derived from the compound (Y); and M is derived from the compounds (Y) and (Z)) can be produced.

Description

Technical field [0001] The present invention relates to a method of manufacturing a phosphoric acid compound and a method of manufacturing a secondary battery. Background technique [0002] In recent years, lithium ion secondary batteries have been widely used as power sources for portable electronic devices such as mobile phones and notebook computers, electric tools, and the like. As the cathode material of lithium ion secondary batteries, layered rock salt LiCoO is mostly used 2 . However, the layered rock salt type LiCoO 2 The safety of Co is insufficient, and Co is a resource scarce element, which has problems such as expensive and large price fluctuations. Furthermore, for the development and popularization of electric vehicles, hybrid vehicles, etc., lithium ion secondary batteries need to be greatly increased in capacity and size while maintaining safety. [0003] On the other hand, from the perspective of resources, safety, cost, and stability, the use of olivine-type li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M4/58
CPCC01B25/45H01M4/136H01M4/5825Y02E60/10H01M4/58
Inventor 别府义久
Owner ASAHI GLASS CO LTD
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