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Lithium iron phosphate powder manufacturing method, olivine structured lithium iron phosphate powder, cathode sheet using said lithium iron phosphate powder, and non-aqueous solvent secondary battery

A lithium iron phosphate and olivine-type technology, which is applied in electrode manufacturing, battery electrodes, structural parts, etc., can solve the problems of low lithium ion density and large positive electrode volume, and achieve improved current load characteristics and charge-discharge cycle characteristics. High fillability and improved energy density

Inactive Publication Date: 2011-02-23
TODA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, a positive electrode compounded with a large amount of carbon or the like is bulky, and there is a disadvantage that the substantial lithium ion density that can be filled per unit volume becomes low.

Method used

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  • Lithium iron phosphate powder manufacturing method, olivine structured lithium iron phosphate powder, cathode sheet using said lithium iron phosphate powder, and non-aqueous solvent secondary battery
  • Lithium iron phosphate powder manufacturing method, olivine structured lithium iron phosphate powder, cathode sheet using said lithium iron phosphate powder, and non-aqueous solvent secondary battery
  • Lithium iron phosphate powder manufacturing method, olivine structured lithium iron phosphate powder, cathode sheet using said lithium iron phosphate powder, and non-aqueous solvent secondary battery

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0132] Using the iron raw material of No. 1 recorded in Table 1, use a crushing machine to mix LiH with the feed ratio Li / Fe=1.01 and P / Fe=1.01 recorded in Table 2. 2 PO 4 , to obtain 10g of lithium iron phosphate particle powder (first process).

[0133] Next, in ZrO 2 In the prepared ball mill container, adjust the mixed powder obtained in the first process and a specified amount of acetylene black with ethanol to make the slurry concentration 30wt%, and use 5mmΦ ZrO 2 The balls were crushed for 24 hours, intimately mixed, and the slurry was dried (removed solvent) at room temperature to obtain a precursor.

[0134] exist figure 2 The secondary electron image of the iron feedstock used here is represented in , in image 3 The reflection electron images of the obtained precursors are shown in . The average primary particle diameter of the iron raw material used was 200 nm. exist figure 2 24 squares of 2 μm × 2 μm were drawn on the reflection electron image of , and i...

Embodiment 2、3、8

[0139] Experiments were performed with the contents described in Table 2. The parts not described were carried out in the same manner as in Example 1. However, a predetermined amount of carbon-containing additives is blended in the dry ball mill after the second step. Table 3 shows the powder properties of the obtained lithium iron phosphate particles having an olivine structure. In this fine powder having an olivine structure, as in Example 1, except for the composition ratio of Li, Fe, P and the additive element C, the composition ratios of all additive elements and Fe were consistent within a measurement error range of 3%.

Embodiment 4、5、7

[0141] After mixing a predetermined amount of main raw materials in a wet (water solvent) ball mill to obtain 150 g of lithium iron phosphate particle powder, it was dried at 70° C. for 12 hours. Using Li as the main raw material containing lithium and phosphorus 3 PO 4 and H 3 PO 4 (first process).

[0142] At 5mmΦZrO 2 The dry product and a predetermined amount of carbon-containing additives were pulverized in a dry ball mill for 24 hours (step A, second step), and calcined at 400° C. for 2 hours in a nitrogen atmosphere (third step). After crushing and mixing with a dry ball mill, heat treatment was performed again at 650° C. under a nitrogen atmosphere for 2 hours (operation A).

[0143] Table 3 shows the powder properties of the obtained lithium iron phosphate particles having an olivine structure. In this fine powder having an olivine structure, as in Example 1, except for the composition ratio of Li, Fe, P and the additive element C, the composition ratios of all ...

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Abstract

Disclosed is an olivine structured lithium iron phosphate powder manufacturing method that uses iron oxide or an aqueous oxide as the iron starting material, and that comprises a first step in which the iron oxide aqueous oxide that comprises 0.1 to 2 mol% each of at least one of elemental Na, Mg, Al, Si, Cr, Mn, Ni per Fe, and comprises 5 to 10 mol% of elemental C per Fe, and wherein there is 40 mol% or less of Fe2+ per the quantity of Fe, and the mean primary particle size of 5 to 300 nm, is mixed together with a lithium starting material and a phosphorous starting material, a second step to adjust the aggregate particle size in the resulting mixture to 0.3 to 5.0 [mu]m, and a third step in which the mixture obtained in the second step is sintered at a temperature of 250 to 750 C in an inert gas or reducing gas atmosphere with 0.1% or less oxygen concentration.

Description

technical field [0001] The present invention is to provide lithium iron phosphate particle powder with an olivine structure that can be easily produced at low cost, has a large charge-discharge capacity as a secondary battery, and is excellent in filling properties and charge-discharge cycle characteristics, and a positive electrode material sheet using the powder. and secondary batteries. Background technique [0002] In recent years, electronic equipment such as AV equipment and personal computers, and power tools such as electric tools have rapidly become portable and cordless, and the demand for small, light-weight, and high-energy-density secondary batteries is increasing as their driving power supply . In addition, in recent years, electric vehicles and hybrid vehicles have been developed and put into practical use in consideration of the global environment, and demand for lithium-ion secondary batteries with excellent charge-discharge cycle characteristics has been i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/04C01B25/45H01M4/62H01M4/02H01M4/58H01M4/587H01M4/136
CPCY02E60/122H01M4/5825C01B25/45Y02E60/10
Inventor 三岛祐司本田晋吾河野芳辉佐藤幸太冈崎精二片元勉
Owner TODA IND
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