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Preparation method of nano iron phosphate with globulomer structure for lithium iron phosphate

A lithium iron phosphate, nano-scale technology, which is applied in the field of preparation of nano-scale iron phosphate, can solve the problems of low ion transmission rate, low electronic conductivity, and difficult nano-materials of lithium iron phosphate, so as to achieve high reactivity and vibration The effect of high density and particle size reduction

Inactive Publication Date: 2012-01-04
IRICO
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

While it has excellent advantages, it also has its fatal disadvantages as a positive electrode material for EV batteries: the electronic conductivity is as low as 10-9s / cm; the ion transmission rate is as low as 10-11s / cm
Most of the current commercially available lithium iron phosphate products are synthesized by high-temperature solid-phase method, and it is difficult to realize the nanometerization of lithium iron phosphate materials by using common commercially available raw materials through high-temperature solid-phase synthesis process

Method used

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  • Preparation method of nano iron phosphate with globulomer structure for lithium iron phosphate
  • Preparation method of nano iron phosphate with globulomer structure for lithium iron phosphate
  • Preparation method of nano iron phosphate with globulomer structure for lithium iron phosphate

Examples

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Embodiment 1

[0022] with Fe 2 (SO 4 ) 3 、H 3 PO 4 as the raw material, where PO 4 3- and Fe 3+ The mass ratio of the substances is 1:1. Dissolve the above reagents in deionized water to obtain a transparent homogeneous solution. After mixing the above solutions evenly, add ammonia solution, adjust the pH to 8, and heat the above mixed liquid in a water bath at 80°C for 1 hour until the active ingredients are fully precipitated. The flocculent suspension is filtered to obtain a white filter cake, and the filter cake is washed with deionized water. The difference in the conductivity value of the two consecutive washes is within 5% before the washing is completed; the liquid phase controlled crystallization process is used to prepare primary particles. Secondary granulation is carried out through the spray drying process. After spray drying, the primary particles with a particle size of 30nm are agglomerated to form spherical aggregates with a particle size of 5-20μm and micron-sized g...

Embodiment 2

[0025] With Fe(NO 3 ) 3 、H 3 PO 4 as the raw material, where PO 4 3- and Fe 3+ The molar ratio of the substances is 1:1.1. Dissolve the above reagents in deionized water to obtain a transparent homogeneous solution. After mixing the above solutions evenly, add ammonia solution, adjust the pH to 7, and then heat the above mixed liquid in a water bath at 60°C for 2 hours until the active ingredients are fully precipitated and form flocs. After filtering, a white filter cake was obtained, and the filter cake was washed with deionized water. The difference between the conductivity values ​​of the two consecutive washes was within 5% and then the washing was completed; the liquid-phase controlled crystallization process was used to prepare the primary particle, and then The secondary granulation is carried out through the spray drying process. After spray drying, the primary particles with a particle size of 30nm are agglomerated to form a spherical aggregate with a particle ...

Embodiment 3

[0027] with FeCl 3 、H 3 PO 4 as the raw material, where PO 4 3- and Fe 3+ The mass ratio of the substances is 1:1.2. Dissolve the above reagents in deionized water to obtain a transparent homogeneous solution, mix the above solutions evenly, add ammonia solution, adjust the pH to 8.5, and heat the above mixed liquid in a water bath at 100°C for 1.5 hours until the active ingredients are fully precipitated and form flocs After filtering, a white filter cake was obtained, and the filter cake was washed with deionized water. The difference between the conductivity values ​​of the two consecutive washes was within 5% and then the washing was completed; the liquid-phase controlled crystallization process was used to prepare the primary particle, and then The secondary granulation is carried out through the spray drying process. After spray drying, the primary particles with a particle size of 30nm are agglomerated to form a spherical aggregate with a particle size of 5-20μm an...

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Abstract

The invention provides a preparation method of nano iron phosphate (FePO4.2H2O) with a globulomer structure for lithium iron phosphate. The preparation method comprises the following steps: dissolving soluble compounds which respectively contain Fe<3+> and PO4<3-> to form a homogeneous phase solution, regulating pH value with an alkaline solution, carrying out water bath heating on a mixed liquid until the effective component of the mixed liquid is sufficiently precipitated to form a white flocculent suspension, filtering and washing; and preparing primary particles by using a liquid phase control crystallization process, and carrying out secondary pelleting with a spray drying process so as to obtain FePO4.2H2O having the globulomer structure and a particle diameter of 5-20 mu m, wherein FePO4.2H2O is formed by agglomeration of primary particles with a particle diameter of 30 nm. According to the invention, prepared FePO4.2H2O has the advantages of uniform particle distribution, high tap density and high reaction activity, and the primary particle is of nano grade; and FePO4.2H2O is used as a raw material so as to improve the consistency of topography of a lithium iron phosphate material, thereby effectively reducing the particle diameter of a lithium iron phosphate positive electrode material and further improving the transmission efficiency of lithium ions in the lithium iron phosphate material; and FePO4.2H2O having a micron globulomer structure, which is obtained by secondary pelleting, is more beneficial to synthesis of a micro lithium iron phosphate material which is easy to coat.

Description

technical field [0001] The invention relates to a preparation method of transition metal phosphate, in particular to a preparation method of nano-scale iron phosphate which can be used to prepare metal lithium phosphate cathode material. Background technique [0002] Lithium iron phosphate (LiFePO 4 ) has the function of deintercalating lithium, has the characteristics of high energy density, low price, and excellent safety, and is considered by the industry to be the most likely cathode material for EV batteries. While it has excellent advantages, it also has its fatal disadvantages as a cathode material for EV batteries: the electronic conductivity is as low as 10-9s / cm; the ion transmission rate is as low as 10-11s / cm. Such a low electron / ion transport rate makes it a serious obstacle to increase the charge and discharge rate, which limits its application in EV and HEV. [0003] Current solution to LiFePO 4 The problem of low electron / ion transport rate is mainly solve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45B82Y40/00H01M4/58
CPCY02E60/10
Inventor 赵金鑫
Owner IRICO
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