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Preparation method of lithium ion battery cathode material nano lithium iron phosphate

A technology for lithium ferrous phosphate and lithium-ion batteries, which is applied to battery electrodes, circuits, electrical components, etc., and can solve the problems of product purity, difficulty in controlling crystal morphology and particle size, difficulty in mixing uniform reactants, and large differences in electrochemical performance, etc. problems, to achieve high product quality consistency, facilitate large-scale production, and shorten the ball milling time

Active Publication Date: 2013-12-04
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the synthesis process of the high-temperature solid-phase method is simple, the reactants are not easy to mix uniformly, the reaction time is long, and multiple sintering is required. Most of the synthesized products have a particle size of microns, and the distribution is uneven, often containing impurities, and the shape is irregular. , the electrochemical properties of different batches of materials are quite different
This is because the solid phase method is difficult to accurately control the ratio of lithium, iron, and phosphorus, and the control of product purity, crystal morphology, and particle size is also very difficult, the stability of the product batch is poor, and the entire production process is long and energy consumption is high. Big

Method used

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  • Preparation method of lithium ion battery cathode material nano lithium iron phosphate
  • Preparation method of lithium ion battery cathode material nano lithium iron phosphate
  • Preparation method of lithium ion battery cathode material nano lithium iron phosphate

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Experimental program
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Effect test

Embodiment 1

[0034] The preparation of lithium iron phosphate nanometer lithium ion battery cathode material is carried out according to the following steps:

[0035] (1) Using lithium hydroxide and sodium carbonate as raw materials, using a rotating packed bed method to prepare nanometer lithium carbonate, the average particle size of the obtained lithium carbonate is 60 nm;

[0036] (2) Ferric nitrate, phosphoric acid and ammonia are used as raw materials to prepare nano-hydrated iron phosphate by the rotating packed bed method. For details, please refer to the applicant’s patent "A method for preparing nano-iron phosphate" (application number: 200910235404.8). The average particle size of nano-hydrated iron phosphate is 40nm;

[0037] (3) Take 620g of FePO nano-hydrated iron phosphate prepared in step (2) 4 ·2H 2 O, in an air atmosphere, the temperature is increased to 550°C at a heating rate of 4°C / min, and roasted for 6 hours to dehydrate to obtain anhydrous nano iron phosphate powder;

[003...

Embodiment 2

[0044] The preparation of lithium iron phosphate nanometer lithium ion battery cathode material is carried out according to the following steps:

[0045] (1) Using iron acetate, phosphoric acid and potassium hydroxide as raw materials, the rotating packed bed method is used to prepare nano-hydrated iron phosphate. For details, please refer to the applicant’s patent "A method for preparing nano-iron phosphate" (application number: 200910235404.8). The average particle size of the obtained nano-hydrated iron phosphate is 20nm;

[0046] (2) Take 620g of FePO nano-hydrated iron phosphate prepared in step (1) 4 ·2H 2 O, roasted at 400°C for 12 hr to dehydrate to obtain anhydrous nano iron phosphate powder;

[0047] (3) Weigh 120g glucose, 500g anhydrous nano iron phosphate and 145g lithium hydroxide with an average particle size of 20nm (molar ratio Li:C:Fe=1.04:1.2:1), add 2000ml water, 80mg polyvinyl alcohol, In the basket ball mill, the ball mill was mixed for 3 hours, and the ball mi...

Embodiment 3

[0053] The preparation of lithium iron phosphate nanometer lithium ion battery cathode material is carried out according to the following steps:

[0054] (1) Using ferric chloride, ammonium dihydrogen phosphate and ammonia as raw materials, the rotating packed bed method is used to prepare nano-hydrated iron phosphate. For details, please refer to the applicant’s patent "A method for preparing nano-iron phosphate" (application number: 200910235404.8 ), the average particle size of the obtained nano-hydrated iron phosphate is 50nm;

[0055] (2) Take 620g of FePO nano-hydrated iron phosphate prepared in step (1) 4 ·2H 2 O, roasted at 450°C for 10 hr in an air atmosphere to obtain anhydrous nano iron phosphate powder;

[0056] (3) Weigh 100g pentaerythritol, 500g anhydrous nano-iron phosphate and 350g nano-lithium acetate (Li:C:Fe=1.04:1.11:1) with an average particle size of 60nm, add 1000ml of water, and add 40mg of sodium lauryl sulfate , Ball milling and mixing in a basket ball mil...

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Abstract

The invention discloses a preparation method of a lithium ion battery cathode material nano lithium iron phosphate which belongs to the technical field of nano lithium iron phosphate preparation. The method comprises the following steps: preparing hydrous nano iron phosphate by a rotating packed bed method; roasting and dehydrating the hydrous nano iron phosphate to obtain anhydrous nano iron phosphate powder; weighing lithium source compound, carbon source compound and anhydrous nano iron phosphate according to a stoichiometric ratio, adding pure water and a dispersant, mixing and stirring the mixture uniformly, preparing a slurry, performing spray drying of the prepared slurry, performing heat treatment of the obtained powder with the protection of inert gas to obtain the nano lithium iron phosphate material. The nano lithium iron phosphate material prepared by the invention has uniform components and good batch stability, has specific discharge capacity at 1C rate of more than 130 mAh / g and specific discharge capacity at 5C rate of more than 110 mAh / g at room temperature, and has great application value in the power-type lithium ion battery field. The method is applicable to large-scale production, and has low cost.

Description

Technical field [0001] The invention belongs to the technical field of preparation of nanometer lithium iron phosphate, and particularly relates to a preparation method of nanometer lithium iron phosphate as a positive electrode material of a lithium ion battery. Background technique [0002] Lithium Iron Phosphate (LiFePO 4 ) Is a new type of cathode material for lithium-ion batteries developed in recent years. It has the advantages of rich sources of raw materials, low preparation cost, high specific capacity, good cycle performance, and low environmental pollution. At present, it has been widely used in a new generation of power or energy storage lithium-ion batteries. [0003] However, it still has shortcomings in terms of high-current charge and discharge performance, low temperature performance, volumetric specific energy, etc. These problems have seriously affected the energy density, power density and other performance of the battery, and also affected the operating perfor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/1397
CPCY02E60/122Y02E60/10
Inventor 蒲薇华任建国武玉玲何向明李建军高剑万春荣姜长印
Owner TSINGHUA UNIV
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