Titanium and zirconium co-doped carbon-coated lithium iron phosphate material as well as preparation method and application thereof

A carbon-coated lithium iron phosphate and co-doping technology is applied in the preparation/purification of carbon, chemical instruments and methods, phosphorus compounds, etc. Electrical conductivity, cheap and wide range of raw materials, effect of improving compaction density

Active Publication Date: 2022-04-12
HUBEI WANRUN NEW ENERGY TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, titanium ion doping on LiFePO 4 The improvement effect of material compaction density is not too significant

Method used

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  • Titanium and zirconium co-doped carbon-coated lithium iron phosphate material as well as preparation method and application thereof
  • Titanium and zirconium co-doped carbon-coated lithium iron phosphate material as well as preparation method and application thereof
  • Titanium and zirconium co-doped carbon-coated lithium iron phosphate material as well as preparation method and application thereof

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preparation example Construction

[0024] The preparation method of the titanium and zirconium co-doped carbon-coated lithium iron phosphate material of the present invention is to mix iron phosphate, lithium carbonate, carbon source, titanium source and zirconium source in a liquid medium, and the mixture is ball milled and sand milled After reaching a certain slurry particle size, spray drying technology is used for granulation, and finally the dried spray material is sintered in an atmosphere furnace and then crushed to finally obtain titanium and zirconium co-doped carbon-coated lithium iron phosphate material; the specific steps are as follows :

[0025] (1) Weigh iron phosphate, lithium carbonate, titanium source and zirconium source according to the element molar ratio Li:Zr:Fe:Ti:P = 1-y:y:1-x:x:1 and put them in the liquid medium Mixing in, where 0.001≤x≤0.05, 0.001≤y≤0.02;

[0026] (2) Add carbon source to the mixture obtained in step (1) and then perform ball milling and sand milling, so that the pa...

Embodiment 1

[0041] Iron phosphate, lithium carbonate, tetrabutyl titanate and zirconium hydroxide are weighed according to the elemental molar ratio Li:Zr:Fe:Ti:P =0.985:0.015:0.99:0.01:1 and mixed in deionized water; After adding glucose to the mixture, it was ball-milled and sand-milled to control the particle size of the slurry at 0.4 µm; the slurry was spray-dried, the atomization frequency was 50 Hz, and the temperature of the heated air inlet was 200 °C. The tuyere temperature is 100°C; finally, the dry spray material is pre-sintered at 350°C for 3 hours in an atmosphere furnace filled with argon, and then sintered at 800°C for 10 hours; after the calcination is completed, it can be pulverized to obtain a black powder of titanium and zirconium co-doped Carbon-coated lithium iron phosphate material with a carbon content of 0.5wt% and a discharge capacity of 158.3 mAh g at 0.1C –1 , the first Coulombic efficiency is 98.4%, and the discharge capacity of 1C is 145.5 mAh g –1 , compacte...

Embodiment 2

[0043] Iron phosphate, lithium carbonate, titanium dioxide and zirconia are weighed and mixed in deionized water according to the elemental molar ratio Li:Zr:Fe:Ti:P = 0.98:0.02:0.96:0.04:1; After adding sucrose, it is ball milled and sand milled to control the particle size of the slurry at 0.2µm; the slurry is spray-dried, the atomization frequency is 60Hz, the temperature of the heated air inlet is 150°C, and the temperature of the air outlet is 70°C ;Finally, pre-sinter the dry spray material at 300°C for 5h in an atmosphere furnace filled with nitrogen, and then continue to sinter at 750°C for 12h; after the calcination is completed, it can be pulverized to obtain a black powder of titanium and zirconium co-doped carbon-coated lithium iron phosphate material, the carbon content of the material is 1.1wt%, and the discharge capacity at 0.1C is 159.1 mAh g –1 , the first Coulombic efficiency is 97.3%, and the discharge capacity of 1C is 148.0 mAh g –1 , compacted density 2....

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Abstract

The invention relates to a titanium and zirconium co-doped carbon-coated lithium iron phosphate material and a preparation method and application thereof, the chemical expression of the material is Li1-yZryFe1-xTixPO4 / C, titanium is doped to the Fe position, zirconium is doped to the Li position, 0.001 < = x < = 0.05, 0.001 < = y < = 0.02; the preparation method comprises the following steps: mixing iron phosphate, lithium carbonate, a carbon source, a titanium source and a zirconium source in a liquid-phase medium, carrying out ball milling and sand milling on the mixture to a certain slurry particle size, granulating by adopting a spray drying technology, and finally sintering the dried spray material in an atmosphere furnace. The material is applied to a lithium ion battery as a positive electrode material. The titanium and zirconium elements are doped into the carbon-coated lithium iron phosphate, so that the ion and electron transmission capability of the lithium iron phosphate is effectively enhanced, the compaction density of the material is improved, and the carbon-coated lithium iron phosphate is very suitable for being used as a high-energy and high-power-density lithium ion power battery positive electrode material.

Description

technical field [0001] The invention belongs to the technical field of new energy materials and their preparation, and in particular relates to a carbon-coated lithium iron phosphate material co-doped with titanium and zirconium and a preparation method thereof. The material can be used as a high-performance cathode material in lithium-ion power batteries. Background technique [0002] In 1997, J. Goodenough et al reported lithium iron phosphate (LiFePO 4 ) can be used as a cathode material for lithium-ion batteries. 4 industrial development process. Due to its advantages of long cycle life, high safety and low cost, LiFePO 4 It has rapidly developed into a very important cathode material for lithium-ion batteries. Lithium-ion batteries using this material as the cathode material have been widely used in fields including portable electronic devices, automobiles, ships and energy storage. In recent years, with the rapid development of my country's new energy vehicle indust...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45C01B32/05H01M4/38H01M4/58H01M4/62
CPCY02E60/10H01M4/58H01M4/38C01B32/05H01M4/62C01B25/45H01M4/366H01M4/5825H01M4/625H01M10/0525H01M2004/028C01P2004/80
Inventor 曹名磊
Owner HUBEI WANRUN NEW ENERGY TECH DEV
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