Preparation method of carbon-coated lithium iron phosphate material with carbon black as carbon source

A carbon-coated lithium iron phosphate and carbon source technology, which is applied to electrical components, battery electrodes, circuits, etc., can solve the problems of low electronic conductivity of lithium iron phosphate and slow diffusion of lithium ions, and improve safety and battery performance , low cost and easy synthesis

Inactive Publication Date: 2013-10-09
HUBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The invention solves the problems of low electronic conductivity of lithium iron phosphate and slow diffusion of lithium ions, and uses cheap precursors, which reduces production costs and enables large-scale industrial production

Method used

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  • Preparation method of carbon-coated lithium iron phosphate material with carbon black as carbon source
  • Preparation method of carbon-coated lithium iron phosphate material with carbon black as carbon source
  • Preparation method of carbon-coated lithium iron phosphate material with carbon black as carbon source

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Ferric nitrate ( Fe(NO 3 ) 3 9H 2 O) 3.9400g, ammonium dihydrogen phosphate (NH 4 h 2 PO 4 ) 1.3452g, citric acid ( C 6 h 8 o 7 ·H 2 O) 2.3155g are mixed to form a homogeneous mixture;

[0021] (2) Slowly add lithium acetate (LiAc·2H 2 O) 1.4143 g of solution to form a mixed material;

[0022] (3) Heat the mixed material to 60°C. When the solution starts to become turbid, impregnate the mesoporous carbon CMK-3 into the solution and stir for 30 minutes, then sonicate for 10 minutes, stir and ultrasonically cycle 3 times in turn until the solution becomes It is muddy; (4) Ultrasonicate and stir the obtained muddy material again for 5 times, and put it in an oven with a constant temperature of 120°C for drying;

[0023] (5) Grinding the dried material for 12 hours;

[0024] (6) Put the obtained powder material into a tube furnace with argon gas, and calcined at three stages of temperature, 220°C for 1 hour, 350°C for 2 hours, and 700°C for 6 hours to obtain...

Embodiment 2

[0028] (1) Ferric nitrate ( Fe(NO 3 ) 3 9H 2 O) 4.3856g, ammonium dihydrogen phosphate (NH 4 h 2 PO 4 ) 1.2539g, citric acid ( C 6 h 8 o 7 ·H 2 O) 2.4231 g are mixed to form a homogeneous mixture;

[0029] (2) Slowly add lithium acetate (LiAc·2H 2 O) 1.3652 g of solution to form a mixed material;

[0030] (3) Heat the mixed material to 70°C. When the solution starts to become turbid, impregnate the mesoporous carbon CMK-3 into the solution and stir for 30 minutes, then sonicate for 10 minutes, and then stir and sonicate for 5 times until the solution becomes turbid. It is muddy; (4) Ultrasonicate and stir the obtained muddy material again for 5 times, and put it into an oven with a constant temperature of 130°C for drying;

[0031] (5) Grinding the dried material for 20 hours;

[0032](6) Put the obtained powder material into a tube furnace with argon gas, and calcine it at three stages of temperature, 220°C for 1 hour, 350°C for 3 hours, and 700°C for 7 hours to o...

Embodiment 3

[0036] (1) Ferric nitrate ( Fe(NO 3 ) 3 9H 2 O) 3.5266g, ammonium dihydrogen phosphate (NH 4 h 2 PO 4 ) 1.9421g, citric acid ( C 6 h 8 o 7 ·H 2 O) 2.5324 g are mixed to form a homogeneous mixture;

[0037] (2) Slowly add lithium acetate (LiAc·2H 2 O) 1.7421 g of solution to form a mixed material;

[0038] (3) Heat the mixed material to 80°C. When the solution starts to become turbid, impregnate the mesoporous carbon CMK-3 into the solution and stir for 30 minutes, then sonicate for 10 minutes, stir and ultrasonically cycle 4 times until the solution turns It is muddy; (4) Ultrasonicate and stir the obtained muddy material again for 5 times, and put it in an oven with a constant temperature of 140°C for drying;

[0039] (5) Grinding the dried material for 18 hours;

[0040] (6) Put the obtained powder material into a tube furnace filled with argon, and calcined at three stages of temperature, 220°C for 1 hour, 350°C for 2 hours, and 700°C for 8 hours to obtain carbo...

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Abstract

The invention provides a preparation method of a carbon-coated lithium iron phosphate material with mesoporous carbon CMK-3 as a carbon source. The preparation method comprises the steps of mixing iron nitrate, ammonium dihydrogen phosphate and citric acid in a certain ratio to form a mixture, slowly dropwise adding a lithium acetate solution to the mixture under the action of stirring to form a mixed material, dipping mesoporous carbon CMK-3 into the solution at a certain temperature, carrying out stirring and ultrasonic treatment to obtain a slurry-shaped solution, drying the obtained slurry-shaped material at a constant temperature, grinding the dried slurry-shaped material and calcining the powder, thus obtaining the carbon-coated lithium iron phosphate powder material. The carbon-coated lithium iron phosphate material prepared by the preparation method has a grain size of 200-400nm, fine and uniform grains and high purity, thus increasing the electron conductivity and the ion diffusion rate. The preparation method is simple and practicable and fast, is pollution-free in preparation processes, can be completed in ordinary chemical laboratories, and can be used for large-scale industrial production. The carbon-coated lithium iron phosphate material prepared by the preparation method can serve as an anode material for lithium ion cells.

Description

technical field [0001] The invention relates to a method for preparing carbon-coated lithium iron phosphate capable of industrial production, and belongs to the field of positive electrode materials and electrochemistry of lithium ion batteries. Background technique [0002] Lithium iron phosphate (LiFePO 4 ) is a lithium battery cathode material with an olivine structure, which has the advantages of wide material sources, low price, non-toxicity, no environmental pollution, high energy density (theoretical specific capacity is 170mAh / g), and good lattice stability. The safe performance and long cycle life of lithium iron phosphate make it a research hotspot in recent years. LiFePO in nature 4 It mainly exists in the form of phospholithium ore, but its impurity content is high, so it cannot be directly used as the positive electrode material of lithium-ion batteries. [0003] Currently LiFePO 4 There are many synthetic methods of D, mainly hydrothermal method, sol-gel, r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M4/62
CPCY02E60/10
Inventor 王升富叶建董超熊华玉文为张修华冯传启
Owner HUBEI UNIV
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