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Preparation method of phase-change type LiFeSO4F cell material stable at high temperature, electrode plate, and usage of lithium ion cell

A lithium-ion battery, high temperature stable technology, applied in battery electrodes, secondary batteries, secondary battery repair/maintenance, etc. Erosion, effect of high capacity retention

Active Publication Date: 2017-10-03
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] There is no literature report on LiFeSO with Triplite structure 4 Charge-discharge performance and phase transition process of F at high temperature

Method used

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  • Preparation method of phase-change type LiFeSO4F cell material stable at high temperature, electrode plate, and usage of lithium ion cell
  • Preparation method of phase-change type LiFeSO4F cell material stable at high temperature, electrode plate, and usage of lithium ion cell
  • Preparation method of phase-change type LiFeSO4F cell material stable at high temperature, electrode plate, and usage of lithium ion cell

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] A high-temperature stable phase-change lithium iron fluorosulfate battery material and a preparation method thereof, comprising the following steps:

[0044] S1.1 by FeSO 4 Measuring ratio to weigh FeSO 4 ·7H 2 O powder, ground, placed in a tube furnace and calcined in argon at 390 °C for 2 hours to obtain FeSO 4 powder.

[0045] S1.2 Weigh the FeSO prepared in step S1.1 according to the molar ratio of 1:1.05 4 and LiF, using ethanol as a medium in a planetary ball mill for 2 hours (the mass ratio of the mixture and ethanol is 3:1), to obtain a slurry, vacuum drying, to obtain FeSO 4 / LiF mixed powder. The mixed powder was calcined in an argon furnace at 450°C for 0.75 hours and ground to obtain LiFeSO 4 F pure phase powder.

[0046] S1.3 the LiFeSO obtained in step S1.2 4 F pure phase powder and nano-conductive carbon (nano-SP) were mixed and ball-milled at a mass ratio of 3.5:1 to obtain uniform LiFeSO 4 F / C carbon coated powder.

[0047] S1.4 LiFeSO obtaine...

Embodiment 2

[0056] FeSO in embodiment two 4 The powder, carbon source, electrolyte, negative electrode sheet and separator are the same as those in Example 1, and the calcination time for synthesizing lithium iron fluorosulfate is different.

[0057] S2.1 will obtain FeSO by embodiment one 4 / LiF mixed powder was calcined in an argon furnace at 450°C for 2.25 hours and ground to obtain LiFeSO 4 F pure phase powder.

[0058] Figure 7 For adopting the LiFeSO prepared in embodiment two 4 XRD pattern of F powder. The results demonstrate the synthesis of pure-phase LiFeSO 4 F.

Embodiment 3

[0060] FeSO in embodiment three 4 The powder, carbon source, electrolyte, negative electrode sheet and separator are the same as those in Example 1, and the calcination temperature for synthesizing lithium iron fluorosulfate is different.

[0061] S3.1 will obtain FeSO by embodiment one 4 / LiF mixed powder was calcined in an argon furnace at 500°C for 0.75 hours and ground to obtain LiFeSO 4 F pure phase powder.

[0062] Figure 8 For adopting the LiFeSO prepared in Example 3 4 XRD pattern of F powder. The results demonstrate the synthesis of pure-phase LiFeSO 4 F.

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Abstract

The invention provides a preparation method of a phase-change type LiFeSO4F cell material stable at high temperature, an electrode plate, and usage of a lithium ion cell. The preparation method of the cell material comprises the following steps of first, weighing one of the followings according to a stoichiometric ratio of FeSO4: i. iron source and sulfur source, and ii. iron-sulfur source, grinding and mixing, and calcining in an inert gas for 1-2 hours at 380-400 DEG C, so as to obtain FeSO4 pure phase powder; second, preparing LiFeSO4F powder: weighing, according to a stoichiometric ratio of LiFeSO4F, ferrous sulfate powder and lithium fluoride powder prepared in the first step, grinding to obtain Li-Fe-S-O-F precursor powder, wherein the molar mass of the lithium fluoride powder is 1-1.05 times that of the ferrous sulfate; and third, calcining mixed powder obtained in the second step in the inert gas for 0.75-2.25 hours at 450-500 DEG C, so as to obtain LiFeSO4F pure phase powder. In charging and discharging of the cell material prepared by the method, phase change from LiFeSO4F of a Triplite structure to LiFeSO4F(1-x)(OH)x of a Tavorite structure occurs, an obvious -3.2V voltage platform is formed, and cycle stability of charging and discharging at 20-60 DEG C is high.

Description

technical field [0001] The invention relates to a method for preparing a high-temperature stable phase-change lithium iron fluorosulfate battery material and a method for using an electrode sheet and a lithium-ion battery, and belongs to the technical field of new electrochemical energy storage materials and their preparation. Background technique [0002] Lithium-ion batteries are considered to be a new type of green energy that can replace fossil energy. At present, commercialized lithium-ion batteries have technical difficulties in terms of structural stability, safety, and high / low temperature stability. At 3.45V lithium iron phosphate (LiFePO 4 ) Introducing fluoride ions into the anion group of the positive electrode material can obtain Tavorite structure lithium iron phosphate (LiFePO 4 F), making the ion channel change from one-dimensional to three-dimensional, increasing the ion conductivity by more than two orders of magnitude, but reducing the working potential t...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/0525H01M4/1397H01M10/42
CPCH01M4/1397H01M4/366H01M4/5825H01M4/628H01M10/0525H01M10/4235Y02E60/10
Inventor 邵刚勤马霏霏毛家威范书豪朱璨张安乐谢贵震顾佳妮晏佳礼
Owner WUHAN UNIV OF TECH
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