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A preparation method of a high-temperature stable phase-change lithium iron fluorosulfate battery material and a method of using an electrode sheet and a lithium-ion battery

A lithium-ion battery, high-temperature stable technology, applied in the direction of battery electrodes, secondary batteries, secondary battery repair/maintenance, etc., can solve the problems of charging and discharging performance and phase change process that have not been reported in the literature, and achieve high discharge capacity, cycle Good stability, good stability effect

Active Publication Date: 2021-02-19
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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  • A preparation method of a high-temperature stable phase-change lithium iron fluorosulfate battery material and a method of using an electrode sheet and a lithium-ion battery
  • A preparation method of a high-temperature stable phase-change lithium iron fluorosulfate battery material and a method of using an electrode sheet and a lithium-ion battery
  • A preparation method of a high-temperature stable phase-change lithium iron fluorosulfate battery material and a method of using an electrode sheet and a lithium-ion battery

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Experimental program
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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 high-temperature stable phase-change lithium iron fluorosulfate battery material and a method of using an electrode sheet and a lithium ion battery. The preparation of this battery material comprises the following steps: 1) according to FeSO 4 Measuring ratio Weigh one of the following two kinds: ① iron source and sulfur source, ② iron and sulfur source, grind and mix, and calcinate in inert gas at 380-400 ℃ for 1-2 hours to obtain FeSO 4 Pure phase powder; 2) LiFeSO 4 Preparation of F powder: by LiFeSO 4 F metering ratio takes step 1) made ferrous sulfate powder and lithium fluoride powder, grinds, obtains Li-Fe-S-O-F precursor powder, wherein the molar weight of lithium fluoride powder is that of ferrous sulfate 1 to 1.05 times the molar weight; 3) Calcining the mixed powder obtained in step 2) in an inert gas at 450 to 500°C for 0.75 to 2.25 hours to obtain LiFeSO 4 F pure phase powder. The battery material prepared by the present invention is produced by the Triplite structure LiFeSO in the charge and discharge process 4 F transformed into Tavorite structure LiFeSO 4 f 1‑x (OH) x phase transition, forming an obvious ~3.2V voltage platform, and has good charge-discharge cycle stability at 20-60°C.

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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Patent Type & Authority Patents(China)
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