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Method for preparing lithium iron phosphate electrode material based on two-time carbon addition process based on liquid phase mixing

A technology of lithium iron phosphate and electrode materials, applied in battery electrodes, secondary batteries, circuits, etc., can solve problems such as increased energy consumption, complicated process, and formation of a good carbon coating layer on the surface of lithium iron phosphate particles, so as to reduce production Effects of energy consumption, reduction of reaction temperature, improvement of batch stability and product performance

Inactive Publication Date: 2017-01-11
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

None of the above methods can solve the problem that it is difficult to form a good carbon coating layer on the surface of lithium iron phosphate particles due to the participation of carbon in the carbothermal reduction process.
[0007] CN102881902 discloses a so-called two-step method for preparing LiFePO by adding carbon source mechanical mixing twice and secondary high-temperature reaction 4 The process of the first mixing and high temperature reaction is to complete the carbothermal reduction and the synthesis of lithium iron phosphate, and the second mixing high temperature reaction process is to realize the carbon coating of lithium iron phosphate, but the second mixing and The secondary high-temperature reaction makes the process more complicated and also increases energy consumption

Method used

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  • Method for preparing lithium iron phosphate electrode material based on two-time carbon addition process based on liquid phase mixing
  • Method for preparing lithium iron phosphate electrode material based on two-time carbon addition process based on liquid phase mixing
  • Method for preparing lithium iron phosphate electrode material based on two-time carbon addition process based on liquid phase mixing

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Experimental program
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Effect test

Embodiment 1

[0041] Weigh 1.208gLiCl·H with the molar ratio of lithium: iron: phosphorus = 1:1:1 2 O, 5.406 g FeCl 3 ·6H 2 0, 2.3006gNH 4 h 2 PO 4, and 0.35g of sucrose, which were dissolved in 20ml of deionized water, and then placed in an oven at a temperature of 195°C and heated in a slightly boiling state. After it was completely dried, the obtained solid residue was mixed with absolute ethanol dissolved in 0.35g PEG400, and ball milled for 5h. The anhydrous ethanol in the obtained ball-milled product was dried, and a high-temperature carbothermal reduction reaction was carried out in a tube furnace under the protection of flowing argon. The reaction temperature was 750° C. and the reaction time was 8 hours. like figure 2 As shown, the position of the XRD diffraction peak is related to that of LiFePO 4 The standard card (JCPDS Card No. 83-2092) matches, indicating that the obtained product is LiFePO 4 .

Embodiment 2

[0043] The preparation steps in this example are exactly the same as those in Example 1 above. The difference is: Weigh 1.379g anhydrous lithium nitrate, 8.08gFe(NO 3 ) 3 9H 2 O, 2.3006gNH 4 h 2 PO 4 , and 1.25 g of sucrose as a reactant. like image 3 As shown, the position of the XRD diffraction peak is related to that of LiFePO 4 The standard card (JCPDS Card No. 83-2092) matches, indicating that the obtained product is LiFePO 4 . Figure 4 Shown is the SEM picture of the material, and the particle size of the material can be seen in the figure to be several hundred nanometers. like Figure 5 As shown, the initial discharge capacity of the material is 156mAh / g at a charge-discharge rate of 0.1C, and the plateau voltage difference is about 0.15V. exist Image 6 Among them, the discharge capacity of the material at 0.1C gradually increases with the activation of the battery and the full infiltration of the electrolyte in the first few cycles, reaching 163 mAh / g at...

Embodiment 3

[0045] The preparation steps in this example are exactly the same as those in Example 2 above. The difference is: (1) The molar ratio of the raw materials added is lithium: iron: phosphorus = 1.05:1:1. (2) 0.45g of PEG400 is added when chain organic matter is added. like Figure 7 As shown, the material in Example 3 has a discharge capacity of 158 mAh / g at 0.1C.

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Abstract

The invention relates to a method for preparing a lithium iron phosphate electrode material by using a twice carbon adding technology based on a liquid phase mixing material. The method comprises the following steps of firstly mixing a lithium source, an iron source, a phosphorus source and a carbon source material to prepare a liquid-state single phase mixture, mixing the obtained solid product with a volatile solvent containing a dissolved solubility organic compound, carrying out mechanical grinding on the obtained mixture so that organic compound and solid particles are mixed fully, so as to reduce the grain diameter of the solid. The carbon source materials in different space positions can respectively and simultaneously reduce ferric iron and coat the surface of lithium iron phosphate with carbon through the twice carbon adding technology, a purpose for preparing carbon coating structure lithium iron phosphate material in a primary high-temperature heating process is reached, and the completeness of a carbothermic reaction and the electric conductivity of the material are good. The method provided by the invention has the advantages that the cost is low, the energy dissipation is low, the cycle is short, and the batch stability is high.

Description

technical field [0001] The present invention relates to a LiFePO 4 The method of / C electrode material, especially a kind of process based on liquid-phase mixed materials adding carbon twice to prepare lithium iron phosphate (hereinafter written as LiFePO) with good carbon-coated structure 4 / C) The method of cathode material for lithium-ion power battery. Background technique [0002] Since the advent of lithium-ion secondary batteries in the early 1990s, they have attracted widespread attention due to their high energy density, good cycle performance, charge retention, and environmental protection, and have developed rapidly in recent years. Of which LiFePO 4 It has the advantages of stable structure, safety and reliability, and low price. The application potential of power batteries used in electric vehicles, hybrid vehicles and energy storage is widely optimistic. Issues such as pollution have broad implications. [0003] LiFePO 4 Belonging to the orthorhombic cryst...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58H01M4/62
CPCH01M4/366H01M4/5825H01M4/625H01M10/0525Y02E60/10
Inventor 赵哲李瑛朱明原夏侯照张敏胡业旻金红明
Owner SHANGHAI UNIV
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