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Template-free hydrothermal preparation method of hierarchical porous LiMn<x>Fe<1-x>PO4/C composite microsphere positive electrode material

A technology of composite microspheres and positive electrode materials, applied in battery electrodes, electrical components, electrochemical generators, etc., can solve the problem of time-consuming and complex synthesis methods

Active Publication Date: 2020-10-23
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, LiMn reported in the prior art x Fe 1-x PO 4 The synthesis method of microspheres is time-consuming and complicated, requiring the use of hard / soft templates, pre-synthesized LiMn x Fe 1-x PO 4 Microspheres or use other methods to synthesize nanostructure precursors

Method used

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  • Template-free hydrothermal preparation method of hierarchical porous LiMn&lt;x&gt;Fe&lt;1-x&gt;PO4/C composite microsphere positive electrode material
  • Template-free hydrothermal preparation method of hierarchical porous LiMn&lt;x&gt;Fe&lt;1-x&gt;PO4/C composite microsphere positive electrode material
  • Template-free hydrothermal preparation method of hierarchical porous LiMn&lt;x&gt;Fe&lt;1-x&gt;PO4/C composite microsphere positive electrode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1. LiMn 0.1 Fe 0.9 PO 4 Preparation of microsphere materials:

[0037] (1) 0.587g LiOH·H 2 O, 0.5g Mn(NO 3 ) 2 Solution (Mn(NO 3 ) 2 The mass fraction is 50%), 5.08gFe(NO 3 ) 3 9H 2 O, 1.61 g NH 4 h 2 PO 4 and 1.26g of glucose were added into 75ml of deionized water, and under continuous stirring conditions, a gray-green suspension was obtained;

[0038] (2) Transfer the suspension obtained in step (1) to a 100ml stainless steel autoclave for hydrothermal reaction, and the reaction conditions are 180° C. for 9 hours;

[0039] (3) After the hydrothermal reaction, the reaction kettle was naturally cooled to room temperature, the product was filtered with suction and washed with deionized water, and dried in a vacuum oven at 60°C for 12 hours to obtain LiMn 0.1 Fe 0.9 PO 4 Precursor powder;

[0040] (4) LiMn obtained from step (3) 0.1 Fe 0.9 PO 4 Precursor powder placed in Ar / H 2 (H 2 In a tube furnace with a volume fraction of 5%) atmosphere, at 5°C ...

Embodiment 2

[0052] 1. LiMn 0.2 Fe 0.8 PO 4 Preparation of microsphere materials

[0053] (1) 0.587g LiOH·H 2 O, 0.423g MnSO 4 , 1.7g FeSO 4 , 1.61g NH 4 h 2 PO 4 and 1.26g of glucose were added to 75ml of deionized water, and under continuous stirring conditions, a gray-green suspension was obtained;

[0054] (2) Transfer the suspension obtained in step (1) to a 100ml stainless steel autoclave for hydrothermal reaction, and the reaction conditions are 180° C. for 9 hours;

[0055] (3) After the hydrothermal reaction, the reaction kettle was naturally cooled to room temperature, the product was filtered with suction and washed with deionized water, and dried in a vacuum oven at 60°C for 12 hours to obtain LiMn 0.2 Fe 0.8 PO 4 Precursor powder;

[0056] (4) LiMn obtained in step (3) 0.2 Fe 0.8 PO 4 Precursor powder placed in Ar / H 2 (H 2 In a tube furnace with a volume fraction of 5%) atmosphere, at 5°C min -1 The heating rate was increased to 650°C for 10 hours to obtain L...

Embodiment 3

[0064] 1. LiMn 0.5 Fe 0.5 PO 4 Preparation of microsphere materials

[0065] (1) 0.587g LiOH·H 2 O, 0.88g MnCl 2 , 1.135g FeCl 3 , 1.61g NH 4 h 2 PO 4 and 1.26g of glucose were added to 75ml of deionized water, and under continuous stirring conditions, a gray-green suspension was obtained;

[0066] (2) Transfer the suspension obtained in step (1) to a 100ml stainless steel autoclave for hydrothermal reaction, and the reaction conditions are 180° C. for 9 hours;

[0067] (3) After the hydrothermal reaction, the reaction kettle was naturally cooled to room temperature, the product was filtered with suction and washed with deionized water, and dried in a vacuum oven at 60°C for 12 hours to obtain LiMn 0.5 Fe 0.5 PO 4 Precursor powder;

[0068] (4) LiMn obtained from step (3) 0.5 Fe 0.5 PO 4 Precursor powder placed in Ar / H 2 (H 2 In a tube furnace with a volume fraction of 5%) atmosphere, at 5°C min -1 The heating rate is increased to 650 ° C for 10 hours to obta...

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Abstract

The invention belongs to the technical field of electrochemical energy storage materials, and discloses a template-free hydrothermal preparation method of a hierarchical porous LiMn<x>Fe<1-x>PO4 / C composite microsphere positive electrode material. The method comprises the steps of nanoparticle formation and self-assembly, carrying out a dissolving-precipitating process in a hydrothermal reaction process, and carrying out simple carbon coating to obtain the porous LiMn<x>Fe<1-x>PO4 / C microspheres, which are of a hierarchical porous microsphere structure, consist of nanoscale LiMn<x>Fe<1-x>PO4 main particles with relatively high crystallinity, and are internally provided with uniform carbon coatings. The unique structure of the hierarchical porous LiMn<x>Fe<1-x>PO4 / C composite microsphere positive electrode material obtained by the invention is combined with design principles of structure, morphology and components at the same time, and the hierarchical porous LiMn<x>Fe<1-x>PO4 / C composite microsphere positive electrode material has excellent structural stability and conduction advantages on electrons and lithium ions.

Description

technical field [0001] The invention relates to the technical field of electrochemical energy storage materials, in particular to a hierarchical porous LiMn x Fe 1- x PO 4 Template-free hydrothermal preparation method of / C composite microsphere cathode material. Background technique [0002] Olivine transition metal phosphate LiMPO 4 (M = Fe, Mn, Ni, or Co) have been considered as potential cathode materials for a class of rechargeable Li-ion batteries due to their good cycle stability, heat resistance, and safety. Among them, LiFePO 4 (LFP) is the most successful and has been applied on a large scale in electric vehicles. However, LiFePO 4 The poor conductivity and low theoretical specific energy make it difficult to meet the increasing demand for higher energy density in practical applications. In this regard, LiMnPO 4 (LMP) is more attractive because it has a higher 4 Higher energy density and higher operating voltage (~4.1V vs. Li + / Li), can provide ratio Li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/485H01M4/58H01M4/62H01M10/0525
CPCH01M4/485H01M4/5825H01M4/625H01M4/366H01M10/0525Y02E60/10
Inventor 孙福根李亚辉丁国彧景鑫国严奉乾朱振徐国军李晓敏岳之浩周浪
Owner NANCHANG UNIV
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