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A graded porous limn x fe 1-x po 4 Template-free hydrothermal preparation of /c composite microsphere cathode materials

A technology of composite microspheres and cathode materials, applied in battery electrodes, structural parts, electrical components, etc., can solve the problem of time-consuming and complicated synthesis methods, and achieve the effect of improving electronic conductivity, fast Li+ conductivity, and easy control of conditions.

Active Publication Date: 2022-07-01
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • A graded porous limn <sub>x</sub> fe <sub>1-x</sub> po <sub>4</sub> Template-free hydrothermal preparation of /c composite microsphere cathode materials
  • A graded porous limn <sub>x</sub> fe <sub>1-x</sub> po <sub>4</sub> Template-free hydrothermal preparation of /c composite microsphere cathode materials
  • A graded porous limn <sub>x</sub> fe <sub>1-x</sub> po <sub>4</sub> Template-free hydrothermal preparation of /c composite microsphere cathode materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0037] (1) 0.587g LiOH·H 2 O, 0.5g Mn (NO 3 ) 2 Solution (Mn(NO 3 ) 2 The mass fraction of 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 the condition of continuous stirring, a gray-green suspension was obtained;

[0038] (2) transferring the suspension obtained in step (1) to a 100ml stainless steel autoclave for hydrothermal reaction, and the reaction condition is that the temperature is kept at 180°C for 9h;

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

[0040] (4) LiMn obtained in step (3) 0.1 Fe 0.9 PO 4 Precursor powder in Ar / H 2 (H 2 The volume fraction of 5%) at...

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 into 75ml of deionized water, and under the condition of continuous stirring, a gray-green suspension was obtained;

[0054] (2) transferring the suspension obtained in step (1) to a 100ml stainless steel autoclave for hydrothermal reaction, and the reaction condition is that the temperature is kept at 180°C for 9h;

[0055] (3) After the hydrothermal reaction is completed, the reaction kettle is naturally cooled to room temperature, the product is suction filtered and washed with deionized water, and dried in a vacuum drying 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 in Ar / H 2 (H 2 The volume fraction of 5%) atmosphere in a tube furnace at 5 °C min -1 The heating rate was incre...

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 into 75ml of deionized water, and under the condition of continuous stirring, a gray-green suspension was obtained;

[0066] (2) transferring the suspension obtained in step (1) to a 100ml stainless steel autoclave for hydrothermal reaction, and the reaction condition is that the temperature is kept at 180°C for 9h;

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

[0068] (4) LiMn obtained in step (3) 0.5 Fe 0.5 PO 4 Precursor powder in Ar / H 2 (H 2 The volume fraction of 5%) atmosphere in a tube furnace at 5 °C min -1 The heating rate was incr...

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Abstract

The invention belongs to the technical field of electrochemical energy storage materials, and discloses a graded porous LiMn x Fe 1‑x PO 4 Template-free hydrothermal preparation method of / C composite microsphere cathode material. The method includes the formation and self-assembly of nanoparticles, and the process of dissolution-precipitation during the hydrothermal reaction, and after simple carbon coating, porous LiMn is obtained x Fe 1‑x PO 4 / C microspheres, the microspheres are hierarchical porous microspheres composed of nano-scale LiMn with high crystallinity x Fe 1‑x PO 4 Main grain composition with a uniform carbon coating inside. The graded porous LiMn obtained by the present invention x Fe 1‑x PO 4 This unique structure of the / C composite microsphere cathode material simultaneously combines the design principles of structure, morphology, and composition, with excellent structural stability and conductive advantages for 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) has been considered as a potential cathode material for a class of rechargeable Li-ion batteries due to its good cycling 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 electrical conductivity is poor and the theoretical specific energy is low, which makes it difficult to meet the increasing requirements of higher energy density in practical applications. In this regard, LiMnPO 4 (LMP) is more attractive because it has better properties than LiFePO 4 Higher energy density and higher operating ...

Claims

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Application Information

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Patent Type & Authority Patents(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