A kind of lithium-rich manganese-based solid solution/graphene composite material and preparation method thereof

A lithium-rich manganese-based, composite material technology, applied in electrical components, battery electrodes, circuits, etc., can solve problems such as poor rate performance, and achieve the effects of short cycle, simple process, and improved rate performance

Active Publication Date: 2015-12-09
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to overcome the defect of poor rate performance of lithium-rich manganese-based solid solution as the positive electrode material of lithium ion batteries, and prepare lithium ion battery positive electrode materials with higher rate discharge specific capacity and excellent high rate cycle performance

Method used

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  • A kind of lithium-rich manganese-based solid solution/graphene composite material and preparation method thereof
  • A kind of lithium-rich manganese-based solid solution/graphene composite material and preparation method thereof
  • A kind of lithium-rich manganese-based solid solution/graphene composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] Example 1 Using nitrate as a raw material, a lithium-rich manganese-based solid solution / graphene composite was prepared by co-precipitation

[0073] (1) Prepare Ni(NO 3 ) 2 ·6H 2 O, Co(NO 3 ) 2 ·6H 2 O and Mn(NO 3 ) 2 mixed solution, the total concentration of transition metal ions is 0.8mol L -1 . Use 1.5mol L -1 NaOH solution as precipitant, 0.3mol L -1 Ammonia solution is used as a complexing agent, and a certain amount of graphene oxide is added at the bottom of the CSTR reaction vessel, wherein the total amount of raw materials (Ni(NO 3 ) 2 ·6H 2 O, Co(NO 3 ) 2 ·6H 2 O and Mn(NO 3 ) 2 ) and graphene oxide weight ratio are 10:0.5;

[0074] (2) Under the protection of an inert gas, the three solutions are co-currently added to the reactor containing the graphene bottom liquid through a peristaltic pump. During the reaction, the pH is controlled to be 11, the stirring speed is 1000rpm, the reaction temperature is 60°C, and the reaction time is 12h....

Embodiment 2

[0080] Example 2 Using sulfate as a raw material, a lithium-rich manganese-based solid solution / graphene composite was prepared by co-precipitation

[0081] (1) Prepare NiSO according to the required molar ratio (0.58:0.11:0.11) 4 ·6H 2 O﹑CoSO 4 ·7H 2 O and MnSO 4 ·H 2 O mixed solution, the total concentration of transition metal ions is 1.0mol L -1 . Use 2.0mol·L -1 NaOH solution as precipitant, 0.5mol L -1 Ammonia solution is used as a complexing agent, and a certain amount of graphene oxide is added at the bottom of the CSTR reaction vessel, wherein the raw material (NiSO 4 ·6H 2 O﹑CoSO 4 ·7H 2 O and MnSO 4 ·H 2 O) and graphene oxide weight ratio are 10:0.5;

[0082] (2) Under the protection of an inert gas, the three solutions are co-currently added to the reactor containing the graphene bottom liquid through a peristaltic pump. During the reaction, the pH is controlled to be 11, the stirring speed is 1000rpm, the reaction temperature is 50°C, and the reactio...

Embodiment 3

[0086] Example 3 Using acetate as a raw material and methanol as an organic solvent, a lithium-rich manganese-based solid solution / graphene composite material was prepared by a solvothermal method.

[0087] (1) The molar ratio (0.58:0.11:0.11) of CH 3 COOLi, (CH 3 COO) 2 Co, (CH 3 COO) 2 Mn, (CH 3 COO) 2 Ni and graphene oxide (the total amount of raw materials (CH 3 COOLi, (CH 3 COO) 2 Co, (CH 3 COO) 2 Mn and (CH 3 COO) 2 The weight ratio of Ni) to graphene oxide is 10:0.5) dissolved or dispersed (for graphene oxide) in methanol, fully stirred to form a mixed dispersion;

[0088] (2) Prepare 1.0mol·L -1 The oxalic acid solution is slowly added in the mixed solution formed in the previous step by a certain molar ratio (the mol ratio of Co and Ni ion total amount to oxalic acid is 1.3:1);

[0089] (3) At room temperature, stir magnetically for 2 hours to make it pre-react;

[0090] (4) All the solutions were transferred to the reactor and reacted at 200°C for 10 h...

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Abstract

The invention provides a lithium-manganese-rich based solid solution / graphene composite material and a preparation method thereof, which are applicable to the technical field of energy materials. The structural general formula of the lithium-manganese-rich based solid solution is xLi2MnO3.(1-x)LiMo2, wherein M is one of Ni, Co, Mn, Cr, Ni-Co, Ni-Mn, Ni-Co-Mn, Fe and Ru, and x is greater than 0 and smaller than 1. The lithium-manganese-rich based solid solution / graphene composite material is characterized in that the lithium-manganese-rich based solid solution is dispersed among layers of the layered graphene in a granular form. The lithium-manganese-rich based solid solution / graphene composite material, provided by the invention, can be used as an anode material for a lithium ion cell, and can effectively improve the electrical conductivity of the lithium-manganese-rich based solid solution. The preparation method has the characteristics of simple technology, low cost and suitability for large-scale production.

Description

technical field [0001] The invention relates to a lithium-rich manganese-based solid solution / graphene composite material and a preparation method thereof, belonging to the technical field of electrochemistry and material synthesis. Background technique [0002] Lithium-rich manganese-based solid solution cathode material xLi with layered structure 2 MnO 3 ·(1-x)LiMO 2 (where M is a transition metal, 0<x<1) the theoretical specific capacity exceeds 300mAh g -1 , the actual available capacity is greater than 250mAh·g -1 , which is about twice the actual capacity of the currently used positive electrode material; 2 and LiNi 1 / 3 mn 1 / 3 co 1 / 3 o 2 Compared with it, it also has the advantages of low cost, good safety, and environmental friendliness. Therefore, xLi 2 MnO 3 ·(1-x)LiMO 2 It is regarded as an ideal choice for the cathode material of the next generation of lithium-ion batteries. However, its poor rate performance limits its further development in co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/505H01M4/525H01M4/62
CPCH01M4/364H01M4/505H01M4/525H01M4/625Y02E60/10
Inventor 王要兵姚建年洪茂椿付芳
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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