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Preparation method of copper-based fluoride solid solution sodium ion battery positive electrode material

A technology for sodium ion batteries and cathode materials, which is applied in the preparation of fluoride, battery electrodes, chemical instruments and methods, etc., can solve the use of electrode materials that cannot be used in secondary batteries, the self-stability is not excellent enough, and the growth rate of copper element is fast, etc. The problem is to achieve the effect of inhibiting the growth of copper particles, excellent electrochemical performance, and simple and convenient synthesis route.

Inactive Publication Date: 2020-04-17
WUHAN MARINE ELECTRIC PROPULSION RES INST CHINA SHIPBUILDING IND CORP NO 712 INST
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In recent years, the more popular positive electrode materials in academic papers mainly include manganese-based layered positive electrode materials and fast ion conductor structure phosphate positive electrode materials. The specific capacity of these two types of positive electrode materials rarely exceeds 180mAh / g. Moreover, the synthesis conditions of these two types of materials are relatively harsh, and their own stability is not excellent enough. Therefore, sodium-ion batteries urgently need to prepare electrode materials with higher specific capacity and simpler synthesis methods.
[0004] The research hotspot of fluoride cathode materials is mainly on iron-based fluoride, which has a high specific capacity, but has a large polarization during the discharge process.
Copper fluoride (CuF 2 ) as an electrode material has a super high theoretical specific capacity and potential, but the growth rate of copper is relatively fast during the discharge process, so it cannot be used as an electrode material for a secondary battery

Method used

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  • Preparation method of copper-based fluoride solid solution sodium ion battery positive electrode material
  • Preparation method of copper-based fluoride solid solution sodium ion battery positive electrode material
  • Preparation method of copper-based fluoride solid solution sodium ion battery positive electrode material

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Experimental program
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Effect test

Embodiment 1

[0020] 10.01g copper fluoride (CuF 2 , purity greater than 97%) and 9.38g ferrous fluoride (FeF 2 Purity greater than 97%) was added to a 150ml zirconia ball mill jar, zirconia balls were used as the grinding medium, the ball-to-material ratio was 2:1, and a sealing film was used to seal the ball mill jar. Assemble the ball mill jar on a high-energy ball mill, and perform ball milling at a speed of 250r / min for 10 hours. After ball milling, a solid solution of copper fluoride and ferrous fluoride (Cu 0.5 Fe 0.5 f 2 ). According to Cu 0.5 Fe 0.5 f 2 The mass ratio of the solid solution is to add 5% Ketjen black (KB) relative to the mass of fluoride in the ball milling jar, seal the ball milling jar, and mill at a speed of 200r / min for 4h to obtain Cu 0.5 Fe 0.5 f 2 @C Composite electrode materials.

[0021] figure 1 , image 3 with Figure 5 The test results show that the electrode material synthesized according to this method is pure phase Cu 0.5 Fe 0.5 f 2 Sol...

Embodiment 2

[0023] According to the method in embodiment 1 FeF 2 The powder is replaced with the same molar amount of NiF 2 , can get Cu 0.5 Ni 0.5 f 2 Fluoride solid solution and Cu 0.5 Ni 0.5 f 2 Composite electrode materials of @C.

[0024] figure 2 , Figure 4 The test results show that the electrode material synthesized according to this method is a pure phase Ni0.5Fe0.5F2 solid solution without CuF 2 Monomer phase.

Embodiment 3

[0026] Regulate MF 2 Fluoride monomer molar ratio, the same method can be used to obtain a series of copper-based fluoride sodium ion battery electrode material Cu with different copper content x m y f 2 , where the value of xy must satisfy x0.1.

[0027] The present invention mainly consists of CuF 2 as the basic material CoF 2 , FeF 2 、NiF 2 and other fluorides through the method of high-energy ball milling to synthesize copper-based fluoride solid solution positive electrode materials, and FeF 2 with CuF 2 Prepared as a solid solution, it can reduce the self-polarization of the iron-based fluoride, and at the same time inhibit the growth of copper elemental particles during the discharge process, and overcome the shortcomings of the two materials.

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Abstract

The invention discloses a preparation method of a copper-based fluoride solid solution sodium ion battery positive electrode material with high capacity and high specific energy. CuF2 and MF2 fluoridemonomers are prepared into a pure-phase copper-based fluoride solid solution CuxMyF2 by adopting a single ball milling method, and then the pure-phase copper-based fluoride solid solution CuxMyF2 iscompounded with a kohlrabi black conductive agent to prepare the sodium ion battery positive electrode material. According to the method, a single ball milling mode is adopted in the synthesis process; the preparation method is simple to operate, high in synthesis efficiency, easy to realize large-scale production and relatively high in practicability, and the sodium ion battery positive electrodematerial prepared by the method provided by the invention shows excellent electrochemical properties that the specific capacity is greater than 450 mAh / g and the discharge mean voltage is greater than 1.8 V in an actual test.

Description

technical field [0001] The invention belongs to the technical field of electrode materials for sodium ion batteries, and in particular relates to a method for preparing a copper-based fluoride solid solution sodium ion battery cathode material with high specific capacity and high specific energy. Background technique [0002] Sodium-ion battery is a new type of chemical power source that has been gradually developed in recent years. With the gradual deepening of the application of lithium-ion batteries, lithium source materials (LiCO 3 , LiOH, etc.) cobalt source material (Co 3 o 4 、CoSO 4 ) is also increasing year by year. Compared with lithium-ion batteries, sodium-ion batteries have the advantages of abundant resources and low price. At the same time, sodium ions have similar physical and chemical properties to lithium ions. These advantages have inspired researchers to study sodium-ion batteries. However, the large ionic radius makes the intercalation and deintercal...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M4/62H01M10/054C01B9/08C01G49/00C01G51/00C01G53/00
CPCC01B9/08C01G49/009C01G51/006C01G53/006C01P2002/72C01P2004/03C01P2006/40H01M4/582H01M4/625H01M10/054Y02E60/10
Inventor 张明林立
Owner WUHAN MARINE ELECTRIC PROPULSION RES INST CHINA SHIPBUILDING IND CORP NO 712 INST
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