A kind of doped modified lithium ion battery vanadate negative electrode material and preparation method thereof

A technology for lithium ion batteries and negative electrode materials, applied in battery electrodes, active material electrodes, negative electrodes, etc., can solve the problems of low conductivity and volume expansion of materials, and achieve the effects of expanding intercalation and deintercalation channels, easy control, and simple operation.

Active Publication Date: 2022-06-24
NINGBO POLYTECHNIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a mixed transition metal oxide, this material also has the same problems as other transition metal oxides. The material has low electrical conductivity, and the volume expands and shrinks severely as lithium is intercalated and extracted in the material during charge and discharge.

Method used

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  • A kind of doped modified lithium ion battery vanadate negative electrode material and preparation method thereof
  • A kind of doped modified lithium ion battery vanadate negative electrode material and preparation method thereof
  • A kind of doped modified lithium ion battery vanadate negative electrode material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Accurately weigh 0.85mol Fe(OH) 3 , 0.14molSb(OH) 3 , 1.0molNH 4 VO 3 , 0.03mol NH 4 F, put into the ball milling tank of the planetary ball mill, add deionized water, and ball mill to obtain a rheological phase mixture. While stirring, 1.0 mol / L oxalic acid solution was added dropwise to the rheological phase mixture, the pH of the mixture was adjusted to 5.8, and the mixture was fully stirred. The mixture was transferred to a stainless steel high-pressure tank, reacted at a constant temperature of 220° C. for 24 hours, taken out and dried, and then the solid mixture was pulverized to obtain a precursor powder. The precursor powder was heated in a program-controlled electric furnace, heated to 720°C at a heating rate of 5°C / min, and kept for 8 hours to obtain doped modified Fe. 0.85 Sb 0.14 VO 4 F 0.03 Vanadate anode material.

[0029] will be synthesized Fe 0.85 Sb 0.14 VO 4 F 0.03 The vanadate negative electrode material, acetylene black and polytetraflu...

Embodiment 2

[0031] Accurately weigh 0.25mol Fe 2 O 3 , 0.05molSb 2 O 3 , 1.0molNH 4 VO 3 , 0.01mol NH 4 F, put into the ball milling tank of the planetary ball mill, add deionized water, and ball mill to obtain a rheological phase mixture. While stirring, add 0.5 mol / L oxalic acid solution dropwise to the rheological phase mixture, adjust the pH of the mixture to 5.1, and stir well. The mixture was transferred to a stainless steel high-pressure tank, reacted at a constant temperature of 150° C. for 60 hours, taken out and dried, and the solid mixture was ground to obtain a precursor powder. The precursor powder was heated in a program-controlled electric furnace, heated to 500°C at a heating rate of 3°C / min, and kept for 1 hour to obtain doped modified Fe. 0.5 Sb 0.1 VO 4 F 0.01 Vanadate anode material.

[0032] will be synthesized Fe 0.5 Sb 0.1 VO 4 F 0.01 The vanadate negative electrode material, acetylene black and polytetrafluoroethylene are mixed uniformly in a mass ra...

Embodiment 3

[0034] Accurately weigh 0.6mol Fe(OH) 3 , 0.19molmolSb 2 O 3 , 1.0mol NH 4 VO 3 , 0.015mol HF, put it into the ball milling tank of a planetary ball mill, add an appropriate amount of deionized water, and ball mill to obtain a rheological phase mixture. While stirring, 1.0 mol / l oxalic acid solution was added dropwise to the rheological phase mixture, the pH of the mixture was adjusted to 5.5, and the mixture was fully stirred. The mixture was transferred to a stainless steel high-pressure tank, reacted at a constant temperature of 160° C. for 56 hours, taken out and dried, and then the solid mixture was pulverized to obtain a precursor powder. The precursor powder was heated in a program-controlled electric furnace, heated to 600°C at a heating rate of 4°C / min, and kept for 3 hours to obtain doped modified Fe 0.6 Sb 0.38 VO 4 F 0.015 Vanadate anode material.

[0035] will be synthesized Fe 0.6 Sb 0.38 VO 4 F 0.015 The vanadate negative electrode material, acetyle...

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Abstract

The invention relates to a doped modified lithium ion battery vanadate negative electrode material and a preparation method thereof, belonging to the field of lithium ion battery material preparation. The doped modified lithium ion battery vanadate negative electrode material is composed of iron source compound, antimony source compound, vanadate source compound and fluorine source compound in molar ratio Fe:Sb:VO 4 3‑ : F=x:y:1:z composition, wherein x=0.5-0.9, y=0.1-0.5, z=0.01-0.1. With vanadate as the main skeleton, ferric ions and antimony ions with different ionic radii and electronic structures and fluorine ions with smaller radii and stronger electronegativity are doped with each other to change the electric field distribution in the unit cell and expand the lithium ions in the crystal. The intercalation channel improves the migration rate of lithium ions, buffers the impact of lithium ions on the crystal structure due to crystal volume changes during the intercalation and extraction process, thereby improving the lithium storage performance of the material and greatly improving the performance of lithium-ion batteries doped with vanadate negative materials. cycle life.

Description

technical field [0001] The invention belongs to the field of preparation of lithium ion battery materials, and in particular relates to a vanadate negative electrode material of a doped modified lithium ion battery and a preparation method thereof. Background technique [0002] With the increasingly serious energy crisis and environmental pollution, human beings need more alternative and environmentally friendly new energy sources. As an environmentally friendly renewable energy, lithium-ion batteries have the advantages of high energy density, good safety performance, and environmental protection, and have received widespread attention in recent years. [0003] Anode materials are the key components of lithium-ion batteries. At present, the lithium storage anode materials that have been practically used in lithium ion batteries are basically carbon materials, such as artificial graphite, natural graphite, mesocarbon microspheres, petroleum coke, carbon fiber, pyrolysis res...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58H01M10/0525
CPCH01M4/5825H01M10/0525H01M2004/027Y02E60/10
Inventor 袁正勇
Owner NINGBO POLYTECHNIC
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