Preparation method of lithium ion battery negative electrode material hollow porous vanadium pentoxide microspheres

A technology of vanadium pentoxide microspheres and lithium ion batteries, applied in vanadium oxide, battery electrodes, secondary batteries, etc., can solve the problem of reducing the advantages of three-dimensional hollow microsphere structure, poor material cycle stability, and low specific surface area. and other problems, to achieve excellent rate performance and cycle stability, overcome the thin shell thickness or easy collapse, and the effect of high specific surface area

Pending Publication Date: 2021-10-01
CHINA THREE GORGES UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

According to public information, the template-free method usually obtains a relatively smooth hollow microsphere composed of nanoparticles, which has a low specific surface area and poor controllability, which reduces the structural advantages of the three-dimensional hollow microsphere to a certain extent. , poor effect on improving material cycle stability
Obviously, it is still a great challenge to develop a simple, effective and rapid synthetic system or method for the construction of hollow porous vanadium pentoxide microspheres

Method used

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  • Preparation method of lithium ion battery negative electrode material hollow porous vanadium pentoxide microspheres
  • Preparation method of lithium ion battery negative electrode material hollow porous vanadium pentoxide microspheres
  • Preparation method of lithium ion battery negative electrode material hollow porous vanadium pentoxide microspheres

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Embodiment 1

[0029] (1) Add 0.4g of vanadium pentoxide and 1.27g of citric acid into 40 mL of deionized water, stir at 80°C for 0.5h to obtain a 0.11 mol / L vanadyl citrate solution; take 3 mL of vanadyl citrate solution Add it to 30mL of n-propanol and ethylene glycol mixed solvent with a volume ratio of 1:1, stir and mix evenly at room temperature, react in an autoclave at 200°C for 18h, after natural cooling, separate the solid and liquid, and wash with ethanol After drying, a dark green powder is obtained, which is the VO organic ligand precursor.

[0030] (2) The VO organic ligand precursor was heat-treated in air at a heating rate of 4° / min to 400°C for 1 hour. After natural cooling, the product was collected to obtain three-dimensional hollow porous vanadium pentoxide microspheres.

[0031] (3) Preparation of lithium-ion battery electrode pole piece for testing: three-dimensional hollow porous vanadium pentoxide microsphere active material, conductive agent acetylene black and binder...

Embodiment 2

[0039] (1) Add 0.4 g of commercial vanadium pentoxide and 1.27 g of citric acid into 40 mL of deionized water, stir at 80°C for 0.5 h to obtain a 0.11 mol / L vanadyl citrate solution; take 3 mL of vanadyl citrate Add the solution into 30mL of n-propanol and ethylene glycol mixed solvent with a volume ratio of 1:1, stir and mix evenly at room temperature, and react in an autoclave at 200°C for 6h. After natural cooling, solid-liquid separation, ethanol After washing and drying, a dark green powder is obtained, which is the precursor of VO organic ligand.

[0040] (2) The VO organic ligand precursor was heat-treated in air at a heating rate of 4° / min to 400°C for 1 hour. After natural cooling, the product was collected to obtain three-dimensional vanadium pentoxide microspheres.

[0041] (3) Preparation of lithium-ion battery electrode pole pieces for testing: the three-dimensional vanadium pentoxide microsphere active material, conductive agent acetylene black and binder polyvin...

Embodiment 3

[0045] (1) Add 0.4 g of commercial vanadium pentoxide and 1.27 g of citric acid into 40 mL of deionized water, stir at 80°C for 0.5 h to obtain a 0.11 mol / L vanadyl citrate solution; take 3 mL of vanadyl citrate Add the solution into 30mL ethylene glycol solvent, stir and mix evenly at room temperature, react in an autoclave at 200°C for 18 hours, after natural cooling, separate solid-liquid, wash and dry with ethanol, and obtain a dark green powder, which is VO organic ligand precursor.

[0046] (2) The VO organic ligand precursor was heat-treated in air at a heating rate of 4° / min to 400°C for 1 hour. After natural cooling, the product was collected to obtain three-dimensional vanadium pentoxide microspheres.

[0047] (3) The preparation, assembly and electrochemical performance test conditions of the lithium-ion battery electrode pole piece described in Example 1 were adopted.

[0048] Figure 7 Scanning electron microscope (a) and transmission electron microscope (b) ima...

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Abstract

The invention discloses a preparation method of lithium ion battery negative electrode material hollow porous vanadium pentoxide microspheres. A solvothermal and oxidation treatment two-step method is adopted for synthesis, a mixed solution of n-propyl alcohol and ethylene glycol serves as a solvent, vanadyl citrate serves as a solute, a hollow porous VO organic ligand precursor is prepared through a solvothermal method, then the precursor is subjected to low-temperature oxidation heat treatment, and the hollow porous V2O5 microspheres can be synthesized. The three-dimensional structure V2O5 is a secondary hollow porous microsphere formed by disorderly stacking primary nanosheets of 10-20 nm, the diameter of the three-dimensional structure V2O5 is about 1 [mu]m, the shell thickness is about 0.3 [mu]m, the pore diameter is 10-20 nm, and the three-dimensional structure V2O5 has a high specific surface area of about 45-50 m<2>/g. When the lithium ion battery negative electrode material hollow porous V2O5 microspheres are used as a negative electrode of a lithium ion battery, the porous V2O5 nanosheets increase the contact area of an electrolyte and effectively shortens the diffusion transmission path of ions; and meanwhile, the hollow structure provides a buffer space for volume change, so that the hollow porous V2O5 microspheres show relatively good rate capability and cycling stability, and the preparation method of the three-dimensional hollow porous V2O5 microspheres is expanded.

Description

technical field [0001] The invention belongs to the field of preparation and application of metal oxide micro-nano materials with special structure, and specifically relates to a simple preparation method of hollow porous vanadium pentoxide microspheres, which are mainly used in the field of rechargeable secondary batteries, especially lithium-ion battery technology direction. Background technique [0002] Vanadium pentoxide (V 2 o 5 ) has significant advantages such as abundant resources, low price, excellent safety, and easy preparation, and has been widely studied as a deintercalated cathode material for lithium-ion batteries for a long time. However, since the transformation reaction mechanism came out in 2000, V 2 o 5 It is also considered to be a very potential high-energy negative electrode material, mainly due to its ability to combine with multiple lithium ions during discharge, so it has a higher theoretical specific capacity. Although, V 2 o 5 When used as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02H01M4/48H01M10/0525B82Y40/00
CPCC01G31/02B82Y40/00H01M4/48H01M10/0525C01P2004/34C01P2004/03C01P2004/04C01P2002/72C01P2006/40C01P2006/12C01P2006/16Y02E60/10
Inventor 颜波高林陶华超张露露杨学林
Owner CHINA THREE GORGES UNIV
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