Preparation method of hollow TiNb2O7 microsphere

A microsphere and hollow technology, applied in chemical instruments and methods, niobium compounds, inorganic chemistry, etc., can solve the problems of not very good cycle performance, unstable structure, capacity fading, etc., to improve cycle performance and rate performance, and prepare Short cycle time, stress relief effect

Active Publication Date: 2017-12-15
FUDAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although they all have excellent electrochemical performance, their cycle performance is not very good
Due to the unstable structure of the electrode material, the volume of the electrode material changes during the charging and discharging process, which leads to serious capacity fading.

Method used

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  • Preparation method of hollow TiNb2O7 microsphere
  • Preparation method of hollow TiNb2O7 microsphere
  • Preparation method of hollow TiNb2O7 microsphere

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Weigh 8.9 g of glucose, measure 70 ml of deionized water, pour them into 100 ml beakers, and magnetically stir for 0.5 h to obtain a clear glucose solution; pour the glucose solution into a 100 ml hydrothermal reaction kettle, and Insulate at 140°C for 8 h; after cooling to room temperature, they were alternately centrifuged twice with absolute ethanol and deionized water, respectively, and placed in an oven at 70°C for 9 h to obtain carbon spheres. Weigh 0.4 g of carbon sphere powder, measure 20 ml of absolute ethanol, pour them into 50 ml beakers, place them in an ultrasonic cleaner, and perform ultrasonic dispersion for 1.5 h to obtain a uniformly dispersed suspension of carbon spheres; weigh 0.52g of niobium pentachloride, 0.28g of titanium isopropoxide, and pour them into the suspension of carbon spheres, and magnetically stir at room temperature for 2 h; finally, pour the uniformly mixed suspension into 50 ml of In the reaction kettle, it was kept at 160 °C for 24...

Embodiment 2

[0025] Weigh 9.0 g of glucose, measure 80 ml of deionized water, pour them into 100 ml beakers, and magnetically stir for 1 h to obtain a clear glucose solution; pour the glucose solution into a 100 ml hydrothermal reaction kettle, and Insulate at 150 °C for 10 h; after cooling to room temperature, they were washed by alternating centrifugation with absolute ethanol and deionized water for 3 times, and placed in an oven at 80 °C for 10 h to obtain carbon spheres. Weigh 0.5 g of carbon sphere powder, measure 22 ml of absolute ethanol, pour them into 50 ml beakers, place them in an ultrasonic cleaner, and carry out ultrasonic dispersion for 2 h to obtain a uniformly dispersed suspension of carbon spheres; 0.54 g of niobium pentachloride, 0.30 g of titanium isopropoxide, and pour them into the suspension of carbon spheres, and magnetically stir at room temperature for 3 h; finally, pour the uniform suspension into 50 ml of In the reaction kettle, it was kept at 170 °C for 22 h, a...

Embodiment 3

[0027] Weigh 9.1 g of glucose, measure 90 ml of deionized water, pour them into 100 ml beakers, and magnetically stir for 1.5 h to obtain a clear glucose solution; pour the glucose solution into a 100 ml hydrothermal reaction kettle, and Insulate at 160 °C for 12 h; after cooling to room temperature, they were washed by alternating centrifugation with absolute ethanol and deionized water for 4 times, and placed in an oven at 90 °C for 12 h to obtain carbon spheres. Weigh 0.6 g of carbon sphere powder, measure 24 ml of absolute ethanol, pour them into 50 ml beakers, place them in an ultrasonic cleaner, and carry out ultrasonic dispersion for 25 h to obtain a uniformly dispersed suspension of carbon spheres; 0.56g niobium pentachloride, 0.32 g titanium isopropoxide, and pour them into the suspension of carbon spheres, stir magnetically at room temperature for 2 h; pour the uniformly mixed suspension into 50 ml of reaction In the still, it was kept at 180 °C for 26 h, and it was ...

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Abstract

Belonging to the technical field of nanomaterial synthesis, the invention specifically relates to a preparation method of a hollow TiNb2O7 microsphere. The method includes: firstly selecting glucose as the carbon source, using deionized water as the solvent, synthesizing uniformly dispersed carbon spheres homogeneous in size by solvothermal method, then taking titanium isopropylate as the titanium source, adopting niobium pentachloride as the niobium source, using ethanol as the solvent, and performing mixing to obtain a uniformly dispersed suspension, and finally using solvothermal method to prepare the hollow TiNb2O7 microsphere with larger specific surface area successfully. Because of high theoretical specific capacity (388 mA h g<-1>), high discharge voltage platform (1.65V) and large specific surface area, the material is expected to become a novel lithium ion battery anode material. In addition, the method has the advantages of simple preparation process, wide raw material sources and low production cost, thus having very broad market application prospects.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial synthesis, in particular to a hollow TiNb 2 o 7 Preparation method of microspheres. Background technique [0002] In recent years, with the rapid development of portable electronic devices and electric vehicles, the demand for high power density and high energy density electrode materials is particularly urgent. Performance plays a decisive role, so it is particularly necessary to develop an anode material with high specific capacity, good cycle performance and excellent rate performance. TiNb 2 o 7 Due to the high theoretical specific capacity (388 mAh g -1 ) 1 , the higher discharge voltage platform (1.65 V) has attracted the attention of researchers 2 , TiNb with various morphologies in recent years 2 o 7 Material is constantly being reported. such as stick 3 , porous nanofibrous 4 , ordered mesoporous 5 , nano pearl string 6 , porous nanotubes 7 , nanoparticles 8 , microsp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/48H01M10/0525C01G33/00
CPCC01G33/00C01P2004/34H01M4/366H01M4/48H01M10/0525H01M2004/021H01M2004/027Y02E60/10
Inventor 车仁超朱国振张捷
Owner FUDAN UNIV
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