Preparation method of nano flower-like titanium dioxide@bismuth trisulfide electrode material

A technology of bismuth trisulfide and titanium dioxide, applied in titanium dioxide, titanium oxide/hydroxide, chemical instruments and methods, etc., can solve the problems of poor reversibility, reduction, and poor rate performance of electrochemical reactions, and achieve regular morphology Control, reduce volume effect, improve the effect of cycle performance

Inactive Publication Date: 2020-12-04
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, based on Sb 2 S 3 There are some disadvantages in the negative electrode materials, and its inherent low conductivity easily leads to large impedance and poor rate performance; at the same time, the huge volume expansion caused during the transformation and further alloying reactions will inevitably lead to large mechanical Internal stress, resulting in the crushing and aggregation of nanoparticles, metal Sb 0 and Na 2 The active reaction interface between S is greatly reduced, resulting in poor reversibility of electrochemical reactions and low capacity retention for long-term cycling.
At the same time, as a negative electrode material, the intercalation and deintercalation of sodium ions during the charge and discharge process will lead to a change in the volume of the material, resulting in a decrease in its specific capacity (100-200mAhg -1 ), poor cycle stability (0.1Ag -1 The specific capacitance retention rate is less than 60% after 100 cycles at a certain current density)

Method used

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  • Preparation method of nano flower-like titanium dioxide@bismuth trisulfide electrode material
  • Preparation method of nano flower-like titanium dioxide@bismuth trisulfide electrode material
  • Preparation method of nano flower-like titanium dioxide@bismuth trisulfide electrode material

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Experimental program
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Effect test

Embodiment 1

[0026] Dissolve 1 mmol of commercial bismuth chloride in 40 ml of ethylene glycol, and stir ultrasonically for 1 hour until the white particles are completely dissolved; add 2 mmol of thioacetamide, and stir ultrasonically for 1 hour until the particles are completely dissolved; add the above solvent to 100 ml of hydrothermal reaction Kettle, heated at 180°C for 12 hours, and cooled to room temperature; the black hydrothermal reaction product was centrifuged and washed several times (3-4 times), dried in an oven at 60°C for 12 hours, collected for use, and the nano-flower-shaped three Bismuth sulfide; take 0.1 gram of nano-flower-shaped bismuth trisulfide powder (place it in a three-necked flask containing 100 ml of water at 80°C, stir in a water bath for 30 minutes; slowly inject 80 mg of tetrabutyl titanate solution into the above-mentioned three-necked flask ( duration of 5 minutes); after 12 hours in a water bath at 80°C, the gray reaction product was washed by centrifugati...

Embodiment 2

[0028] Dissolve 1 mmol of commercial bismuth chloride in 60 ml of ethylene glycol, and stir ultrasonically for 1 hour until the white particles are completely dissolved; add 3 mmol of thiourea, and stir ultrasonically for 1 hour until the particles are completely dissolved; put the above solvent in a 100 ml hydrothermal reactor, Heat at 200°C for 12 hours, then cool to room temperature; the black hydrothermal reaction product (nano flower-like bismuth trisulfide) is washed by centrifugation for several times (3-4 times), dried in an oven at 60°C for 12 hours, and then collected for use ; Take 0.1 gram of black reaction product (nano flower-like bismuth trisulfide) and place it in a three-necked flask containing 80 milliliters of water at 60° C., stir in a water bath for 30 minutes; slowly inject 100 mg of tetrabutyl titanate solution into the above-mentioned three-necked flask ( duration of 5 minutes); after 24 hours in a water bath at 60°C, the gray reaction product (TiO 2 @B...

Embodiment 3

[0030] Dissolve 1 mmol of commercial bismuth chloride in 40 ml of ethylene glycol, and stir ultrasonically for 1 hour until the white particles are completely dissolved; add 1.5 mmol of sodium sulfide, and stir ultrasonically for 1 hour until the particles are completely dissolved; put the above solvent in a 100 ml hydrothermal reactor , heated at 150°C for 12 hours, and cooled to room temperature; the black hydrothermal reaction product (nano flower-like bismuth trisulfide) was washed by centrifugation for many times (3-4 times), dried in an oven at 60°C for 12 hours, and then collected. Use; take 0.1 g of the black reaction product (nanoflower-like bismuth trisulfide) and place it in a three-necked flask containing 60 ml of water at 70°C, stir in a water bath for 30 minutes; slowly inject 60 mg of tetrabutyl titanate solution into the above-mentioned three-necked flask (duration 5 minutes); after 12 hours in a 70°C water bath, the gray reaction product (TiO 2 @Bi 2 S 3 Nan...

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Abstract

The invention provides a preparation method of a nano flower-like titanium dioxide@bismuth trisulfide electrode material, which comprises the following steps: (1) dissolving bismuth chloride in an ethylene glycol solution, carrying out ultrasonic stirring until the bismuth chloride is dissolved, adding water-soluble sulfide into the ethylene glycol solution of bismuth chloride, transferring the prepared solution into a hydrothermal reaction kettle, carrying out ultrasonic stirring to obtain a mixed solution, reacting for 1-15 hours in a constant-temperature box at the temperature of 60-200 DEGC, cooling, filtering, separating, washing with deionized water, washing with absolute ethyl alcohol, and drying, so as to obtain bismuth trisulfide nanoflowers, and (2) dispersing the prepared bismuth trisulfide powder into deionized water, transferring the solution into a three-neck flask, adding tetrabutyl titanate, carrying out oil bath reaction for 1-24 hours at the temperature of 60-90 DEGC, cooling, carrying out centrifugal separation, washing with deionized water, and drying to obtain the nano flower-shaped titanium dioxide@bismuth trisulfide electrode material. The invention also provides an application of the nano flower-like titanium dioxide@bismuth trisulfide electrode material as a sodium ion battery negative electrode material.

Description

technical field [0001] The invention belongs to the technical field of preparation of electrode materials for sodium-ion batteries, and in particular relates to a method for preparing nano-flower-shaped titanium dioxide@bismuth trisulfide electrode materials and its application in negative electrode materials for sodium-ion batteries. Background technique [0002] Lithium-ion batteries have the advantages of flexible application and long service life, but the shortage of Li resources greatly limits the long-term development and application of lithium-ion batteries. Compared with lithium-ion batteries, sodium-ion batteries have a similar energy storage mechanism, but the relative abundance of sodium in the earth's crust is much greater than that of lithium (2.75% vs 0.0065%). Therefore, sodium-ion batteries, as the best substitute for lithium-ion batteries, have attracted the attention of researchers all over the world. [0003] At present, the anode materials for sodium-ion...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053C01G29/00H01M4/36H01M4/58H01M4/62H01M10/054
CPCC01G23/053C01G29/00C01P2002/72C01P2004/03C01P2004/30C01P2006/40H01M4/366H01M4/5815H01M4/628H01M10/054H01M2004/021H01M2004/027Y02E60/10
Inventor 欧星曹亮夏海峰张佳峰张宝
Owner CENT SOUTH UNIV
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