Preparation method of ultra-fine Beta-FeOOH nanorod self-assembly hollow microspheres under urea action

A nanorod and self-assembly technology, applied in the field of electrochemistry, can solve the problems of large product particle size, long time-consuming, shortened reaction time, etc., and achieve the effect of simple experimental method, easy implementation, and low cost

Active Publication Date: 2019-03-01
SHAANXI UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Xu Junge et al. (Chemical Journal of Chinese Universities, 2015, 1, 45-54) used ferrous sulfate, urea and ethanol as raw materials to prepare FeOOH nanomaterials with a three-dimensional flower-like structure by a low-temperature and atmospheric-pressure one-step reflux method; Ou Equal (Materials Letters, 2008, 62, 914-917) synthesized large-scale FeOOH nanowires with uniform diameter and high aspect ratio at 100°C by hydrothermal method, but both have hydrothermal reactions and take a long time , and the shortcomings of the large particle size of the prepared product can further shorten the reaction time, reduce the cost, reduce the product particle size, increase the specific surface area and provide more active sites, and increase the application potential of FeOOH in the field of electrochemistry

Method used

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  • Preparation method of ultra-fine Beta-FeOOH nanorod self-assembly hollow microspheres under urea action
  • Preparation method of ultra-fine Beta-FeOOH nanorod self-assembly hollow microspheres under urea action
  • Preparation method of ultra-fine Beta-FeOOH nanorod self-assembly hollow microspheres under urea action

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Experimental program
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Effect test

Embodiment 1

[0025] 1) Add analytically pure soluble iron salts ferric chloride, sodium chloride and urea to 10mL of absolute ethanol and 40mL of deionized water, stir well to dissolve the salt, wherein the concentration of iron salt is 0.05mol / L, sodium salt The concentration is 2 / 3 of the iron salt concentration, the urea concentration is 1 / 1 of the iron salt concentration, and then the mixed solution is dispersed by an ultrasonic generator to obtain a suspension A;

[0026] 2) Pour the suspension A prepared above into the polytetrafluoroethylene lining of the homogeneous hydrothermal reactor, the filling degree is 30%, then seal the reactor, and then put it into the homogeneous hydrothermal reactor Carry out hydrothermal reaction at 50°C for 5 hours, and naturally cool to room temperature after the reaction to obtain product B;

[0027] 3) The product B was washed with water and alcohol for 3 times in a centrifuge, each centrifugation time was 1 min, and the centrifugation speed was 300...

Embodiment 2

[0032] 1) Add analytically pure soluble iron salts ferric chloride, sodium chloride and urea to 25mL of absolute ethanol and 25mL of deionized water, stir well to dissolve the salt, wherein the concentration of iron salt is 0.2mol / L, sodium salt The concentration is 2 / 3 of the iron salt concentration, the urea concentration is 1 / 1 of the iron salt concentration, and then the mixed solution is dispersed by an ultrasonic generator to obtain a suspension A;

[0033] 2) Pour the suspension A prepared above into the polytetrafluoroethylene lining of the homogeneous hydrothermal reactor, the filling degree is 80%, then seal the reactor, and then put it into the homogeneous hydrothermal reactor Carry out hydrothermal reaction at 70°C for 4 hours, and naturally cool to room temperature after the reaction to obtain product B;

[0034] 3) The product B was washed with water and alcohol for 3 times in a centrifuge, each centrifugation time was 4 minutes, and the centrifugation speed was ...

Embodiment 3

[0037] 1) Add analytically pure soluble iron salts ferric chloride, sodium chloride and urea to 30mL of absolute ethanol and 20mL of deionized water, stir well to dissolve the salt, wherein the concentration of iron salt is 0.2mol / L, sodium salt The concentration is 2 / 3 of the iron salt concentration, the urea concentration is 1 / 1 of the iron salt concentration, and then the mixed solution is dispersed by an ultrasonic generator to obtain a suspension A;

[0038] 2) Pour the suspension A prepared above into the polytetrafluoroethylene lining of the homogeneous hydrothermal reactor, the filling degree is 60%, then seal the reactor, and put it into the homogeneous hydrothermal reactor Perform hydrothermal reaction at 150°C for 3 hours, and naturally cool to room temperature after the reaction to obtain product B;

[0039] 3) The product B was washed with water and alcohol for 3 times in a centrifuge, each centrifugation time was 2 minutes, and the centrifugation speed was 5000 r...

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Abstract

The invention discloses a preparation method of ultra-fine Beta-FeOOH nanorod self-assembly hollow microspheres under urea action. The preparation method comprises the following steps: adding solublesalt ferric trichloride, sodium chloride and urea of certain amount into absolute ethyl alcohol and deionized water to obtain suspension A; pouring the suspension A into a homogeneous-phase hydrothermal reaction kettle, and sealing the reaction kettle; putting the reaction kettle in a homogeneous-phase hydrothermal reaction instrument for a hydrothermal reaction; then naturally cooling to room temperature to obtain a product B; washing the product B with water and alcohol respectively, and dispersing the washed product in water to obtain a product C; performing freeze drying on the product C to obtain the ultra-fine Beta-FeOOH nanorod self-assembly hollow microspheres under urea action. Through the homogeneous-phase hydrothermal process, the preparation method disclosed by the invention has the advantages of simplicity, short time, low cost and easiness in implementation; with a larger specific surface area, the ultra-fine Beta-FeOOH nanorod self-assembly hollow microspheres under ureaaction can provide more electrochemical reaction active sites to improve the reaction activity of a Beta-FeOOH conversion reaction.

Description

technical field [0001] The invention relates to the technical field of electrochemistry, in particular to a method for preparing ultrafine β-FeOOH nanorod self-assembled hollow microspheres under the action of urea. Background technique [0002] β-FeOOH is an important component of iron oxides, and has long been considered as a promising anode material for a new generation of Li / Na-ion batteries due to its high capacity (>1000mAh / g), abundant natural resources, non-toxicity, and low cost. promising candidate. At present, there are various methods for preparing iron oxides, which can be divided into liquid-phase method, gas-phase method and solid-phase method according to different preparation raw materials. Due to the advantages of simple equipment, easy access to raw materials, high purity, good uniformity, and accurate chemical composition control, the liquid phase method is more widely used. Liquid-phase methods mainly include hydrolysis, precipitation, hydrothermal,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/52H01M10/052H01M10/054B82Y40/00
CPCB82Y40/00H01M4/52H01M10/052H01M10/054Y02E60/10
Inventor 曹丽云马萌齐慧李嘉胤黄剑锋姚恺陈文卓吴桂娟
Owner SHAANXI UNIV OF SCI & TECH
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