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Method for controllably synthesizing niobium pentoxide microspheres and microflowers without template solvent heat

A technology of niobium pentoxide and microspheres, which is applied in chemical instruments and methods, inorganic chemistry, niobium compounds, etc., can solve the problems of expensive experimental drugs and complex synthetic routes, and achieve simple experimental conditions, wide application prospects, and small size Effect

Inactive Publication Date: 2018-02-27
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The synthesis of niobium pentoxide, the research object, is mostly reported in the literature using hydrothermal / solvothermal synthesis methods, and most of the prepared niobium pentoxide nanorods and microspheres are also prepared by other methods such as oxidation. Niobium pentoxide, this kind of synthetic method requires special experimental equipment, the synthetic route is complicated, and experimental drugs are often expensive

Method used

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  • Method for controllably synthesizing niobium pentoxide microspheres and microflowers without template solvent heat
  • Method for controllably synthesizing niobium pentoxide microspheres and microflowers without template solvent heat
  • Method for controllably synthesizing niobium pentoxide microspheres and microflowers without template solvent heat

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Effect test

example 1

[0029] Add 1.5 mmol of niobium pentachloride and 7.5 mmol of sodium carbonate powder into 30 mL of absolute ethanol, put it in a 100 mL beaker, put it into an ultrasonic instrument for 15 minutes to make it evenly mixed, and then pour it into 50 mL polytetrafluoroethylene Put it in a reaction kettle with vinyl fluoride substrate, seal it, put it in an oven, control the temperature of the oven at 200°C, and react for 12 hours. Wash several times and dry at 80°C for 3 hours to obtain niobium pentoxide microspheres. figure 1 Among them, there are no other miscellaneous peaks, and the positions and relative intensities of each diffraction peak are consistent with the JPCDS card (28-0317), indicating that the product is hexagonal-like niobium pentoxide. From figure 2 It can be seen that the diameter of the microsphere is about 1.2 microns.

example 2

[0031] Add 1.5 mmol of niobium pentachloride and 7.5 mmol of sodium carbonate powder into 30 mL of ethylene glycol, put it in a 100 mL beaker, put it into an ultrasonic instrument for 15 minutes to make it evenly mixed, and then pour it into 50 mL polytetrafluoroethylene Put it in a reaction kettle with vinyl fluoride substrate, seal it, put it in an oven, control the temperature of the oven at 200 °C, and react for 12 hours. After washing several times and drying at 80°C for 3 hours, the niobium pentoxide nanoflowers were obtained. From image 3 It can be seen that the diameter of the nanoflower is about 3.6 microns, composed of nanosheets, and the thickness is about 12 nanometers.

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Abstract

The invention belongs to the technical field of inorganic nanomaterials, and particularly relates to a method for controllably synthesizing niobium pentoxide microspheres and microflowers without template solvent heat. The method comprises the following steps: firstly, mixing a certain amount of niobium inorganic matter ionic salt with a precipitant according to a certain ratio, and respectively dissolving into two different organic solvents; then performing ultrasonic treatment for 15-30 minutes, completely dissolving solid powder and evenly mixing; and finally, respectively transferring thetwo solutions into a reaction kettle with a polytetrafluoroethylene substrate, sealing, putting into a drying oven, controlling the temperature of the drying oven to be 180-200 DEG C, reacting for 8-12 hours, and after the reaction is over, cooling the product to be at room temperature; centrifugally separating the precipitated product, collecting solids, rinsing for multiple times with deionizedwater and absolute ethyl alcohol, and performing vacuum drying, to obtain the niobium pentoxide microspheres and microflowers.

Description

technical field [0001] The invention belongs to the technical field of inorganic nanometer materials, and in particular relates to a method for synthesizing niobium pentoxide microspheres and microflowers without a template and solvothermal controllable. Background technique [0002] Niobium pentoxide is an important n-type wide-bandgap semiconductor material with a bandgap of 3.4 eV at room temperature. It has been widely studied and used in the field of energy storage materials because of its special layered structure. As an energy storage material, niobium pentoxide undergoes an intercalation reaction of ions in the bulk phase. The size of the ionic radius matches the interlayer spacing of niobium pentoxide, which can effectively weaken the stress caused by ion intercalation. In this way, the insertion / extraction of ions does not It will cause the structural change of the niobium pentoxide nanomaterial itself, and when it is used as an energy storage material, it can grea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G33/00
CPCC01G33/00C01P2002/72C01P2004/03C01P2004/04C01P2004/45
Inventor 连加彪李圣远汪婷李华明
Owner JIANGSU UNIV
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