Hydrothermal preparation method for nanometer NbO2F powder

A powder and nano technology, applied in the field of preparation of nano NbO2F powder, to achieve the effect of process safety and environmental protection, cost saving and low cost

Active Publication Date: 2015-04-22
PINGHU HAITE ALLOY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the hydrothermal method is used t...

Method used

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  • Hydrothermal preparation method for nanometer NbO2F powder
  • Hydrothermal preparation method for nanometer NbO2F powder
  • Hydrothermal preparation method for nanometer NbO2F powder

Examples

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Embodiment 1

[0024] At room temperature, weigh 0.005 moles of Nb 2 o 5 Powder, the powder is transferred to a volume of 100ml and has a polytetrafluoroethylene-lined reactor; in the fume hood, add 0.25 mole HF (that is, 25 grams of mass percent concentration is 20% hydrofluoric acid solution), then add 3ml of polyvinyl alcohol (PVA-124) solution with a concentration of 2.0g / L, and stir the reaction kettle evenly with a glass rod. Place the reaction kettle in an oven at 180°C for 24 hours of constant temperature reaction, let the reaction kettle cool down to room temperature naturally in the oven, pour the product in the reaction kettle into a plastic beaker, filter and wash 3 times, and finally put the product in the Dry in an oven at 80°C to get Nb 2 o 5 Powder products. Carry out X-ray diffraction analysis (XRD), scanning electron microscope (SEM) and ultraviolet-visible diffuse reflectance absorption spectrum (DRS) test to the product obtained respectively, the result is as follows:...

Embodiment 2

[0030] At room temperature, weigh 0.015 moles of Nb 2 o 5 Powder, the powder is transferred to a volume of 100ml and has a polytetrafluoroethylene-lined reactor; in a fume hood, add 0.375 moles of HF (i.e. 37.5 grams of 20% hydrofluoric acid concentration in the reactor) acid solution), and then add 9ml of polyvinyl alcohol (PVA-124) solution with a concentration of 2.0g / L, stir evenly with a glass rod, and seal the reaction kettle. Put the reaction kettle in an oven at 190°C for 18 hours of constant temperature reaction, let the reaction kettle cool down to room temperature naturally in the oven, pour the product in the reaction kettle into a plastic beaker, filter and wash 3 times, and finally put the product in the Drying in an oven at 60°C to obtain nano-NbO 2F powder products. According to the same photocatalytic experimental method as in Example 1, when the photocatalytic degradation of 20mg / L MO solution was carried out for 50 minutes, the MO decolorization rate reac...

Embodiment 3

[0032] At room temperature, weigh 0.10 moles of Nb 2 o 5 Powder, the powder is transferred to a volume of 100ml and has a polytetrafluoroethylene-lined reactor; in the fume hood, add 4.0 moles (that is, 40 grams of mass percent concentration is 20% hydrofluoric acid solution in the reactor) ), then add 6ml of polyvinyl alcohol (PVA-124) solution with a concentration of 2.0g / L, and stir the reaction kettle evenly with a glass rod. Place the reaction kettle in an oven at 190°C for 12 hours of constant temperature reaction, let the reaction kettle cool down to room temperature naturally in the oven, pour the product in the reaction kettle into a plastic beaker, filter and wash 3 times, and finally put the product in the Drying in an oven at 70°C to obtain nano-NbO 2 F powder products. According to the same photocatalytic experimental method as in Example 1, when the photocatalytic degradation of 20mg / L MO solution was carried out for 50 minutes, the MO decolorization rate reac...

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Abstract

The invention relates to a hydrothermal preparation method for nanometer NbO2F powder and relates to a preparation method for a niobium oxyfluoride nanometer material. According to the hydrothermal preparation method, the hydrothermal technology is used for preparing the nanometer NbO2F powder with the main raw materials of Nb2O5 powder, hydrofluoric acid with the concentration, by mass, of 20% and polyving akohol, wherein the mean grain size of the grains of the nanometer NbO2F powder ranges from 50 nm to 80 nm, the band gap of the nanometer NbO2F powder is 3.35 eV, and the nanometer NbO2F powder has the good photocatalytic activity. The hydrothermal preparation method comprises the two steps of preparing a reaction precursor and preparing nanometer powder under the hydrothermal condition. By means of the hydrothermal preparation method for the nanometer NbO2F powder, the technological cost is low, energy is saved, environmental friendliness is achieved, and industrial production is easy.

Description

technical field [0001] The present invention relates to the preparation of oxyfluoride nanomaterials, in particular to a kind of nanometer NbO 2 The preparation method of F powder. Background technique [0002] NbO 2 F (niobium dioxide monofluoride) is a kind of oxyfluoride series, as documented in Journal of Power Sources, 2006, 162: 1312-1321, Journal of Solid State Chemistry, 2002, 166: 73-80 and Journal of Physical Chemistry As reported by B, 2005, 109:13420-13423, NbO 2 F is a semiconductor material, which has broad application prospects in the fields of battery materials and photocatalysis. [0003] Currently, the preparation of NbO 2 The method of F is relatively simple, usually using metal niobium (Nb) powder and hydrofluoric acid (HF) as the main raw materials, and is prepared by dissolution-evaporation method. As reported in the literature (Journal of Solid State Chemistry, 2002, 166:73-80), niobium powder was dissolved in 48% hydrofluoric acid, the solution w...

Claims

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Application Information

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IPC IPC(8): C01G33/00B82Y30/00
CPCC01G33/00C01P2002/72C01P2002/84C01P2004/03C01P2004/64C01P2006/90
Inventor 唐培松陈海锋曹枫潘国祥张玉建
Owner PINGHU HAITE ALLOY
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