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Preparation method of spindle niobium oxides
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A niobium oxide and spindle technology, applied in the field of niobium oxide materials, can solve problems such as few reports, and achieve the effects of simple preparation process, low energy consumption and high product purity
Inactive Publication Date: 2014-11-05
SOUTHWEST JIAOTONG UNIV
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Problems solved by technology
The sol-gel method can prepare nano-powders with a particle size of less than 100nm and uniform distribution. At the same time, the sol-gel method is also an effective method for preparing porous materials, but there are still few reports on one-dimensional Nb2O5 nanomaterials.
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Embodiment 1
[0024] 1, a kind of preparation method of spindle niobium oxide, its concrete practice is:
[0025] a. Substrate pre-treatment
[0026] The purchased niobium foil (d=0.2mm) was cut into a size of 10mm*30mm, followed by ultrasonic cleaning in deionized water, alcohol, and acetone solution, and dried in air for later use.
[0027] b. Configure the mixed solution
[0028] In the mixed solution (20ml hydrogen peroxide (30wt%) and 20ml deionized water) container that contains hydrogen peroxide and deionized water, add ammonium fluoride, fully dissolve, and configure a mixed solution, the concentration of ammonium fluoride in the mixed solution It is 0.06684mol / L.
[0029] c. Hydrothermal treatment
[0030] Put the niobium foil in step a obliquely into the autoclave, take 20ml of the solution in step b and move it into the inner tank of the autoclave, leaving a gap of 1 mm in the inner cover to facilitate the volatilization of the solution, then seal the autoclave; The reaction ...
Embodiment 2
[0034] The preparation of spindle body niobium oxide, its specific practice is:
[0035] a. Substrate pre-treatment
[0036] The purchased niobium foil (d=0.2mm) was cut into a size of 10mm*30mm, followed by ultrasonic cleaning in deionized water, alcohol, and acetone solution, and dried in air for later use.
[0037] b. Configure the mixed solution
[0038] In the mixed solution (20ml hydrogen peroxide (30wt%) and 20ml deionized water) container that contains hydrogen peroxide and deionized water, add ammonium fluoride, fully dissolve, and configure a mixed solution, the concentration of ammonium fluoride in the mixed solution It is 0.068mol / L.
[0039] c. Hydrothermal treatment
[0040] Put the niobium foil in step a obliquely into the autoclave, take 20ml of the solution in step b and move it into the inner tank of the autoclave, leaving a gap of 1 mm in the inner cover to facilitate the volatilization of the solution, then seal the autoclave; The reaction kettle was ke...
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Abstract
The invention discloses a preparation method of spindle niobium oxides, which comprises the following specific steps of: carrying out ultrasonic cleaning on a niobium foil sequentially in deionized water, alcohol and an acetone solution, drying the niobium foil in air for later use; in a container filled with a mixed solution of hydrogen peroxide and deionized water, adding and completely dissolving ammonium fluoride so as to obtain a fluorine-containing mixed solution, wherein the concentration of ammonium fluoride in the mixed solution is 0.06684-0.07 mol / L; obliquely putting the niobium foil in a high-pressure reaction kettle, taking 20 parts of the fluorine-containing mixed solution and moving the 20 parts of fluorine-containing mixed solution to a liner of the reaction kettle, carrying out heat preservation on the high-pressure reaction kettle for 15 hours at a temperature of 150 DEG C, cooling the niobium foil to room temperature with the furnace; and taking out a substrate of the niobium foil and spindle niobium oxides growing on the substrate in the high-pressure reaction kettle, washing the substrate for many times by using deionized water, and drying the obtained product so as to obtain a target product. According to the method disclosed by the invention, spindle niobium oxide preparation equipment is simple, and the experiment process is simple and easy to implement.
Description
technical field [0001] The invention relates to the technical field of niobium oxide materials, especially the preparation method of spindle niobium oxide. Background technique [0002] Since Tanabe et al. discovered that niobic acid (Nb2O5·nH2O) had unique catalytic properties, the application of niobium oxides in heterogeneous catalysis has attracted widespread attention. For the dispersed state of niobium oxide (NbOx) species on the surface of supported Nb2O5 catalysts and Some researches on the catalytic performance have been carried out, and due to the difference in the type of support and the loading amount of Nb2O5, the NbOx species have different structural states and properties on the support surface. Wachs et al. believe that the structural state of NbOx species is related to the acidity and alkalinity of the support surface. On the surface of basic oxide supports such as MgO, NbOx exists in the octahedral form of highly distorted oxygen hexa-coordination (NbO6), w...
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