A kind of narrow bandgap black zirconia nanotube thin film and preparation method thereof

A technology of zirconia and nanotubes, which is applied in the field of narrow bandgap black zirconia nanotube films and its preparation, can solve problems such as limitations, and achieve the effects of improving absorption performance, reducing bandgap width, and strong adsorption capacity

Active Publication Date: 2020-05-01
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the energy band structure of titanium oxide, its conduction band position is relatively correct, which limits its application in photodegradation of organic pollutants and photoreduction.
As a wide bandgap semiconductor with stable physical and chemical properties, zirconia has a much more negative conduction band position than titanium oxide, and has great potential for application in the fields of photodegradation and photoreduction, but its absorption of light can only absorb ultraviolet light

Method used

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  • A kind of narrow bandgap black zirconia nanotube thin film and preparation method thereof
  • A kind of narrow bandgap black zirconia nanotube thin film and preparation method thereof
  • A kind of narrow bandgap black zirconia nanotube thin film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1: the preparation of zirconia nanotube film

[0043] (1) Select a zirconium sheet with a diameter of 23 mm to be mechanically polished to a mirror surface as an anodic oxidation raw material;

[0044] (2) Add 0vol% hydrofluoric acid (analytical pure, 40%), 0.35mol / L ammonium fluoride, 1vol% deionized water to glycerol (analytical pure, 99%), stir evenly, as anode Oxidation electrolyte A is stand-by; In glycerol (analytical pure, 99%), add the hydrofluoric acid (analytical pure, 40%) of 0vol%, the ammonium fluoride of 0.35mol / L, 10vol% deionized water, stir Uniform, as the anodic oxidation electrolyte B stand-by.

[0045] (3) A two-electrode system is adopted, the graphite sheet is used as the cathode, and the zirconium sheet is used as the anode, and the anodic oxidation is carried out in the electrolyte solution A and the electrolyte solution B respectively. Constant temperature 25 ℃, supplemented by magnetic stirring electrolyte for anodic oxidation prep...

Embodiment 2

[0048] Embodiment 2: Preparation of narrow bandgap black zirconia nanotube film

[0049] (1) Select a zirconium sheet with a diameter of 23 mm to be mechanically polished to a mirror surface as an anodic oxidation raw material;

[0050] (2) Add 2vol% hydrofluoric acid (analytically pure, 40%) in glycerol (analytical pure, 99%), the ammonium fluoride (solid) of 0.35mol / L, 2.5vol% deionized water, stir Uniform, as anodizing electrolyte.

[0051] (3) A two-electrode system is adopted, graphite sheet is used as cathode, zirconium sheet is used as anode, DC power supply is constant voltage 50V, constant temperature is 25°C, supplemented by magnetic stirring electrolyte for anodic oxidation preparation, and the duration is 2h.

[0052] (4) Rinse the anodized zirconia nanotube film prepared above with deionized water, and dry at 80° C. for 2 hours.

[0053] (5) Heat-treat the dried zirconia nanotube films at 500°C and 800°C respectively in an argon atmosphere for 2 hours, then cool...

Embodiment 3

[0056] (1) The anodized zirconia nanotube films prepared in steps (1)-(4) in Example 2 were heat-treated and kept for 2 hours in an argon atmosphere at 500°C, 600°C, and 800°C respectively, and then Cool down to room temperature with the furnace, and the preparation is completed, and a black zirconia nanotube film with a narrow band gap is obtained.

[0057] (2) Characterized by ultraviolet diffuse reflectance absorption spectrum, the maximum absorption peak of the black zirconia nanotube film annealed at 500°C is around 384nm, the absorption edge is around 568nm, and the optical band gap is 2.35eV, as Figure 4 As shown; after annealing at 600°C, the maximum absorption peak of the black zirconia nanotube film is around 325nm, the absorption edge is around 525nm, and the optical band gap is 2.9eV; after annealing at 800°C, the maximum absorption peak of the black zirconia nanotube film is around 436nm, It has absorption in the whole visible light range, and the optical band ga...

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Abstract

The invention discloses a low energy gap black zirconia nanotube thin film and a preparation method thereof. The width of the optical energy gap of the black zirconia nano tube thin film ranges from 1.0-3.0eV. The preparation method comprises the following steps that (1) an inert electrode is taken as a cathode, the polished zirconia sheet is taken as an anode, and anodic oxidation is carried outin fluorine-containing electrolyte to prepare a zirconium oxide nanotube film; and (2) the zirconium oxide nanotube thin film is cleaned and dried, the zirconium oxide nanotube thin film is subjectedto a protective atmosphere or a vacuum atmosphere, and the heat treatment is carried out at the temperature of 500-800 DEG C to obtain the low energy gap black zirconia nanotube thin film. According to the preparation method, the zirconia nanotube thin film with the low energy gap width and the black appearance is obtained for the first time, the low temperature can be prepared by a simple and convenient method, the cost is low, and the method is suitable for large-scale production.

Description

technical field [0001] The invention relates to a narrow band gap black zirconia nanotube film and a preparation method thereof. Background technique [0002] The increasingly prominent problem of energy shortage has made new energy materials a research hotspot in various countries. Solar energy has undoubtedly become the focus of new energy research due to its renewability; at the same time, with the rapid development of chemical, pharmaceutical and other industries, the solution to environmental problems A breakthrough is also urgently needed, and efficient and pollution-free photocatalytic technology has attracted much attention. However, the fundamental reason for limiting the application of solar energy or photocatalytic technology is that there are various problems in existing materials that make the utilization of sunlight not high. The light absorption ability mainly depends on the energy band structure and surface state of the material. Usually, reducing the band g...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D11/26B82Y40/00
CPCB82Y40/00C25D11/26
Inventor 周灵平陈庆伶杨武霖朱家俊符立才李德意
Owner HUNAN UNIV
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