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Method for preparing porous oxide film resistant to weak acid corrosion

A porous oxide and thin film technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, chemical/physical processes, etc., can solve the problem of pore size, distribution and area limitation, template method Expensive preparation cost, easy to damage the porous structure of the film, etc., to achieve the effect of mature preparation equipment, wide application range and excellent performance

Active Publication Date: 2019-04-12
WUYI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the preparation cost of the template method is usually relatively expensive, and the preparation process is complicated, and heat treatment or solvent dissolution is required to remove the template, which is easy to destroy the porous structure of the film, and the size, distribution and area of ​​the pores are limited by the template.

Method used

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  • Method for preparing porous oxide film resistant to weak acid corrosion
  • Method for preparing porous oxide film resistant to weak acid corrosion
  • Method for preparing porous oxide film resistant to weak acid corrosion

Examples

Experimental program
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Effect test

Embodiment 1

[0029] A preparation method of a porous oxide film resistant to weak acid corrosion, comprising the following steps:

[0030] S1), the preparation of precursor solution, the titanium acetate of 0.2g, and the zinc chloride (ZnCl) of 0.04g 2 ), 0.2g of polyethylene glycol (PEG), and 30mL of ethylene glycol were mixed, and stirred at 80°C for 60min using a magnetic stirrer to make titanium acetate, ZnCl 2 and polyethylene glycol are completely dissolved in ethylene glycol to obtain a precursor solution;

[0031] S2), the preparation of the precursor film, put the cleaned substrate on the spin coater and absorb it, use a dropper to drop 6 drops of the precursor solution on the substrate, start the spin coater, first at 400 rpm Rotate at a speed of 120s, then rotate at a medium speed of 1200 rpm for 60s, and then rotate at a high speed of 3000 rpm for 120s; then use a hot plate to dry at 150°C and then spin-coat again, and spin-coat repeatedly 20 times. Thereby obtaining the prec...

Embodiment 2

[0035] A preparation method of a porous oxide film resistant to weak acid corrosion, comprising the following steps:

[0036] S1), the preparation of precursor solution, the tin acetate of 0.4g, and the zinc chloride (ZnCl) of 0.08g 2 ), 0.2g of polyethylene glycol (PEG, molecular weight 2000-6000), and 30mL of ethylene glycol were mixed, and stirred at 80°C for 60min using a magnetic stirrer to make tin acetate, ZnCl 2 and polyethylene glycol are completely dissolved in ethylene glycol to obtain a precursor solution;

[0037] S2), the preparation of the precursor film, put the cleaned substrate on the spin coater and absorb it, use a dropper to drop 6 drops of the precursor solution on the substrate, start the spin coater, first at 500 rpm Rotate at a high speed for 60s, then rotate at a medium speed of 1300 rpm for 60s, and then rotate at a high speed of 3500 rpm for 120s; then use a hot plate to dry at 150°C and then spin-coat again, and repeat the spin-coating 25 times. ...

Embodiment 3

[0041] Performance Analysis of Porous Oxide Thin Film Resistant to Weak Acid Corrosion

[0042] figure 1 It is the porous TiO after high temperature sintering prepared in Example 1 2 High-magnification SEM picture of the film; it can be clearly observed from the picture that there are some holes on the surface of the film, and some raised ZnO nanocolumns are distributed with a diameter of 70-120nm.

[0043] figure 2 It is the weak acid corrosion resistant porous TiO prepared in Example 1 of the present invention 2 High-magnification SEM image of the film, after etching, the pores of the film increase significantly; image 3 It is the weak acid corrosion resistant porous TiO prepared in Example 1 2 Absorption spectrum of photocatalytic degradation of methylene blue by thin film, after weak acid corrosion resistant porous TiO 2 After 2 hours of catalytic degradation of the film, the absorption value of methylene blue decreased rapidly from 1.70 to 0.69, which proves that the...

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Abstract

The invention relates to the technical field of thin films, in particular to a method for preparing a porous oxide film resistant to weak acid corrosion. According to the invention, an acetate is taken as a raw material, zinc chloride and polyethylene glycol are taken as pore-forming agents, and ethylene glycol is taken as a solvent, high-temperature sintering is carried out, and etching is carried out for pore forming by an weak acid, so that finally the porous oxide film resistant to weak acid corrosion is obtained. A preparation device of the method of the invention is mature, the process is simple, and the preparation cost is low. In the sintering process, the acetate is decomposed into a weak-acid-resistant metal oxide, water and carbon dioxide, ZnCl2 reacts with the acetate radical or polyethylene glycol for forming ZnO, hydrogen chloride, water and carbon dioxide through decomposition, and the hydrogen chloride, water and carbon dioxide volatilize to cause forming of pores. Dueto the faster rate of ZnCl2, nano columns with a short length are formed. The invention provides a whisker-reinforced porous ZnO film, and the whisker in the film is a single crystal ZnO nano column.The whisker-reinforced porous ZnO film has excellent performance and can be widely used in the fields of gas sensing detectors, photocatalytic degradation and the like.

Description

technical field [0001] The invention relates to the technical field of thin films, in particular to a method for preparing porous oxide thin films resistant to weak acid corrosion. Background technique [0002] ZnO, SnO 2 , Fe 2 o 3 、TiO 2 Oxides are semiconductor materials with excellent physical and chemical properties, and play an important role in electronic information devices, light-emitting devices, photocatalytic degradation, catalytic reactions, solar cells, lithium batteries and other fields. Therefore, oxide semiconductor materials are a research focus and hotspot in the field of materials. [0003] Oxide thin film materials, especially porous oxide thin film materials are an important research direction at present. Especially when the pore size of the porous oxide thin film material reaches the nanometer level, it has outstanding advantages such as large specific surface area, significant quantum effect and local surface enhancement effect, making the porous...

Claims

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Application Information

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IPC IPC(8): C04B35/81C04B35/457C04B35/46C04B35/622C04B35/624C04B38/02B01J23/06
CPCC04B35/457C04B35/46C04B35/62218C04B35/624C04B38/02B01J23/06C04B2235/9692C04B2235/5276B01J35/33H99Z99/00
Inventor 杨为家王诺媛刘艳怡刘俊杰刘铭全何鑫陈梅
Owner WUYI UNIV
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