Method for in-situ preparation of PbTiO3 nano-tube array film by using hydrothermal process

A nanotube array and in-situ preparation technology is applied in the field of in-situ preparation of PbTiO3 nanotube array films by hydrothermal method, and can solve the problem that the nanotube array films are not suitable for the preparation of nanotube array films, alkaline mineralizers are unfavorable to grow nanotube array films, etc. problems, to achieve the effect of suitable for large-scale production, controllable conditions, and low energy consumption

Inactive Publication Date: 2008-07-30
TSINGHUA UNIV
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Problems solved by technology

[0004] The traditional hydrothermal synthesis of new materials is carried out in hydrothermal solutions containing alkaline mineralizers. The disadvantages are: (1) the use of alkaline mineralizers is not conducive to the in-situ growth of nanotube array films; (2) The introduction of mineralizers often leads to the introduction of impurities in the hydrothermal system
Therefore, the traditional hydrothermal method is not suitable for the preparation of perovskite-structured nanotube array films that require high purity.

Method used

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  • Method for in-situ preparation of PbTiO3 nano-tube array film by using hydrothermal process

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Embodiment 1

[0027] 1. Polish the titanium foil with 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh SiC sandpaper respectively, and then use 0.05μm Al 2 o 3 Polish to mirror brightness, put the polished titanium foil into acetone and deionized water for 10 minutes and ultrasonically clean it, and dry it for later use;

[0028] 2. Add 12 milliliters of phosphoric acid to 136 milliliters of deionized water, and mix evenly under magnetic stirring to prepare a 1 mol / liter phosphoric acid solution, then add 25 milliliters of hydrofluoric acid to the above phosphoric acid solution, and continue stirring under magnetic force and mix evenly, and be prepared into a water-based electrolyte containing 5% hydrofluoric acid by mass percent;

[0029] 3. At room temperature, put the pretreated titanium foil and platinum sheet into a 5% water-based electrolyte, anodize for 0.5 hours under a constant voltage of 25 volts, and anodize The final titanium foil was washed with deionized water and then ...

Embodiment 2

[0033] 1. Polish the titanium foil with 400 mesh, 600 mesh, 800 mesh, 1000 mesh and 1200 mesh SiC sandpaper respectively, and then use 0.05μm Al 2 o 3 Polish to mirror brightness, put the polished titanium foil into acetone and deionized water for 10 minutes and ultrasonically clean it, and dry it for later use;

[0034] 2. Add 6 milliliters of phosphoric acid to 136 milliliters of deionized water, and mix evenly under magnetic stirring to prepare a 0.5 mol / liter phosphoric acid solution, then add 2.5 milliliters of hydrofluoric acid to the above phosphoric acid solution, and continue stirring under magnetic force and mix evenly, and prepare a water-based electrolyte solution containing 1% hydrofluoric acid by mass.

[0035] 3. At room temperature, put the pretreated titanium foil and platinum sheet into a two-electrode system in a 1% water-based electrolyte, and perform anodic oxidation at a constant voltage of 25 volts for 5 hours, and the anodic oxidation The final titani...

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Abstract

The invention relates to a method of preparing a PbTiO3 nanotube array film in situ by utilizing the hydrothermal method. The method adopts phosphoric acid, hydrofluoric acid, lead acetate and deionized water as raw materials. Firstly, a TiO2 nanotube array film is prepared on the titanium foil sheet through anodic oxidation; and secondly, under the condition that the lead acetate aqueous solution with a molarity of 0.00001 to 10 mol per liter is used as the medium, the TiO2 nanotube array film is adopted as the template, and the hydrothermal reacting solution with a volume percentage of 20 to 90 percent, i.e. the lead acetate aqueous solution is added in and kept constant for 0.5 to 50 hours at a temperature of 150 to 300 DEG C and then the PbTiO3 nanotube array film is finally obtained. The method is fit for manufacturing electronic devices of various types and has a far-ranging application prospect in the industrial fields of piezoelectricity, pyroelectricity and semiconductors.

Description

technical field [0001] The invention relates to a method for nanotube array film, in particular to a method for in-situ preparation of PbTiO by hydrothermal method 3 A method for nanotube array thin films. Background technique [0002] Due to its high dielectric constant and ferroelectricity, lead titanate thin film has great potential for development from the perspective of industrial production and scientific research. It is well known that TiO 2 It is an intermediate in the synthesis of titanate, so TiO is used 2 The nanotube array film is used as a template to prepare a variety of titanium-containing ceramic materials. Ceramic materials with this structure have many potential applications in the fields of microelectronics and biomedicine. [0003] The hydrothermal method refers to the use of aqueous solution as the reaction system in a special closed reactor-autoclave, and creates a relatively high temperature and high pressure reaction environment by heating, pressur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/32C30B29/62C30B7/10
Inventor 王晓慧杨阳李龙土
Owner TSINGHUA UNIV
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