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Preparation method of single crystal titanium dioxide thin film and evaporation rack for preparation

A titanium dioxide and thin film technology, applied in the field of inorganic nanomaterial preparation, can solve problems such as poor adhesion, easy falling off of single crystal thin films, etc., and achieve the effects of being beneficial to industrial production, beneficial to biological utilization, and reducing costs.

Active Publication Date: 2020-09-18
SHENZHEN INST OF ADVANCED TECH CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The invention patent of CN 101949054A "A Preparation Method of Single Crystal Anatase Titanium Dioxide Film" directly adopts the hydrothermal reaction of metal titanium plate in hydrofluoric acid aqueous solution to form single crystal anatase titanium dioxide film. This method is simple and easy, but the titanium surface forms The single crystal thin film is easy to fall off after ultrasonic treatment, and the adhesion is poor

Method used

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  • Preparation method of single crystal titanium dioxide thin film and evaporation rack for preparation
  • Preparation method of single crystal titanium dioxide thin film and evaporation rack for preparation
  • Preparation method of single crystal titanium dioxide thin film and evaporation rack for preparation

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preparation example Construction

[0029] The preparation method of the monocrystalline titanium dioxide thin film that the present invention adopts can comprise:

[0030] (1) pickling

[0031] First, the titanium-based metal is cleaned with pickling solution;

[0032] Here, the titanium-based metal may include titanium metal or an alloy of titanium and other metals. For example, a round titanium alloy with a diameter of 15 mm and a height of 1 mm may be subjected to surface pickling pretreatment. Specifically, the titanium-based metal may be cleaned for 0.5-5 minutes.

[0033] The pickling solution can be HF and HNO 3 mixed solution. More specifically, the pickling solution can be 66.7% pure water by volume fraction, 20% HF (mass fraction 48%) and 13.3% HNO 3 (mass fraction 48%) solutions are mixed, then diluted 5-30 times, more preferably diluted 10-15 times to obtain pickling solution. After the titanium-based metal, such as titanium alloy, is cleaned by the pickling solution for 30 seconds, it can be c...

Embodiment 1

[0044] First, measure 20ml of pure water, 6ml of 48% HF and 4ml of 48% HNO 3 , Diluted 15 times after mixing to prepare pickling solution. Take an appropriate amount of pickling solution and put it into a beaker, put the titanium alloy into it and wash it for 30 seconds, then discard the obtained light yellow-green liquid, and ultrasonically clean it three times with ultrapure water. In the second step, 120 μL of HF acid with a mass concentration of 48% and 60 mL of pure water were placed in a 100 mL polytetrafluoroethylene evaporating kettle, and a custom-made polytetrafluoroethylene evaporation rack was placed in the dilute acid solution; the cleaned titanium Put the alloy on the tray of the polytetrafluoroethylene evaporation rack, add 5mL of pure water to immerse the titanium alloy, and carry out the dilute acid wet steaming treatment at 180°C for 0.5 hours (180°C / 0.5h). After the treatment, it was ultrasonically cleaned with ultrapure water for 10 minutes, and then dried...

Embodiment 2

[0046] The titanium alloy was pre-cleaned and acid steamed by the method in Example 1, except that dilute acid wet steaming (180° C. / 1 h) was performed. figure 2 B is the topography of the titanium dioxide film formed on the surface of the titanium alloy treated at 180℃ / 1h. It can be seen from the figure that the treated topography and figure 2 A is different, forming nanoparticles with very small crystal faces.

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Abstract

The invention discloses a preparation method of a monocrystal titanium dioxide thin film, wherein the preparation method includes the steps: cleaning a titanium-based metal with a pickling solution for 0.5-5 min; placing the pickled titanium-based metal on an evaporation rack, adding a morphology guide liquid to immerse the titanium-based metal, placing the evaporation rack in an evaporation kettle loaded with an acid evaporation solution, heating to 120-230 DEG C, and carrying out wet evaporation treatment for 0.5-24 hours. The invention also discloses the evaporation rack for preparation ofthe monocrystal titanium dioxide thin film. The preparation method of the monocrystal titanium dioxide thin film does not need a template, has no need of additional addition of a titanium source or asurfactant except the titanium-based metal, has no need of increase of subsequent calcination heat treatment, crystallization or any other treatment, can form titanium oxide monocrystals with controllable morphology and size on the surface of the titanium-based metal matrix in situ; moreover, the bonding force between the prepared monocrystals and the titanium-based metal is strong; In addition, the method adopts precious little acid content, can simplify the post-treatment process, reduces costs, and is environmentally friendly.

Description

technical field [0001] The invention relates to the field of preparation of inorganic nanometer materials. More specifically, it relates to a method for preparing a single crystal titanium dioxide film and an evaporation rack for preparation. Background technique [0002] Titanium dioxide is a polymorphic compound, mainly including three crystal forms: rutile, anatase and brookite. It has good biocompatibility, photoelectric properties and electromagnetic properties, and is widely used in photoelectric thermosensitive functional ceramics, semiconductor sensors and surface coatings of medical metal implants. Bare single-crystal titanium oxide has been extensively studied because of its high surface energy, large specific surface area, and excellent performance. Single crystal titanium oxide with regular morphology is mainly obtained by hydrothermal synthesis, and it is mainly used in researches such as solar cells, photocatalytic degradation of organic pollutants, hydrogen ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C22/54C23C22/34
CPCC23C22/34C23C22/54
Inventor 王国成宋小霞
Owner SHENZHEN INST OF ADVANCED TECH CHINESE ACAD OF SCI