CN103132064B - Method for preparing titanium dioxide film on surface of low-melting-point substrate through utilizing laser - Google Patents

Method for preparing titanium dioxide film on surface of low-melting-point substrate through utilizing laser Download PDF

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CN103132064B
CN103132064B CN201310064638.7A CN201310064638A CN103132064B CN 103132064 B CN103132064 B CN 103132064B CN 201310064638 A CN201310064638 A CN 201310064638A CN 103132064 B CN103132064 B CN 103132064B
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substrate
titanium dioxide
film
laser
coated
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CN103132064A (en
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刘富荣
韩欣欣
陈继民
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Beijing University of Technology
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Beijing University of Technology
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Abstract

The invention discloses a method for preparing a titanium dioxide film on the surface of a low-melting-point substrate through utilizing laser. The method comprises the following steps: adding water to 15-20nm titanium dioxide nanopowder to prepare a sol; cleaning the substrate, and coating the cleaned substrate with the prepared titanium dioxide sol; putting the substrate on a platform in a mode that the surface of the substrate coated with titanium dioxide is downward; adjusting the experiment platform to make a 1064nm laser spot focus on a sheet; coating titanium dioxide on the substrate through adjusting the parameters comprising the scanning speed, the scanning interval, the scanning power and the like of the laser; and cleaning the film with ethanol and water, and drying to obtain a clean sheet having the titanium dioxide film. The method which allows the titanium dioxide film to be prepared on the low-melting-point substrate has a good application prospect.

Description

Laser is utilized to prepare the method for titanium deoxid film at the substrate surface of low melting point
Technical field:
The present invention relates to Material Field, be specially field of nanometer material technology, especially a kind of preparation method of titanium deoxid film.
Background technology:
Titanic oxide material relies on the physical and chemical performance of its uniqueness to receive the extensive concern of people.Well-known titanium dioxide has photocatalytic, and energy decomposing organic matter, has antibacterial anti-pollution function; Secondly, titanium dioxide has Superhydrophilic, utilizes this character can produce antifog, automatically cleaning product.These two kinds of phenomenons can occur on titanium deoxid film simultaneously.Therefore industrially, the preparation of titanium deoxid film has extremely important status.
Traditional preparation TiO 2the method of film has chemical vapour deposition (CVD) method, reactive sputtering, liquid phase deposition, electrochemical process, sol-gel method, ion self-assembling technique, spray heating decomposition etc.Traditional method utilizing laser to prepare titanium deoxid film is generally Laser vaporization.According to the related data display of consulting, this prepares the method for titanium deoxid film, is generally take titanium dioxide as target, with silicon chip or glass for substrate, utilizes Laser vaporization to prepare titanium deoxid film.The above-mentioned method preparing titanium deoxid film all needs to carry out under the high temperature conditions, so the substrate prepared needed for film is all generally the material that the fusing point such as glass, metal is higher.And no matter be as photocatalyst or as hydrophilic film now, the material of low melting point has very important application, such as the preparation of flexible solar battery.Prepare titanium deoxid film for the low-melting material such as PET, PMMA do substrate, the method that traditional high temperature prepares film is no longer applicable.
The method that the substrates at low temperatures of present low melting point prepares titanium deoxid film mainly contains: low-temperature sintering method, hydrothermal method, pressurization, uv light irradiation method, microwave method etc.In low-temperature growth thin-film process, in order to obtain flawless and the film with good adhesion, generally in titanic oxide nano powder, add a large amount of organism, the titanium deoxid film purity of preparation is not high like this, and performance also receives certain impact.
Summary of the invention:
The object of the present invention is to provide a kind of laser in the substrate of low melting point, plate the method for titanium deoxid film.The method is compared with other methods preparing titanium deoxid film, and equipment is simple, and easy to operate, undope in preparation process organic impurity, and can on the material that fusing point is lower plated film.Material absorbs few to 1064nm optical-fiber laser, so when laser radiation is in substrate, major part can directly be passed.Arrival is coated on the TiO 2 sol in substrate lower surface, and TiO 2 sol absorbing laser energy, reacts, and occurs bonding each other, and is attached in substrate, thus forms titanium deoxid film.
The object of the invention is reached by following measure, and its concrete technology flow process is:
(1) choose the substrate that transmitance is greater than 85 percent, and require that its fusing point is between 120 to 265 degree, cleans with ultrasonic washing instrument and dries up, guaranteeing that substrate surface does not have dust;
(2) in nano titanium dioxide powder, instill water, make colloidal sol, and it is coated in substrate;
(3) substrate obtained in (2) is placed on experiment porch, makes scribble titanium dioxide one to face down.Open laser apparatus regulation experiment podium level, make the focus of laser beam drop on substrate surface, wherein laser apparatus is the optical fiber laser of 1064nm;
(4) shape needing to prepare titanium deoxid film in substrate is drawn out, and to debug laser frequency be 20HZ, sweep velocity is between 750-1000mm/s, and scanning interval is between 0.003-0.007mm, scan power, between 3-4 watt, prepares titanium deoxid film.
(5) recycle ultrasonic washing instrument unnecessary colloidal sol is washed, obtain the clean substrate being coated with titanium deoxid film.
Described base material can be the conductive substrates that surface is coated with ITO conductive film.
In described colloidal sol, the mass ratio of titania powder and water is between 1: 1 and 1: 2.
The particle diameter of described titania powder is between 15-20nm.
Substrate transmitance is greater than 85 percent, refers to the laserable material transmitance for the laser apparatus adopted.
Feature of the present invention:
1. equipment is simple, easy to operate, changes the feature that original laser splash plated film is high to equipment requirements.
2. the base material of plated film is the material of low melting point.Because material melting point is low, traditional film coating method is no longer applicable.Utilize present method can prepare titanium deoxid film in the substrate of low melting point.
3. do not add any organic impurity in titanic oxide nano during plated film.
Accompanying drawing illustrates:
Fig. 1: the device schematic diagram preparing titanium deoxid film.
Fig. 2: the structural representation preparing titanium deoxid film.
Fig. 3: the optical microscope photograph preparing titanium deoxid film.
Embodiment:
First be necessary to herein means out be the present embodiment only for being further elaborated to the present invention, can not limiting the scope of the invention be interpreted as.
Processing units is connected according to the processing unit (plant) schematic diagram shown in Fig. 1.Computer data connecting line connects in laser apparatus; PET material to be processed is directly acted on by laser apparatus Emission Lasers.
Example 1
(1) in beaker, adding dehydrated alcohol, is 0 by thickness.The PET of 18 millimeters puts into beaker, all immerses in ethanol.Clean 20 minutes with ultrasonic washing instrument, and dried up; In another beaker, adding clear water, putting into cleaning the PET gone over, recycling ultrasonic washing instrument cleans 20 minutes, then dries up, and guarantees that pet sheet face does not have dust;
(2) crucible is put at the titania powder of 15nm-20nm in 1 gram particle footpath, utilize dropper to instill 1 ml water, utilize stirring rod to stir, make colloidal sol, and this colloidal sol is coated on PET;
(3) PET obtained in (2) is placed on experiment porch, makes scribble titanium dioxide one to face down.Open laser apparatus adjustment three-dimensional experiment platform, make the focus of laser beam drop on PET lower surface;
(4) draw out the square needing to prepare the shape 1cm*1cm of titanium deoxid film on PET, and be adjusted to the centre of PET thin slice.Then adjusting laser scanning speed is 1000mm/s, and scanning interval is 0.003mm, scan power 4W, and sweep rate is 20HZ.Finally prepare titanium deoxid film.
(5) PET being coated with film is put into dehydrated alcohol, utilize ultrasonic washing instrument to carry out cleaning 30 minutes, unnecessary colloidal sol is removed, obtain the clean PET being coated with titanium deoxid film.Again above-mentioned film is put into water, utilize ultrasonic washing instrument to clean 30 minutes, then dry up, obtain clean titanium deoxid film.
Example 2
(1) in beaker, adding dehydrated alcohol, is that the conducting PET film (surface is coated with ito thin film) of 0.18 puts into beaker by thickness, makes it all immerse in ethanol.Clean 20 minutes with ultrasonic washing instrument, and dry up; In another beaker, adding clear water, putting into cleaning the PET gone over, recycling ultrasonic washing instrument cleans 20 minutes, then dries up, and guarantees that pet sheet face does not have dust;
(2) titanic oxide nano powder being 15nm-20nm by 1 gram particle footpath puts into crucible, utilizes dropper to instill 2 ml waters, utilizes stirring rod to stir, make colloidal sol, and be coated on the conducting surface of PET by this colloidal sol;
(3) PET obtained in (2) is placed on experiment porch, makes scribble titanium dioxide one to face down.Open laser apparatus adjustment three-dimensional experiment platform, make the focus of laser beam drop on PET lower surface;
(4) draw out the square needing to prepare the shape 1cm*1cm of titanium deoxid film on PET, and be adjusted to the centre of PET thin slice.Then adjusting laser scanning speed is 750mm/s, and scanning interval is 0.007mm, scan power 3W, and sweep rate is 20HZ.Finally prepare titanium deoxid film.
(5) PET having plated film is put into dehydrated alcohol, utilize ultrasonic washing instrument to carry out cleaning 30 minutes, unnecessary colloidal sol is removed.Again above-mentioned film is put into distilled water, utilize ultrasonic washing instrument to clean 30 minutes, then dry up, obtain clean titanium deoxid film.

Claims (4)

1. utilize laser to prepare a method for titanium deoxid film at the substrate surface of low melting point, it is characterized in that, its step comprises:
(1) choose the substrate that transmitance is greater than 85 percent, and require that its fusing point is between 120 to 265 degree, cleans with ultrasonic washing instrument and dries up, guaranteeing that substrate surface does not have dust;
(2) in nano titanium dioxide powder, instill water, make colloidal sol, and it is coated in substrate;
(3) substrate being coated with colloidal sol is placed on experiment porch, makes scribble titanium dioxide one to face down; Open laser apparatus regulation experiment podium level, make the focus of laser beam drop on substrate surface, wherein laser apparatus is the optical fiber laser of 1064nm;
(4) shape needing to prepare titanium deoxid film in substrate is drawn out, and to debug laser frequency be 20HZ, sweep velocity is between 750-1000mm/s, and scanning interval is between 0.003-0.007mm, scan power, between 3-4 watt, prepares titanium deoxid film;
(5) recycle ultrasonic washing instrument unnecessary colloidal sol is washed, obtain the clean substrate being coated with titanium deoxid film.
2. according to the method for claim 1, it is characterized in that, base material is the conductive substrates that surface is coated with ITO conductive film.
3. according to the method for claim 1, it is characterized in that, in colloidal sol, the mass ratio of titania powder and water is between 1: 1 and 1: 2.
4. according to the method for claim 1, it is characterized in that, the particle diameter of titania powder is between 15-20nm.
CN201310064638.7A 2013-02-28 2013-02-28 Method for preparing titanium dioxide film on surface of low-melting-point substrate through utilizing laser Expired - Fee Related CN103132064B (en)

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Citations (2)

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Publication number Priority date Publication date Assignee Title
CN101391210A (en) * 2008-10-21 2009-03-25 东华大学 Preparation method of laser modified titanium dioxide photocatalyst
CN102701740A (en) * 2012-05-04 2012-10-03 北京工业大学 Method for preparing potassium sodium niobate functional ceramic film on glass base surface by using laser

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101391210A (en) * 2008-10-21 2009-03-25 东华大学 Preparation method of laser modified titanium dioxide photocatalyst
CN102701740A (en) * 2012-05-04 2012-10-03 北京工业大学 Method for preparing potassium sodium niobate functional ceramic film on glass base surface by using laser

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