CN110747449B - Preparation method of self-cleaning hydrophobic film layer for electronic screen - Google Patents

Preparation method of self-cleaning hydrophobic film layer for electronic screen Download PDF

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CN110747449B
CN110747449B CN201911134545.0A CN201911134545A CN110747449B CN 110747449 B CN110747449 B CN 110747449B CN 201911134545 A CN201911134545 A CN 201911134545A CN 110747449 B CN110747449 B CN 110747449B
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film layer
deposition
purging
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cleaning
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CN110747449A (en
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李杨
吴晓宏
洪杨
卢松涛
康红军
秦伟
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Harbin Institute of Technology
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C23C16/45555—Atomic layer deposition [ALD] applied in non-semiconductor technology

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  • Metallurgy (AREA)
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  • Inorganic Chemistry (AREA)
  • Surface Treatment Of Glass (AREA)
  • Physical Vapour Deposition (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

A self-cleaning hydrophobic film layer for electronic screen and its preparation method belong to self-cleaning hydrophobic film technologyThe field of the technology. The method solves the problems that the existing method for preparing the self-cleaning hydrophobic membrane layer is complex and has high requirements on equipment and process. The invention uses the atomic layer deposition technology to deposit Al on the surface of the glass2O3And TiO2A composite film layer structure. The Al-O-Ti bonds and the Al-O-Ti bonds between the atomic layers can enable the film layers to be tightly combined, so that the problem that the barrier property of the film to water and oxygen is poor due to fine cracks generated by amorphous alumina along with the increase of the thickness of the film is solved, and the problem that the bonding force between the titanium oxide film layer and the substrate is insufficient is also solved. The composite film layer is an ultrathin film integrating high transmittance of a visible light region, high reflectivity of an infrared region and high stability, has good hydrophobic property, has a hydrophobic angle of 130-150 degrees and a transmittance of 90-95 percent, and has a very wide application prospect in the fields of electronic screens and the like.

Description

Preparation method of self-cleaning hydrophobic film layer for electronic screen
Technical Field
The invention relates to a self-cleaning hydrophobic film layer for an electronic screen and a preparation method thereof, belonging to the technical field of hydrophobic self-cleaning films.
Background
The self-cleaning effect of lotus leaves has attracted much interest since the 70 s of the 20 th century. The surface of the lotus leaf can be endowed with super-hydrophobic performance under the combined action of the micron-nanometer microstructure and the low surface energy. In view of the existence of strong water repellent effect of the super-hydrophobic material, common phenomena such as corrosion, icing, oxidation and the like are inhibited on the surface of the super-hydrophobic material, so that the super-hydrophobic material has various unique performances such as pollutant adsorption, corrosion resistance, pollution resistance and the like, has strong self-cleaning function, and has wide application prospect in industry and daily life.
The currently known methods for preparing the hydrophobic self-cleaning film layer mainly comprise a template method, a vapor deposition method, a sol-gel method and the like, but most of the methods have the problems of high requirements on equipment and processes and the like. Therefore, it is necessary to provide a self-cleaning hydrophobic film layer for an electronic screen and a preparation method thereof.
Disclosure of Invention
The invention provides a self-cleaning hydrophobic self-cleaning film layer for an electronic screen and a preparation method thereof, aiming at solving the problems that the existing method for preparing the hydrophobic self-cleaning film layer is complex and has high requirements on equipment and process.
The technical scheme of the invention is as follows:
a self-cleaning hydrophobic film layer for an electronic screen and a preparation method thereof are disclosed, the method comprises the following operation steps:
step 1, cleaning a glass substrate;
step 2, drying the cleaned glass substrate by using nitrogen, then placing the glass substrate into a deposition cavity of an atomic layer deposition instrument, and pumping the deposition cavity to 4 multiplied by 10-3Torr～6×10-3Torr, then introducing carrier gas until the pressure of the chamber is 0.1 Torr-0.2 Torr, and the temperature in the deposition chamber is 150 ℃ to 200 ℃; and then, carrying out atomic layer periodic deposition growth on the surface of the glass substrate to obtain the glass plated with the metal oxide film layer.
Preferably: the thickness of the metal oxide film layer is 30 nm-60 nm.
Preferably: the operation process of cleaning the glass substrate in the step 1 is as follows: sequentially using glass cleaning liquid, deionized water and absolute ethyl alcohol in an ultrasonic cleaning machine, wherein the ultrasonic frequency is 30 KHz-50 KHz, the ultrasonic time is 20 min-30 min, and then immersing the glass cleaning liquid, the deionized water and the absolute ethyl alcohol in the absolute ethyl alcohol for storage for later use.
Most preferably: the glass cleaning solution is neutral coated glass cleaning solution.
Preferably: the specific operation process of the step 2 for carrying out the atomic layer periodic deposition growth of the film layer on the surface of the glass substrate is as follows: 1) injecting a titanium source into a deposition cavity of the atomic layer deposition instrument in a pulse mode for a pulse time t1Is 0.03s to 0.06 s; 2) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t2Is 30s to 60 s; 3) injecting water source into the deposition cavity of the atomic layer deposition instrument in a pulse mode with pulse time t3Is 0.02 s-0.04 s(ii) a 4) Opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t4Is 30s to 60 s; 5) repeating the growth cycles 1) to 4) for 50 to 100 times; 6) injecting an aluminum source into a deposition cavity of the atomic layer deposition instrument in a pulse mode for a pulse time t6Is 0.02s to 0.04 s; 7) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t7Is 30s to 60 s; 8) injecting water source into the deposition cavity of the atomic layer deposition instrument in a pulse mode with pulse time t8Is 0.01s to 0.03 s; 9) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t9Is 30s to 60 s; 10) repeating the growth cycles 6) to 9) for 50-100 times; 11) repeating the growth cycles 1) to 10) for 1to 5 times to obtain the Al-plated film2O3And TiO2Glass with composite film.
The titanium source is titanium tetraisopropoxide, the aluminum source is trimethylaluminum, and the water source is deionized water.
The glass size is a rectangle of 38 x 12 mm.
The invention has the following beneficial effects: the invention uses the atomic layer deposition technology to deposit Al on the surface of the glass2O3And TiO2The composite film layer structure integrates high transmittance of a visible light region, high reflectivity of an infrared region and high stability, has good hydrophobic property, can reach a hydrophobic angle of 130-150 degrees, and has a transmittance of 90-95 percent.
Al in the composite film prepared by the invention2O3And TiO2Al-O-Ti bonds are bonded between atomic layers, and the Al-O-Ti bonds can enable film layers to be tightly bonded and delay Al2O3The hydrolysis process in the electrolyte solution. Solves the problem of single-layer Al2O3Is amorphous, and easily generates fine cracks along with the increase of the thickness of the film, so that the film pair H is formed2O and O2The barrier property of (a) becomes poor, thereby affecting the performance of the film. Also solves the problem that under the ultraviolet illumination, the single-layer TiO2The film layer is excited to generate electron-hole pairs, and the electrons are transferred to the substrate to cause the electric potential to shift towards the negative direction, thereby protectingProtection of the substrate from corrosion, TiO2The film layer and the substrate have the problem of insufficient bonding force. And Al in the composite film prepared by the invention2O3-TiO2The combined effect of the nanostructuring and the low surface energy of (a) can impart hydrophobic properties to the surface. The self-cleaning and anti-pollution composite screen has excellent self-cleaning and anti-pollution performance and has very wide application prospect in the field of electronic screens.
Drawings
FIG. 1 is an XPS spectrum of a self-cleaning hydrophobic membrane layer;
FIG. 2 is an AFM photograph of a self-cleaning hydrophobic membrane layer;
FIG. 3 is a self-cleaning hydrophobic membrane layer contact angle measurement view;
FIG. 4 is a graph showing the transmittance of the self-cleaning hydrophobic film layer.
Detailed Description
The experimental procedures used in the following examples are conventional unless otherwise specified. The materials, reagents, methods and apparatus used, unless otherwise specified, are conventional in the art and are commercially available to those skilled in the art.
Embodiment mode 1: preparation of self-cleaning hydrophobic film layer
Firstly, cleaning a glass substrate: sequentially using glass cleaning liquid, deionized water and absolute ethyl alcohol to respectively perform ultrasonic treatment in an ultrasonic cleaning machine for 20min, and then immersing in new absolute ethyl alcohol for storage for later use.
Secondly, drying the cleaned glass sheet by using nitrogen, then placing the glass sheet into a deposition cavity of an atomic layer deposition instrument, and pumping the deposition cavity to 5 multiplied by 10-3Torr, then a carrier gas is introduced until the pressure in the chamber is 0.15Torr and the temperature in the deposition chamber is 150 ℃. Then, carrying out atomic layer periodic deposition growth of a film layer on the surface of the glass substrate, wherein the specific operation process is as follows: 1) injecting titanium tetraisopropoxide into a deposition cavity of the atomic layer deposition instrument in a pulse mode, wherein the pulse time t is1Is 0.06 s; 2) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t2Is 60 s; 3) injecting water source into the deposition cavity of the atomic layer deposition instrument in a pulse mode with pulse time t3Is 0.02 s; 4) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t4Is 40 s; 5) repeating the growth cycles 1) to 4) for 100 times; 6) injecting trimethyl aluminum into a deposition cavity of the atomic layer deposition instrument in a pulse mode for a pulse time t6Is 0.02 s; 7) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t7Is 30 s; 8) injecting water source into the deposition cavity of the atomic layer deposition instrument in a pulse mode with pulse time t80.015 s; 9) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t9Is 30 s; 10) repeating the growth cycles 6) to 9) for 100 times; 11) repeating the growth cycles 1) to 10) for 3 times to obtain Al-plated film2O3And TiO2The glass of the composite film layer was designated as sample (i).
The thickness of the composite film layer of sample (i) was measured to be 50nm using an ellipsometer.
Comparative example 1: al (Al)2O3Preparation of the film layer
Firstly, cleaning a glass substrate: sequentially using glass cleaning liquid, deionized water and absolute ethyl alcohol to respectively perform ultrasonic treatment in an ultrasonic cleaning machine for 20min, and then immersing in new absolute ethyl alcohol for storage for later use.
Secondly, drying the cleaned glass sheet by using nitrogen, then placing the glass sheet into a deposition cavity of an atomic layer deposition instrument, and pumping the deposition cavity to 5 multiplied by 10-3Torr, then a carrier gas is introduced until the pressure in the chamber is 0.15Torr and the temperature in the deposition chamber is 150 ℃. Then, carrying out atomic layer periodic deposition growth of a film layer on the surface of the glass substrate, wherein the specific operation process is as follows: 1) injecting trimethyl aluminum into a deposition cavity of the atomic layer deposition instrument in a pulse mode for a pulse time t1Is 0.02 s; 2) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t2Is 30 s; 3) injecting water source into the deposition cavity of the atomic layer deposition instrument in a pulse mode with pulse time t30.015 s; 4) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t4Is 30 s; 5) repeating the growth cycles 1) to 4) for 100 times; 11) repeating the growth cycles 1) to 5) for 3 times to obtain Al-plated film2O3The glass of the film layer was designated as sample (ii).
Comparative example 2: TiO 22Preparation of the film layer
Firstly, cleaning a glass substrate: sequentially using glass cleaning liquid, deionized water and absolute ethyl alcohol to respectively perform ultrasonic treatment in an ultrasonic cleaning machine for 20min, and then immersing in new absolute ethyl alcohol for storage for later use.
Secondly, drying the cleaned glass sheet by using nitrogen, then placing the glass sheet into a deposition cavity of an atomic layer deposition instrument, and pumping the deposition cavity to 5 multiplied by 10-3Torr, then a carrier gas is introduced until the pressure in the chamber is 0.15Torr and the temperature in the deposition chamber is 150 ℃. Then, carrying out atomic layer periodic deposition growth of a film layer on the surface of the glass substrate, wherein the specific operation process is as follows: 1) injecting titanium tetraisopropoxide into a deposition cavity of the atomic layer deposition instrument in a pulse mode, wherein the pulse time t is1Is 0.06 s; 2) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t2Is 60 s; 3) injecting water source into the deposition cavity of the atomic layer deposition instrument in a pulse mode with pulse time t3Is 0.02 s; 4) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t4Is 40 s; 5) repeating the growth cycles 1) to 4) for 100 times; 6) repeating the growth cycles 1) to 5) for 3 times to obtain the TiO-coated film2The glass of the film layer was designated sample (iii).
The results of the x-ray photoelectron tests performed on the samples (i), (ii), and (iii) are shown in FIG. 1, in which FIG. 1 (a) is an Al spectrum contrast chart and FIG. 1 (b) is a Ti spectrum contrast chart. As can be seen from FIG. 1, Al2O3Film layer and TiO2The core energy level peaks of the film layer are respectively 75.2eV (Al 2p), 461.7eV (Ti 2p 1/2) and 456.0eV (Ti 2p2/3) in Al2O3/TiO2In the XPS plot of the composite film, the Al 2p level peak was shifted to lower binding energies (74.5eV) and the Ti 2p level peak was shifted to higher binding energies relative to the above reference peaks (462.0 eV for Ti 2p 1/2 and 456.3eV for Ti 2p 3/2). The electronegativity of Al (1.61) and Ti (1.54) suggests that Al and Ti tend to attract and donate electrons, respectively. From this, it is understood that the shift of the core levels of Al and Ti is caused by Al2O3And TiO2The Al-O-Ti bonding process between atomic layers. The Al-O-Ti bond can make the film layer tightly combined and delay Al2O3The hydrolysis process in the electrolyte solution.
The atomic force microscopy test was performed on sample (i) and the results are shown in FIG. 2. As can be seen from FIG. 2, Al produced by atomic layer deposition according to the present invention2O3-TiO2The micro-morphology of the composite film is in a nano island shape, the whole film is compact and uniform, the surface roughness is large, and the root mean square roughness is calculated to be 5.73 nm. Al (Al)2O3-TiO2The combined action of the nano microstructure of the composite film and the low surface energy can endow the surface with hydrophobic property. The self-cleaning and pollution-resistant composite material has excellent self-cleaning and pollution-resistant performances, and has extremely wide application prospects in the fields of aerospace and the like.
Al test with contact Angle for sample (i) and glass substrate2O3-TiO2The hydrophobicity of the composite film is shown in fig. 3, where (1) in fig. 3 is a water contact angle of the glass substrate in an air environment, and (2) in fig. 3 is a water contact angle of the sample (i) in an air environment. As shown in (1) of fig. 3, the contact angle of the glass substrate is 28.2 °, and it is a hydrophilic interface, which also proves that the glass surface is easily contacted with the solution, resulting in that it is easily contaminated. From (2) of FIG. 3, it can be seen that Al is produced by atomic layer deposition2O3-TiO2After the film is formed, the contact angle of the interface is increased from 28.2 degrees to 132.5 degrees, and the film shows excellent hydrophobicity. This is because the glass has a loose porous structure, has a larger internal surface area, can adsorb more precursor molecules, and can provide more active sites to promote the generation of film molecules. And the surface layer Al2O3-TiO2The combined effect of the nanostructuring and the low surface energy of the film is to impart hydrophobic properties to the surface of the sample (i).
The transmittance test was carried out on the sample (i) and the glass substrate, and the result is shown in FIG. 4 with an enlarged view of the transmittance curve between 380 and 800 nm. As can be seen from FIG. 4, the transmittance of the glass substrate is 92%, and the transmittance of the self-cleaning hydrophobic film layer prepared by the atomic layer deposition method is about 90%, and no obvious effect is obtainedReduction, which also indicates Al produced by atomic layer deposition methods2O3-TiO2The composite film is suitable for being used as a transparent self-cleaning film.

Claims (4)

1. A preparation method of a self-cleaning hydrophobic film layer for an electronic screen is characterized by comprising the following steps: the method comprises the following operation steps:
step 1, cleaning a glass substrate;
2, drying the cleaned glass substrate by using nitrogen, then placing the glass substrate into a deposition cavity of an atomic layer deposition instrument, and pumping the deposition cavity to 5 multiplied by 10-3Torr, then introducing carrier gas until the pressure of the chamber is 0.15Torr, and the temperature in the deposition chamber is 150 ℃; then, carrying out atomic layer periodic deposition growth of the film layer on the surface of the glass substrate to obtain the glass plated with the metal oxide film layer;
the specific operation process of the step 2 for carrying out the atomic layer periodic deposition growth of the film layer on the surface of the glass substrate is as follows: 1) injecting a titanium source into a deposition cavity of the atomic layer deposition instrument in a pulse mode for a pulse time t1Is 0.06 s; 2) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t2Is 60 s; 3) injecting water source into the deposition cavity of the atomic layer deposition instrument in a pulse mode with pulse time t3Is 0.02 s; 4) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t4Is 40 s; 5) repeating the growth cycles 1) to 4) for 100 times; 6) injecting an aluminum source into a deposition cavity of the atomic layer deposition instrument in a pulse mode for a pulse time t6Is 0.02 s; 7) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t7Is 30 s; 8) injecting water source into the deposition cavity of the atomic layer deposition instrument in a pulse mode with pulse time t80.015 s; 9) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t9Is 30 s; 10) repeating the growth cycles 6) to 9) for 100 times; 11) repeating the growth cycles 1) to 10) for 3 times to obtain Al-plated film2O3And TiO2Glass of the composite film layer;
the titanium source is titanium tetraisopropoxide, the aluminum source is trimethylaluminum, and the water source is deionized water;
al obtained2O3And TiO2The microscopic morphology of the composite film layer is in a nano island shape, the whole composite film layer is compact and uniform, the surface roughness is large, the root mean square roughness is calculated to be 5.73nm, and the contact angle is 132.5 degrees.
2. The method for preparing a self-cleaning hydrophobic film layer for an electronic screen according to claim 1, wherein the method comprises the following steps: the thickness of the metal oxide film layer is 50 nm.
3. The method for preparing a self-cleaning hydrophobic film layer for an electronic screen according to claim 1, wherein the method comprises the following steps: and the carrier gas in the step 2 is nitrogen with the mass fraction of 99.99%.
4. The method for preparing a self-cleaning hydrophobic film layer for an electronic screen according to claim 1, wherein the method comprises the following steps: the glass substrate has a rectangular shape of 38X 12mm in size.
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CN106436281A (en) * 2016-10-12 2017-02-22 武汉纺织大学 Preparation method of self-cleaning fabric with ultraviolet resistant effect

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