CN106630677B - A method of realizing the super hydrophilic and super-hydrophobic controllable inversion of glass surface - Google Patents

A method of realizing the super hydrophilic and super-hydrophobic controllable inversion of glass surface Download PDF

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CN106630677B
CN106630677B CN201611179426.3A CN201611179426A CN106630677B CN 106630677 B CN106630677 B CN 106630677B CN 201611179426 A CN201611179426 A CN 201611179426A CN 106630677 B CN106630677 B CN 106630677B
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glass surface
glass
interface performance
hydrophobic
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CN106630677A (en
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罗炳威
刘大博
罗飞
田野
祁洪飞
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BEIJING INSTITUTE OF AERONAUTICAL MATERIALS CHINA AVIATION INDUSTRY GROUP Corp
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/3411Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
    • C03C17/3429Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B25/00Annealing glass products
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/20Materials for coating a single layer on glass
    • C03C2217/21Oxides
    • C03C2217/212TiO2
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/20Materials for coating a single layer on glass
    • C03C2217/28Other inorganic materials
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/70Properties of coatings
    • C03C2217/75Hydrophilic and oleophilic coatings
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/70Properties of coatings
    • C03C2217/76Hydrophobic and oleophobic coatings
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/10Deposition methods
    • C03C2218/11Deposition methods from solutions or suspensions
    • C03C2218/111Deposition methods from solutions or suspensions by dipping, immersion
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/10Deposition methods
    • C03C2218/15Deposition methods from the vapour phase
    • C03C2218/154Deposition methods from the vapour phase by sputtering
    • C03C2218/156Deposition methods from the vapour phase by sputtering by magnetron sputtering

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

The invention belongs to technical field of surface, are related to a kind of method for realizing the super hydrophilic and super-hydrophobic controllable inversion of glass surface.It is characterized by: realizing the super hydrophilic and super-hydrophobic controllable inversion of glass surface by growing different nanometer layers in glass surface.The invention proposes a kind of methods for realizing the super hydrophilic and super-hydrophobic controllable inversion of glass surface, it can be changed by controlled material surface micro-structure, realize super hydrophilic and super-hydrophobic controllable inversion, overcome super hydrophilic and super-hydrophobic inversion in the prior art it is uncontrollable and under light beam irradiation the unstable disadvantage of performance.

Description

A method of realizing the super hydrophilic and super-hydrophobic controllable inversion of glass surface
Technical field
The invention belongs to technical field of surface, are related to a kind of super hydrophilic and super-hydrophobic controllable inversion of realization glass surface Method.
Background technique
Wellability is a kind of important feature of the surface of solids.Studies have shown that wellability is by its chemical composition and microcosmic several (T.Onda, S.Shibuichi, N.Satoh, K.Tsujii, the Langmuir1996,12,2125- what structure codetermines 2127;S.Shibuichi,T.Onda,N.Satoh,K.Tsujii,J.Phys.Chem.1996,100,19512- 19517.W.Chen,A.Y.Fadeev,M.C.Hsieh,et al.Langmuir,1999,15,3395-3399.).Superhydrophilic It is the main forms of surface wettability with super-hydrophobicity, the contact angle of liquid and interface that ordinary meaning is taken on interface exists It is super hydrophilic when the liquid of interface surface and the contact angle at interface are at 10 degree or less to be super-hydrophobic at 150 degree or so (T.Onda,S.Shibuichi,N.Satoh,K.Tsujii,Langmuir 1996,12,2125-2127;H.Y.Erbil, A.L.Demirel,Y.Avcl et al.Science,2003,299,1377.).The material for having this performance is raw in industrial or agricultural There is very main application in production.Such as the froth flotation of mineral, waterproof, washing;Super-hydrophobic boundary material is used for aircraft skylight Antifog, exterior aerial, can be to prevent accumulated snow, to guarantee the reception of high-quality signal;It is coated in shell, the burning deposit of steamer Case can achieve antifouling, corrosion-resistant effect.
Currently, the method for regulation interface hydrophilicity and hydrophobicity is the microstructure change by controlling the surface of solids, such as pass through CdTe three-dimensional manometer stick array prepares stable super-hydrophobic interface performance (B.W.Luo, Y.Deng, Y Wang et al.Applied Surface Science,2013,280,550.).Super-hydrophobic and super hydrophilic controllable transformation is on the surface of the material Technical field has important application.In terms of realizing super hydrophilic and super-hydrophobic transformation, have been reported that using ultraviolet lighting ZnO nano Stick array realizes the super hydrophilic and super-hydrophobic transformation in interface (X.J.Feng, L.Feng, M.H.Jin et al.Journal of American Chemistry Society, 2004,126,62-63.).It is this that close and distant performance is changed by high-energy light beam guiding irradiation Method have invertibity, make its performance less stable, limit the engineering application of material.
Summary of the invention
The purpose of the present invention: a kind of method for realizing the super hydrophilic and super-hydrophobic controllable inversion of glass surface is proposed, to lead to Regulation material surface microstructure change is crossed, super hydrophilic and super-hydrophobic controllable inversion is realized, overcomes super hydrophilic and super in the prior art Hydrophobic inversion it is uncontrollable and under light beam irradiation the unstable disadvantage of performance.
Technical solution of the present invention: a method of realizing the super hydrophilic and super-hydrophobic controllable inversion of glass surface, feature It is: by growing different nanometer layers in glass surface, realizes the super hydrophilic and super-hydrophobic controllable inversion of glass surface, step It is as follows:
1, realize that glass surface is super hydrophilic:
One layer of TiO is grown in glass surface2Monodimension nano stick array makes glass surface have super hydrophilic interface performance; Grow TiO2The method of monodimension nano stick array is:
1.1, it prepares hydrochloric acid solution: by 30% mixed in hydrochloric acid of deionized water and equivalent, hydrochloric acid solution is obtained, in air Middle stirring at least 1min;
1.2, it prepares the mixed solution of butyl titanate and hydrochloric acid: butyl titanate, metatitanic acid four being added into hydrochloric acid solution The volume ratio of butyl ester and hydrochloric acid solution is 0.01~0.03, stirs at least 5min, by the mixed of obtained butyl titanate and hydrochloric acid It closes solution and is put into stainless steel autoclave;
1.3, it cleans glass: glass being put into after cleaning at least 30min in the ultrasonic cleaner equipped with cleaning solution and taken out, With being dried after distilled water flushing at least 1min;Cleaning solution is distilled water: acetone: isobutanol=1:1:1 mixed solution;
1.4, it prepares ultra-hydrophilic surface: glass being put into stainless steel autoclave, butyl titanate and salt are immersed in In the mixed solution of acid, autoclave is reacted at least 8h in the baking oven that temperature is 135 DEG C, then glass is taken out, is used It is dried after distilled water flushing at least 1min, glass surface at this time has super hydrophilic interface performance;
2, the glass surface of super hydrophilic interface performance is changed into the glass surface of super-hydrophobic interface performance:
Cadmium telluride is sputtered by the glass surface in super hydrophilic interface performance, the glass surface of super hydrophilic interface performance is turned Become the glass surface of super-hydrophobic interface performance;The method of sputtering cadmium telluride is: it is true that cadmium telluride target is put into magnetic control sputtering device On radio frequency platform in empty room;The glass of super hydrophilic interface performance is placed on sample stage;Adjust sample stage and radio frequency platform away from From d=60mm~120mm;To vacuum chamber, the indoor vacuum degree of vacuum is made to reach 1.0 × 10- 3Pa~4.0 × 10? 4Pa;The glass of super hydrophilic interface performance is heated to 25 DEG C~100 DEG C;It is filled with argon gas into vacuum chamber, and Ar Pressure is emphasized It saves to 0.4Pa~4.0Pa;Apply radio-frequency current 10mA~140mA, radio-frequency voltage is adjusted to 0.1kV~0.60kV;Sedimentation time For 5min~20min, then cooled to room temperature, glass surface at this time have super-hydrophobic interface performance;
3, super-hydrophobic glass surface is changed into super hydrophilic:
The cadmium telluride that the glass surface of super hydrophilic interface performance is sputtered at by removing changes super-hydrophobic glass surface For super hydrophilic glass surface;The method of removal is: the glass of super-hydrophobic interface performance is placed in high temperature rapid thermal annealing furnace, is added Hot temperature is 600 DEG C~800 DEG C, then soaking time at least 20min naturally cools to room temperature, and glass surface at this time restores For super hydrophilic interface performance.
The invention has the advantages that proposing a kind of method for realizing the super hydrophilic and super-hydrophobic controllable inversion of glass surface, energy Changed by controlled material surface micro-structure, realizes super hydrophilic and super-hydrophobic controllable inversion, overcome super hydrophilic in the prior art With super-hydrophobic inversion it is uncontrollable and under light beam irradiation the unstable disadvantage of performance.Meanwhile the present invention have it is easy to operate, Controllable inversion effect is good, the stable advantage of performance.
Detailed description of the invention
Fig. 1 is the stereoscan photograph with the glass surface of super hydrophilic interface performance.It is up-narrow and down-wide TiO in figure2 Monodimension nano stick array, since its special micro-structure makes it have super hydrophilicity.
Fig. 2 is the stereoscan photograph with the glass surface of super-hydrophobic interface performance.TiO is sputtered in figure for CdTe2 Monodimension nano stick array surface makes it have ultra-hydrophobicity since its interface microstructure becomes coarse.
Fig. 3 is the contact angle microphoto with the glass surface of super hydrophilic interface performance.It is divided into water droplet compared with blackboard in figure Shape, circular arc degree are each 6.1 degree of left and right, are defined as less than 10 degree super hydrophilic.
Fig. 4 is the contact angle microphoto with the glass surface of super-hydrophobic interface performance.Rounded portion is water droplet in figure Shape, circular arc degree be left and right it is each be defined as close to 150 degree it is super-hydrophobic.
Fig. 5 is the contact angle microphoto for reverting to the glass surface of super hydrophilic interface performance.It is divided into water compared with blackboard in figure Shape is dripped, circular arc degree is defined as super hydrophilic for each 10 degree of left and right.
Specific embodiment
The invention will be described in further detail below.It is a kind of to realize glass surface super hydrophilic and super-hydrophobic controllable inversion Method, it is characterised in that: by growing different nanometer layers in glass surface, realize glass surface it is super hydrophilic and super-hydrophobic can Inversion is controlled, steps are as follows:
1, realize that glass surface is super hydrophilic:
One layer of TiO is grown in glass surface2Monodimension nano stick array makes glass surface have super hydrophilic interface performance; Grow TiO2The method of monodimension nano stick array is:
1.1, it prepares hydrochloric acid solution: by 30% mixed in hydrochloric acid of deionized water and equivalent, hydrochloric acid solution is obtained, in air Middle stirring at least 1min;
1.2, it prepares the mixed solution of butyl titanate and hydrochloric acid: butyl titanate, metatitanic acid four being added into hydrochloric acid solution The volume ratio of butyl ester and hydrochloric acid solution is 0.01~0.03, stirs at least 5min, by the mixed of obtained butyl titanate and hydrochloric acid It closes solution and is put into stainless steel autoclave;
1.3, it cleans glass: glass being put into after cleaning at least 30min in the ultrasonic cleaner equipped with cleaning solution and taken out, With being dried after distilled water flushing at least 1min;Cleaning solution is distilled water: acetone: isobutanol=1:1:1 mixed solution;
1.4, it prepares ultra-hydrophilic surface: glass being put into stainless steel autoclave, butyl titanate and salt are immersed in In the mixed solution of acid, autoclave is reacted at least 8h in the baking oven that temperature is 135 DEG C, then glass is taken out, is used It is dried after distilled water flushing at least 1min, glass surface at this time has super hydrophilic interface performance;
2, the glass surface of super hydrophilic interface performance is changed into the glass surface of super-hydrophobic interface performance:
Cadmium telluride is sputtered by the glass surface in super hydrophilic interface performance, the glass surface of super hydrophilic interface performance is turned Become the glass surface of super-hydrophobic interface performance;The method of sputtering cadmium telluride is: it is true that cadmium telluride target is put into magnetic control sputtering device On radio frequency platform in empty room;The glass of super hydrophilic interface performance is placed on sample stage;Adjust sample stage and radio frequency platform away from From d=60mm~120mm;To vacuum chamber, the indoor vacuum degree of vacuum is made to reach 1.0 × 10- 3Pa~4.0 × 10? 4Pa;The glass of super hydrophilic interface performance is heated to 25 DEG C~100 DEG C;It is filled with argon gas into vacuum chamber, and Ar Pressure is emphasized It saves to 0.4Pa~4.0Pa;Apply radio-frequency current 10mA~140mA, radio-frequency voltage is adjusted to 0.1kV~0.60kV;Sedimentation time For 5min~20min, then cooled to room temperature, glass surface at this time have super-hydrophobic interface performance;
3, super-hydrophobic glass surface is changed into super hydrophilic:
The cadmium telluride that the glass surface of super hydrophilic interface performance is sputtered at by removing changes super-hydrophobic glass surface For super hydrophilic glass surface;The method of removal is: the glass of super-hydrophobic interface performance is placed in high temperature rapid thermal annealing furnace, is added Hot temperature is 600 DEG C~800 DEG C, then soaking time at least 20min naturally cools to room temperature, and glass surface at this time restores For super hydrophilic interface performance.
The working principle of the invention is: passing through up-narrow and down-wide TiO2The special micro-structure of monodimension nano stick array, makes its tool There is super hydrophilic interface performance;TiO is covered by CdTe2Material surface change micro-structure, realize it is super hydrophilic be changed into it is super-hydrophobic;It is logical The CdTe for crossing removal covering TiO2 material surface, restores Superhydrophilic.
Embodiment 1:
1. realizing that glass surface is super hydrophilic:
1.1, it prepares hydrochloric acid solution: the hydrochloric acid 24ml of the deionized water of 24ml and 30% is mixed in beaker.It will mixing Object stirs 1min in air;
1.2, it prepares the mixed solution of butyl titanate and hydrochloric acid: 1.5ml butyl titanate being added into hydrochloric acid solution, stirs 5min is mixed, the mixed solution of obtained butyl titanate and hydrochloric acid is put into stainless steel autoclave;
1.3, it cleans glass: glass being put into after cleaning 30min in the ultrasonic cleaner equipped with cleaning solution and taken out, with steaming Distilled water is dried after rinsing 1min;Cleaning solution is distilled water: acetone: isobutanol=1:1:1 mixed solution;
1.4, it prepares ultra-hydrophilic surface: glass being put into stainless steel autoclave, butyl titanate and salt are immersed in In the mixed solution of acid, autoclave is reacted into 8h in the baking oven that temperature is 135 DEG C, is then taken out glass, with distillation Water is dried after rinsing 1min, and glass surface at this time has super hydrophilic interface performance;
2, the glass surface of super hydrophilic interface performance is changed into the glass surface of super-hydrophobic interface performance:
Cadmium telluride target is put on the radio frequency platform in magnetic control sputtering device vacuum chamber;The glass of super hydrophilic interface performance is put It is placed on sample stage;Adjust sample stage and radio frequency platform distance d=60mm;To vacuum chamber, make the indoor vacuum of vacuum Degree reaches 4.0 × 10- 4Pa;The glass of super hydrophilic interface performance is heated to 25 DEG C;It is filled with argon gas into vacuum chamber, and by argon Air pressure is adjusted to by force 0.4Pa;Apply radio-frequency current 140mA, radio-frequency voltage is adjusted to 0.10kV;Sedimentation time is 5min, then Cooled to room temperature, glass surface at this time have super-hydrophobic interface performance;
3, super-hydrophobic glass surface is changed into super hydrophilic:
The cadmium telluride that the glass surface of super hydrophilic interface performance is sputtered at by removing changes super-hydrophobic glass surface For super hydrophilic glass surface;The method of removal is: the glass of super-hydrophobic interface performance is placed in high temperature rapid thermal annealing furnace, is added Hot temperature is 600 DEG C, and then soaking time 25min naturally cools to room temperature, glass surface at this time reverts to super hydrophilic interface Performance.
4, sample characterization:
By above-mentioned glass super hydrophilic interface (TiO2Monodimension nano stick array) and the super-hydrophobic interface (TiO of glass2/ CdTe is one-dimensional Nanometer stick array) it is scanned electron microscope observation, as illustrated in fig. 1 and 2.Surface contact angle table is carried out to above-mentioned three kinds of materials Sign, as a result as in Figure 3-5
Embodiment 2:
1. realizing that glass surface is super hydrophilic:
1.1, it prepares hydrochloric acid solution: the hydrochloric acid 50ml of the deionized water of 50ml and 30% is mixed in beaker.It will mixing Object stirs 5min in air;
1.2, it prepares the mixed solution of butyl titanate and hydrochloric acid: 1.0ml butyl titanate being added into hydrochloric acid solution, stirs 15min is mixed, the mixed solution of obtained butyl titanate and hydrochloric acid is put into stainless steel autoclave;
1.3, it cleans glass: glass being put into after cleaning 60min in the ultrasonic cleaner equipped with cleaning solution and taken out, with steaming Distilled water is dried after rinsing 2min;Cleaning solution is distilled water: acetone: isobutanol=1:1:1 mixed solution;
1.4, it prepares ultra-hydrophilic surface: glass being put into stainless steel autoclave, butyl titanate and salt are immersed in In the mixed solution of acid, autoclave is reacted into 12h in the baking oven that temperature is 135 DEG C, is then taken out glass, with distillation Water is dried after rinsing 5min, and glass surface at this time has super hydrophilic interface performance;
2, the glass surface of super hydrophilic interface performance is changed into the glass surface of super-hydrophobic interface performance:
Cadmium telluride is sputtered by the glass surface in super hydrophilic interface performance, the glass surface of super hydrophilic interface performance is turned Become the glass surface of super-hydrophobic interface performance;The method of sputtering cadmium telluride is: it is true that cadmium telluride target is put into magnetic control sputtering device On radio frequency platform in empty room;The glass of super hydrophilic interface performance is placed on sample stage;Adjust sample stage and radio frequency platform away from From d=120mm;To vacuum chamber, the indoor vacuum degree of vacuum is made to reach 1.0 × 10- 3Pa;Super hydrophilic interface performance Glass be heated to 100 DEG C;It is filled with argon gas into vacuum chamber, and ar pressure is adjusted to 4.0Pa;Apply radio-frequency current 10mA, radio-frequency voltage are adjusted to 0.60kV;Sedimentation time is 20min, then cooled to room temperature, glass surface tool at this time There is super-hydrophobic interface performance;
3, super-hydrophobic glass surface is changed into super hydrophilic:
The cadmium telluride that the glass surface of super hydrophilic interface performance is sputtered at by removing changes super-hydrophobic glass surface For super hydrophilic glass surface;The method of removal is: the glass of super-hydrophobic interface performance is placed in high temperature rapid thermal annealing furnace, is added Hot temperature is 800 DEG C, and then soaking time 20min naturally cools to room temperature, glass surface at this time reverts to super hydrophilic interface Performance.
Embodiment 3:
1. realizing that glass surface is super hydrophilic:
1.1, it prepares hydrochloric acid solution: the concentrated hydrochloric acid 12ml of the deionized water of 12ml and 30% is mixed in beaker.It will mix It closes object and stirs 3min in air;
1.2, it prepares the mixed solution of butyl titanate and hydrochloric acid: 0.48ml butyl titanate being added into hydrochloric acid solution, 25min is stirred, the mixed solution of obtained butyl titanate and hydrochloric acid is put into stainless steel autoclave;
1.3, it cleans glass: glass being put into after cleaning 40min in the ultrasonic cleaner equipped with cleaning solution and taken out, with steaming Distilled water is dried after rinsing 3min;Cleaning solution is distilled water: acetone: isobutanol=1:1:1 mixed solution;
1.4, it prepares ultra-hydrophilic surface: glass being put into stainless steel autoclave, butyl titanate and salt are immersed in In the mixed solution of acid, autoclave is reacted into 10h in the baking oven that temperature is 135 DEG C, is then taken out glass, with distillation Water is dried after rinsing 10min, and glass surface at this time has super hydrophilic interface performance;
2, the glass surface of super hydrophilic interface performance is changed into the glass surface of super-hydrophobic interface performance:
Cadmium telluride is sputtered by the glass surface in super hydrophilic interface performance, the glass surface of super hydrophilic interface performance is turned Become the glass surface of super-hydrophobic interface performance;The method of sputtering cadmium telluride is: it is true that cadmium telluride target is put into magnetic control sputtering device On radio frequency platform in empty room;The glass of super hydrophilic interface performance is placed on sample stage;Adjust sample stage and radio frequency platform away from From d=90mm;To vacuum chamber, the indoor vacuum degree of vacuum is made to reach 8.0 × 10- 4Pa;Super hydrophilic interface performance Glass is heated to 65 DEG C;It is filled with argon gas into vacuum chamber, and ar pressure is adjusted to 2.0Pa;Apply radio-frequency current 30mA, penetrates Frequency voltage is adjusted to 0.30kV;Sedimentation time is 10min, then cooled to room temperature, and glass surface at this time has super thin Water termination performance;
3, super-hydrophobic glass surface is changed into super hydrophilic:
The cadmium telluride that the glass surface of super hydrophilic interface performance is sputtered at by removing changes super-hydrophobic glass surface For super hydrophilic glass surface;The method of removal is: the glass of super-hydrophobic interface performance is placed in high temperature rapid thermal annealing furnace, is added Hot temperature is 700 DEG C, and then soaking time 25min naturally cools to room temperature, glass surface at this time reverts to super hydrophilic interface Performance.

Claims (1)

1. a kind of method for realizing the super hydrophilic and super-hydrophobic controllable inversion of glass surface, it is characterised in that: by glass surface Different nanometer layers is grown, realizes the super hydrophilic and super-hydrophobic controllable inversion of glass surface, steps are as follows:
1.1, realize that glass surface is super hydrophilic:
One layer of TiO is grown in glass surface2Monodimension nano stick array makes glass surface have super hydrophilic interface performance;Growth TiO2The method of monodimension nano stick array is:
1.1.1, prepare hydrochloric acid solution: by 30% mixed in hydrochloric acid of deionized water and equivalent volumes, hydrochloric acid solution is obtained, in sky At least 1min is stirred in gas;
1.1.2, prepare the mixed solution of butyl titanate and hydrochloric acid: butyl titanate, four fourth of metatitanic acid being added into hydrochloric acid solution The volume ratio of ester and hydrochloric acid solution is 0.01~0.03, at least 5min is stirred, by the mixing of obtained butyl titanate and hydrochloric acid Solution is put into stainless steel autoclave;
1.1.3, clean glass: glass being put into after cleaning at least 30min in the ultrasonic cleaner equipped with cleaning solution and taken out, use It is dried after distilled water flushing at least 1min;Cleaning solution is distilled water: acetone: isobutanol=1:1:1 mixed solution;
1.1.4, prepare ultra-hydrophilic surface: glass being put into stainless steel autoclave, butyl titanate and hydrochloric acid are immersed in Mixed solution in, in temperature be to react at least 8h in 135 DEG C of baking oven by autoclave, then take out glass, with steaming Distilled water is dried after rinsing at least 1min, and glass surface at this time has super hydrophilic interface performance;
1.2, the glass surface of super hydrophilic interface performance is changed into the glass surface of super-hydrophobic interface performance:
Cadmium telluride is sputtered by the glass surface in super hydrophilic interface performance, the glass surface of super hydrophilic interface performance is changed into The glass surface of super-hydrophobic interface performance;The method of sputtering cadmium telluride is: cadmium telluride target is put into magnetic control sputtering device vacuum chamber In radio frequency platform on;The glass of super hydrophilic interface performance is placed on sample stage;Adjust sample stage and radio frequency platform distance d= 60mm~120mm;To vacuum chamber, the indoor vacuum degree of vacuum is made to reach 1.0 × 10- 3Pa~4.0 × 10- 4Pa;Super The glass of hydrophilic interface performance is heated to 25 DEG C~100 DEG C;It is filled with argon gas into vacuum chamber, and ar pressure is adjusted to 0.4Pa~4.0Pa;Apply radio-frequency current 10mA~140mA, radio-frequency voltage is adjusted to 0.1kV~0.60kV;Sedimentation time is 5min~20min, then cooled to room temperature, glass surface at this time have super-hydrophobic interface performance;
1.3, super-hydrophobic glass surface is changed into super hydrophilic:
The cadmium telluride that the glass surface of super hydrophilic interface performance is sputtered at by removing, super-hydrophobic glass surface is changed into super Hydrophilic glass surface;The method of removal is: the glass of super-hydrophobic interface performance is placed in high temperature rapid thermal annealing furnace, heating temperature Degree is 600 DEG C~800 DEG C, and then soaking time at least 20min naturally cools to room temperature, glass surface at this time reverts to super Hydrophilic interface performance.
CN201611179426.3A 2016-12-19 2016-12-19 A method of realizing the super hydrophilic and super-hydrophobic controllable inversion of glass surface Active CN106630677B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1760113A (en) * 2005-11-16 2006-04-19 厦门大学 Method for preparing film of Nano tube array of titanium dioxide in both ultra hydrophilicity and lipophilicity, and ultra hydrophobicity
CN102503554A (en) * 2011-11-02 2012-06-20 西南交通大学 Method for preparing oil-water-soaked light-operated reversible SiO2/TiO2 composite coating on silicon substrate surface
CN103135224A (en) * 2013-03-25 2013-06-05 武汉工程大学 Preparation method for light-operated reversible wetting coating
CN105887158A (en) * 2016-05-25 2016-08-24 哈尔滨工业大学 Nanocrystalline metal oxide array with under-oil super-hydrophobicity and super-hydrophilicity reversible transition function and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1760113A (en) * 2005-11-16 2006-04-19 厦门大学 Method for preparing film of Nano tube array of titanium dioxide in both ultra hydrophilicity and lipophilicity, and ultra hydrophobicity
CN102503554A (en) * 2011-11-02 2012-06-20 西南交通大学 Method for preparing oil-water-soaked light-operated reversible SiO2/TiO2 composite coating on silicon substrate surface
CN103135224A (en) * 2013-03-25 2013-06-05 武汉工程大学 Preparation method for light-operated reversible wetting coating
CN105887158A (en) * 2016-05-25 2016-08-24 哈尔滨工业大学 Nanocrystalline metal oxide array with under-oil super-hydrophobicity and super-hydrophilicity reversible transition function and preparation method thereof

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