CN106630677A - Method for achieving controlled super-hydrophilic and super-hydrophobic inversion of glass surface - Google Patents
Method for achieving controlled super-hydrophilic and super-hydrophobic inversion of glass surface Download PDFInfo
- Publication number
- CN106630677A CN106630677A CN201611179426.3A CN201611179426A CN106630677A CN 106630677 A CN106630677 A CN 106630677A CN 201611179426 A CN201611179426 A CN 201611179426A CN 106630677 A CN106630677 A CN 106630677A
- Authority
- CN
- China
- Prior art keywords
- super
- glass surface
- hydrophobic
- glass
- interface performance
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface 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
- C03C17/3429—Surface 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/212—TiO2
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/28—Other inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/75—Hydrophilic and oleophilic coatings
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/76—Hydrophobic and oleophobic coatings
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/154—Deposition methods from the vapour phase by sputtering
- C03C2218/156—Deposition methods from the vapour phase by sputtering by magnetron sputtering
Landscapes
- Chemical & Material Sciences (AREA)
- 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 the technical field of surface treatment, and relates to a method for achieving controlled super-hydrophilic and super-hydrophobic inversion of a glass surface. The method is characterized in that controlled super-hydrophilic and super-hydrophobic inversion of the glass surface is achieved through growing different nano layers on the glass surface. According to the method for achieving controlled super-hydrophilic and super-hydrophobic inversion of the glass surface, controlled super-hydrophilic and super-hydrophobic inversion can be achieved through regulating and controlling a microstructure change of the material surface, and the defects of uncontrollable super-hydrophilic and super-hydrophobic inversion and unstable performance under light irradiation in the prior art are overcome.
Description
Technical field
The invention belongs to technical field of surface, is related to one kind and realizes the super hydrophilic and super-hydrophobic controllable inversion of glass surface
Method.
Background technology
Wellability is a kind of key character of the surface of solids.Research shows that wellability is several by its chemical composition and microcosmic
(T.Onda, S.Shibuichi, N.Satoh, K.Tsujii, Langmuir1996,12,2125- that what structure is together decided on
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
The liquid being taken on interface with the main forms that super-hydrophobicity is surface wettability, ordinary meaning and the contact angle at interface exist
It is super-hydrophobic when 150 degree or so, is super hydrophilic when the liquid of interface surface and the contact angle at interface are below 10 degree
(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 possessing this performance is given birth in industrial or agricultural
There is very main application in product.Such as froth flotation, waterproof, the washing of mineral；Super-hydrophobic boundary material is used for aircraft skylight
Antifog, exterior aerial, can be in case accumulated snow, so as to ensure the reception of high-quality signal；It is coated in shell, the burning deposit of steamer
Case, can reach antifouling, corrosion-resistant effect.
At present, the method for regulating and controlling interface hydrophilicity and hydrophobicity is the microstructure change by controlling the surface of solids, is such as passed through
CdTe three-dimensional manometer rod arrays prepare 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 in material surface
Technical field has important application.In terms of super hydrophilic and super-hydrophobic transformation is realized, have been reported that using ultraviolet lighting ZnO nano
Rod 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 there is invertibity so as to performance less stable, limit the engineering application of material.
The content 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 and control material surface microstructure change is crossed, super hydrophilic and super-hydrophobic controllable inversion is realized, overcomes super hydrophilic and super in prior art
Hydrophobic inversion it is uncontrollable and light beam irradiation under unstable properties shortcoming.
Technical scheme：A kind of method for realizing the super hydrophilic and super-hydrophobic controllable inversion of glass surface, its feature
It is：By growing different nanometer layers in glass surface, the super hydrophilic and super-hydrophobic controllable inversion of glass surface, step are realized
It is as follows：
1st, 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：
1.1st, hydrochloric acid solution is prepared：By the 30% of deionized water and equivalent mixed in hydrochloric acid, hydrochloric acid solution is obtained, in air
Middle stirring at least 1min；
1.2nd, the mixed solution of butyl titanate and hydrochloric acid is prepared：Butyl titanate, metatitanic acid four are added in 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 the butyl titanate for obtaining and hydrochloric acid
Close solution and be put into stainless steel autoclave；
1.3rd, glass is cleaned：Glass is put into the ultrasonic cleaner equipped with cleaning fluid to clean after at least 30min and is taken out,
With distilled water flushing at least 1min post-dryings；Cleaning fluid is distilled water：Acetone：Isobutanol=1：1：1 mixed solution；
1.4th, ultra-hydrophilic surface is prepared：Glass is put into stainless steel autoclave, butyl titanate and salt is 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 take out in glass, used
Distilled water flushing at least 1min post-dryings, glass surface now has super hydrophilic interface performance；
The 2nd, 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
It is changed into the glass surface of super-hydrophobic interface performance；Sputtering the method for cadmium telluride is：Cadmium telluride target is put into magnetic control sputtering device true
On radio frequency platform in empty room；The glass of super hydrophilic interface performance is positioned on sample stage；Adjust sample stage and radio frequency platform away from
From d=60mm～120mm；To vacuum chamber, the vacuum in vacuum room is set 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；Argon gas is filled with vacuum chamber, and Ar Pressure is emphasized
Save 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, room temperature is then naturally cooled to, glass surface now has super-hydrophobic interface performance；
3rd, super-hydrophobic glass surface is changed into super hydrophilic：
By the cadmium telluride for removing the glass surface for sputtering at super hydrophilic interface performance, super-hydrophobic glass surface is changed
For super hydrophilic glass surface；The method of removal is：The glass of super-hydrophobic interface performance is positioned in high temperature rapid thermal annealing stove, plus
Hot temperature is 600 DEG C～800 DEG C, and then temperature retention time at least 20min naturally cools to room temperature, and glass surface now recovers
For super hydrophilic interface performance.
It is an advantage of the invention that：Propose 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, realize super hydrophilic and super-hydrophobic controllable inversion, overcome super hydrophilic in prior art
Uncontrollable with super-hydrophobic inversion and the unstable properties under light beam irradiation shortcomings.Meanwhile, the present invention have it is simple to operate,
Controllable inversion effect is good, the advantage of stable performance.
Description of the drawings
Fig. 1 is the stereoscan photograph of the glass surface with super hydrophilic interface performance.It is up-narrow and down-wide TiO in figure2
Monodimension nano stick array, because its special micro-structural makes it have super hydrophilicity.
Fig. 2 is the stereoscan photograph of the glass surface with super-hydrophobic interface performance.TiO is sputtered in figure for CdTe2
Monodimension nano stick array surface, because its interface microstructure becomes coarse ultra-hydrophobicity is made it have.
Fig. 3 is the contact angle microphoto of the glass surface with super hydrophilic interface performance.It is divided into water droplet compared with blackboard in figure
Shape, its circular arc number of degrees are that left and right is each 6.1 degree, are defined as less than 10 degree super hydrophilic.
Fig. 4 is the contact angle microphoto of the glass surface with super-hydrophobic interface performance.Rounded portion is water droplet in figure
Shape, its circular arc number of degrees be left and right it is each close 150 degree be defined as it is super-hydrophobic.
Fig. 5 is the contact angle microphoto of the glass surface for reverting to super hydrophilic interface performance.It is divided into water compared with blackboard in figure
Drop shape, its circular arc number of degrees be left and right it is each 10 degree be defined as it is super hydrophilic.
Specific embodiment
The present invention is 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
Control inversion, step is as follows：
1st, 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：
1.1st, hydrochloric acid solution is prepared：By the 30% of deionized water and equivalent mixed in hydrochloric acid, hydrochloric acid solution is obtained, in air
Middle stirring at least 1min；
1.2nd, the mixed solution of butyl titanate and hydrochloric acid is prepared：Butyl titanate, metatitanic acid four are added in 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 the butyl titanate for obtaining and hydrochloric acid
Close solution and be put into stainless steel autoclave；
1.3rd, glass is cleaned：Glass is put into the ultrasonic cleaner equipped with cleaning fluid to clean after at least 30min and is taken out,
With distilled water flushing at least 1min post-dryings；Cleaning fluid is distilled water：Acetone：Isobutanol=1：1：1 mixed solution；
1.4th, ultra-hydrophilic surface is prepared：Glass is put into stainless steel autoclave, butyl titanate and salt is 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 take out in glass, used
Distilled water flushing at least 1min post-dryings, glass surface now has super hydrophilic interface performance；
The 2nd, 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
It is changed into the glass surface of super-hydrophobic interface performance；Sputtering the method for cadmium telluride is：Cadmium telluride target is put into magnetic control sputtering device true
On radio frequency platform in empty room；The glass of super hydrophilic interface performance is positioned on sample stage；Adjust sample stage and radio frequency platform away from
From d=60mm～120mm；To vacuum chamber, the vacuum in vacuum room is set 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；Argon gas is filled with vacuum chamber, and Ar Pressure is emphasized
Save 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, room temperature is then naturally cooled to, glass surface now has super-hydrophobic interface performance；
3rd, super-hydrophobic glass surface is changed into super hydrophilic：
By the cadmium telluride for removing the glass surface for sputtering at super hydrophilic interface performance, super-hydrophobic glass surface is changed
For super hydrophilic glass surface；The method of removal is：The glass of super-hydrophobic interface performance is positioned in high temperature rapid thermal annealing stove, plus
Hot temperature is 600 DEG C～800 DEG C, and then temperature retention time at least 20min naturally cools to room temperature, and glass surface now recovers
For super hydrophilic interface performance.
The present invention operation principle be：By up-narrow and down-wide TiO2The special micro-structural of monodimension nano stick array so as to have
There is super hydrophilic interface performance；TiO is covered by CdTe2Material surface change micro-structural, realize it is super hydrophilic be changed into it is super-hydrophobic；It is logical
Cross and remove the CdTe for covering TiO2 material surfaces, reduce Superhydrophilic.
Embodiment 1：
1. realize that glass surface is super hydrophilic：
1.1st, hydrochloric acid solution is prepared：The hydrochloric acid 24ml of the deionized water of 24ml and 30% is mixed in beaker.Will mixing
Thing stirs in atmosphere 1min；
1.2nd, the mixed solution of butyl titanate and hydrochloric acid is prepared：1.5ml butyl titanates are added in hydrochloric acid solution, is stirred
5min is mixed, the mixed solution of the butyl titanate for obtaining and hydrochloric acid is put into stainless steel autoclave；
1.3rd, glass is cleaned：Glass is put into the ultrasonic cleaner equipped with cleaning fluid to clean after 30min and is taken out, with steaming
Distilled water rinses 1min post-dryings；Cleaning fluid is distilled water：Acetone：Isobutanol=1：1：1 mixed solution；
1.4th, ultra-hydrophilic surface is prepared：Glass is put into stainless steel autoclave, butyl titanate and salt is immersed in
In the mixed solution of acid, autoclave is reacted into 8h in the baking oven that temperature is 135 DEG C, then taken out in glass, with distillation
Water rinses 1min post-dryings, and glass surface now has super hydrophilic interface performance；
The 2nd, the glass surface of super hydrophilic interface performance is changed into the glass surface of super-hydrophobic interface performance：
On the radio frequency platform that cadmium telluride target is put into magnetic control sputtering device vacuum chamber；The glass of super hydrophilic interface performance is put
It is placed on sample stage；Sample stage is adjusted with radio frequency platform apart from d=60mm；To vacuum chamber, the vacuum in vacuum room is made
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 in vacuum chamber, and by argon
Air pressure is emphasized to save to 0.4Pa；Apply radio-frequency current 140mA, radio-frequency voltage is adjusted to 0.10kV；Sedimentation time is 5min, then
Room temperature is naturally cooled to, glass surface now has super-hydrophobic interface performance；
3rd, super-hydrophobic glass surface is changed into super hydrophilic：
By the cadmium telluride for removing the glass surface for sputtering at super hydrophilic interface performance, super-hydrophobic glass surface is changed
For super hydrophilic glass surface；The method of removal is：The glass of super-hydrophobic interface performance is positioned in high temperature rapid thermal annealing stove, plus
Hot temperature is 600 DEG C, and then temperature retention time 25min naturally cools to room temperature, and glass surface now reverts to super hydrophilic interface
Performance.
4th, 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) electron microscope observation is scanned, as illustrated in fig. 1 and 2.Surface contact angle table is carried out to above-mentioned three kinds of materials
Levy, as a result as in Figure 3-5
Embodiment 2：
1. realize that glass surface is super hydrophilic：
1.1st, hydrochloric acid solution is prepared：The hydrochloric acid 50ml of the deionized water of 50ml and 30% is mixed in beaker.Will mixing
Thing stirs in atmosphere 5min；
1.2nd, the mixed solution of butyl titanate and hydrochloric acid is prepared：1.0ml butyl titanates are added in hydrochloric acid solution, is stirred
15min is mixed, the mixed solution of the butyl titanate for obtaining and hydrochloric acid is put into stainless steel autoclave；
1.3rd, glass is cleaned：Glass is put into the ultrasonic cleaner equipped with cleaning fluid to clean after 60min and is taken out, with steaming
Distilled water rinses 2min post-dryings；Cleaning fluid is distilled water：Acetone：Isobutanol=1：1：1 mixed solution；
1.4th, ultra-hydrophilic surface is prepared：Glass is put into stainless steel autoclave, butyl titanate and salt is immersed in
In the mixed solution of acid, autoclave is reacted into 12h in the baking oven that temperature is 135 DEG C, then taken out in glass, with distillation
Water rinses 5min post-dryings, and glass surface now has super hydrophilic interface performance；
The 2nd, 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
It is changed into the glass surface of super-hydrophobic interface performance；Sputtering the method for cadmium telluride is：Cadmium telluride target is put into magnetic control sputtering device true
On radio frequency platform in empty room；The glass of super hydrophilic interface performance is positioned on sample stage；Adjust sample stage and radio frequency platform away from
From d=120mm；To vacuum chamber, the vacuum in vacuum room is set to reach 1.0 × 10- 3Pa；Super hydrophilic interface performance
Glass be heated to 100 DEG C；Argon gas is filled with vacuum chamber, and ar pressure is adjusted to 4.0Pa；Apply radio-frequency current
10mA, radio-frequency voltage is adjusted to 0.60kV；Sedimentation time is 20min, then naturally cools to room temperature, and glass surface now has
There is super-hydrophobic interface performance；
3rd, super-hydrophobic glass surface is changed into super hydrophilic：
By the cadmium telluride for removing the glass surface for sputtering at super hydrophilic interface performance, super-hydrophobic glass surface is changed
For super hydrophilic glass surface；The method of removal is：The glass of super-hydrophobic interface performance is positioned in high temperature rapid thermal annealing stove, plus
Hot temperature is 800 DEG C, and then temperature retention time 20min naturally cools to room temperature, and glass surface now reverts to super hydrophilic interface
Performance.
Embodiment 3：
1. realize that glass surface is super hydrophilic：
1.1st, hydrochloric acid solution is prepared：The concentrated hydrochloric acid 12ml of the deionized water of 12ml and 30% is mixed in beaker.Will be mixed
Compound stirs in atmosphere 3min；
1.2nd, the mixed solution of butyl titanate and hydrochloric acid is prepared：0.48ml butyl titanates are added in hydrochloric acid solution,
Stirring 25min, by the mixed solution of the butyl titanate for obtaining and hydrochloric acid stainless steel autoclave is put into；
1.3rd, glass is cleaned：Glass is put into the ultrasonic cleaner equipped with cleaning fluid to clean after 40min and is taken out, with steaming
Distilled water rinses 3min post-dryings；Cleaning fluid is distilled water：Acetone：Isobutanol=1：1：1 mixed solution；
1.4th, ultra-hydrophilic surface is prepared：Glass is put into stainless steel autoclave, butyl titanate and salt is immersed in
In the mixed solution of acid, autoclave is reacted into 10h in the baking oven that temperature is 135 DEG C, then taken out in glass, with distillation
Water rinses 10min post-dryings, and glass surface now has super hydrophilic interface performance；
The 2nd, 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
It is changed into the glass surface of super-hydrophobic interface performance；Sputtering the method for cadmium telluride is：Cadmium telluride target is put into magnetic control sputtering device true
On radio frequency platform in empty room；The glass of super hydrophilic interface performance is positioned on sample stage；Adjust sample stage and radio frequency platform away from
From d=90mm；To vacuum chamber, the vacuum in vacuum room is set to reach 8.0 × 10- 4Pa；Super hydrophilic interface performance
Glass is heated to 65 DEG C；Argon gas is filled with vacuum chamber, and ar pressure is adjusted to 2.0Pa；Apply radio-frequency current 30mA, penetrate
Frequency voltage-regulation is 0.30kV；Sedimentation time is 10min, then naturally cools to room temperature, and glass surface now is with super thin
Water termination performance；
3rd, super-hydrophobic glass surface is changed into super hydrophilic：
By the cadmium telluride for removing the glass surface for sputtering at super hydrophilic interface performance, super-hydrophobic glass surface is changed
For super hydrophilic glass surface；The method of removal is：The glass of super-hydrophobic interface performance is positioned in high temperature rapid thermal annealing stove, plus
Hot temperature is 700 DEG C, and then temperature retention time 25min naturally cools to room temperature, and glass surface now 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 in glass surface
The different nanometer layer of growth, realizes the super hydrophilic and super-hydrophobic controllable inversion of glass surface, and step is as follows：
1.1st, realize that glass surface is super hydrophilic：
One layer of TiO2 monodimension nano stick array is grown in glass surface, makes glass surface that there is super hydrophilic interface performance；Growth
The method of TiO2 monodimension nano stick arrays is：
1.1.1, hydrochloric acid solution is prepared：By the 30% of deionized water and equivalent mixed in hydrochloric acid, hydrochloric acid solution is obtained, in atmosphere
Stirring at least 1min；
1.1.2 the mixed solution of butyl titanate and hydrochloric acid, is prepared：Butyl titanate, the fourth of metatitanic acid four are added in 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 the butyl titanate for obtaining and hydrochloric acid
Solution is put into stainless steel autoclave；
1.1.3, glass is cleaned：Glass is put into the ultrasonic cleaner equipped with cleaning fluid to clean after at least 30min and is taken out, used
Distilled water flushing at least 1min post-dryings；Cleaning fluid is distilled water：Acetone：Isobutanol=1：1：1 mixed solution；
1.1.4, ultra-hydrophilic surface is prepared：Glass is put into stainless steel autoclave, butyl titanate and hydrochloric acid is immersed in
Mixed solution in, autoclave is reacted at least 8h in the baking oven that temperature is 135 DEG C, then glass is taken out, with steaming
Distilled water rinses at least 1min post-dryings, and glass surface now has super hydrophilic interface performance；
The 1.2nd, 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；Sputtering the method for 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 positioned on sample stage；Sample stage is adjusted with radio frequency platform apart from d=
60mm～120mm；To vacuum chamber, the vacuum in vacuum room is set 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；Be filled with argon gas in vacuum chamber, and by ar pressure adjust 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 naturally cools to room temperature, and glass surface now has super-hydrophobic interface performance；
1.3rd, super-hydrophobic glass surface is changed into super hydrophilic：
By the cadmium telluride for removing the glass surface for sputtering at super hydrophilic interface performance, super-hydrophobic glass surface is changed into super
Hydrophilic glass surface；The method of removal is：The glass of super-hydrophobic interface performance is positioned in high temperature rapid thermal annealing stove, heating temperature
Spend for 600 DEG C～800 DEG C, then temperature retention time at least 20min naturally cools to room temperature, glass surface now reverts to super
Hydrophilic interface performance.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611179426.3A CN106630677B (en) | 2016-12-19 | 2016-12-19 | A method of realizing the super hydrophilic and super-hydrophobic controllable inversion of glass surface |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611179426.3A CN106630677B (en) | 2016-12-19 | 2016-12-19 | A method of realizing the super hydrophilic and super-hydrophobic controllable inversion of glass surface |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106630677A true CN106630677A (en) | 2017-05-10 |
| CN106630677B CN106630677B (en) | 2019-06-04 |
Family
ID=58833781
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611179426.3A Active CN106630677B (en) | 2016-12-19 | 2016-12-19 | A method of realizing the super hydrophilic and super-hydrophobic controllable inversion of glass surface |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106630677B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108707871A (en) * | 2018-05-25 | 2018-10-26 | 西安交通大学 | A kind of preparation method of the metal/non-metal laminated film with superhydrophobic characteristic |
| CN108751738A (en) * | 2018-06-01 | 2018-11-06 | 合肥学院 | Bi2S3/TiO2Composite material nano rod array and preparation method thereof |
| WO2018205813A1 (en) * | 2017-05-12 | 2018-11-15 | 京东方科技集团股份有限公司 | Anti-fogging film, anti-fogging component, adjustment method therefor, and vehicle-mounted device |
| CN110180496A (en) * | 2019-06-06 | 2019-08-30 | 济南大学 | Light-weight inorganic particle surface loads the preparation method of the reversible oil slick recovery catalyst of rodlike titanium dioxide array |
| CN115231827A (en) * | 2022-09-13 | 2022-10-25 | 中国科学院长春光学精密机械与物理研究所 | Transparent glass with convertible wettability |
Citations (4)
| 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 |
-
2016
- 2016-12-19 CN CN201611179426.3A patent/CN106630677B/en active Active
Patent Citations (4)
| 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 |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018205813A1 (en) * | 2017-05-12 | 2018-11-15 | 京东方科技集团股份有限公司 | Anti-fogging film, anti-fogging component, adjustment method therefor, and vehicle-mounted device |
| US11644601B2 (en) | 2017-05-12 | 2023-05-09 | Chengdu Boe Optoelectronics Technology Co., Ltd. | Anti-fogging film, anti-fogging component, adjustment method therefor, and vehicle-mounted device |
| CN108707871A (en) * | 2018-05-25 | 2018-10-26 | 西安交通大学 | A kind of preparation method of the metal/non-metal laminated film with superhydrophobic characteristic |
| CN108751738A (en) * | 2018-06-01 | 2018-11-06 | 合肥学院 | Bi2S3/TiO2Composite material nano rod array and preparation method thereof |
| CN110180496A (en) * | 2019-06-06 | 2019-08-30 | 济南大学 | Light-weight inorganic particle surface loads the preparation method of the reversible oil slick recovery catalyst of rodlike titanium dioxide array |
| CN110180496B (en) * | 2019-06-06 | 2022-01-25 | 济南大学 | Preparation method of reversible floating oil recovery agent with rod-shaped titanium dioxide array loaded on surface of light inorganic particle |
| CN115231827A (en) * | 2022-09-13 | 2022-10-25 | 中国科学院长春光学精密机械与物理研究所 | Transparent glass with convertible wettability |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106630677B (en) | 2019-06-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106630677B (en) | A method of realizing the super hydrophilic and super-hydrophobic controllable inversion of glass surface | |
| CN101962769B (en) | Method for preparing hydrophobic film on surface of material | |
| EP2671970A1 (en) | A method for depositing crystalline titania nanoparticles and films | |
| CN110804395B (en) | Anti-icing coating, anti-icing material and preparation method thereof | |
| CN103981488A (en) | Method for preparing vanadium oxide nanoparticle array by rapid heat treatment | |
| CN106733555B (en) | Super-hydrophobic surface capable of controlling rebound direction of impact liquid drops and construction method thereof | |
| CN112030108B (en) | Organic-metal nano composite film and preparation method and application thereof | |
| Mamedov et al. | Enhanced hydrophobicity of CeO2 thin films: Role of the morphology, adsorbed species and crystallography | |
| Lee et al. | Large-area sodium titanate nanorods formed on titanium surface via NaOH alkali treatment | |
| CN107190235B (en) | A kind of preparation method of pulse laser deposition that realizing a variety of vanadium dioxide low dimensional structures | |
| CN101139701B (en) | Method for preparing silicon-based rutile phase TiO2 film by pulsed laser deposition | |
| CN106167892B (en) | A kind of bimetallic/ceramic composite film and preparation method thereof | |
| CN114799532B (en) | Method for preparing high-quality amorphous alloy micro-pits by combining laser irradiation with wax sealing polishing | |
| CN1298883C (en) | Ag/TiO2 composite film with adjustable contact angle and preparation method thereof | |
| CN107393977B (en) | A kind of ultra wide band antireflective film and preparation method thereof | |
| CN104975291A (en) | Device and method for preparing bismuth ferrite film and preparation method of solar cell | |
| Portella et al. | Nanostructured titanium film deposited by pulsed plasma magnetron sputtering (Pdms) on a high voltage ceramic insulator for outdoor use | |
| CN112047327B (en) | Preparation method of three-dimensional vertical graphene | |
| CN101139702B (en) | Method for preparing silicon-based octahedrite phase TiO2 film by pulsed laser deposition | |
| CN112239853B (en) | Preparation method of micro-nano structure film with durable super-hydrophilic characteristic | |
| Liu et al. | A superhydrophobic photothermal carbon black-coated waste face mask for efficient water desalination | |
| Peng et al. | Influence of annealing temperature on the properties of TiO2 films annealed by ex situ and in situ TEM | |
| CN107254657B (en) | A kind of sodium tetraborate catalysis oxidation preparation array-like TiO of pure Ti2Method | |
| CN114685844A (en) | Preparation method of efficient oil-water separation sponge | |
| Wang et al. | Fabrication of TiO2 films on glass substrates by a pulsed dc reactive magnetron sputtering |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |