CN109338304A - A kind of transparent hydrophobic film, preparation method and application - Google Patents
A kind of transparent hydrophobic film, preparation method and application Download PDFInfo
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- CN109338304A CN109338304A CN201811297045.4A CN201811297045A CN109338304A CN 109338304 A CN109338304 A CN 109338304A CN 201811297045 A CN201811297045 A CN 201811297045A CN 109338304 A CN109338304 A CN 109338304A
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
- C23C14/5853—Oxidation
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Abstract
The present invention relates to a kind of transparent hydrophobic film, preparation method and applications, transparent hydrophobic film includes zinc-oxide film and is supported on the thickness of transparent hydrophobic film described in the hexadecyl trimethoxy silane film of zinc oxide films film surface in 500 ~ 1000nm, visible light transmittance rate is 50 ~ 90%, contact angle with water is at 165 ° or more, and the roll angle with water is at 2 ° or less.Preparation method includes S1 using the progress zinc film preparation of rf magnetron sputtering system, then carries out the processing of zinc Thin-film anneal, obtains zinc-oxide film；S2 carries out moditied processing to the zinc-oxide film that S1 is obtained, and obtains transparent hydrophobic film.Transparent hydrophobic film is used for external wall, glass for vehicle window, photoelectric device or optical device.The surface of the transparent hydrophobic film has nano bar-shape structure, has excellent ultra-hydrophobicity, light transmission, self-cleaning performance and anti-fog performance, and the translucency of glass surface under sleet, foggy weather can be improved and reduce glass surface contamination.
Description
Technical field
The present invention relates to transparent hydrophobic film manufacturing techniques fields, and in particular to a kind of transparent hydrophobic film is based on
Magnetron sputtering technique prepares the method for transparent hydrophobic film and the application of transparent hydrophobic film.
Background technique
Because having excellent hydrophobicity performance, water droplet can tumble easily and take away dust super hydrophobic surface, therefore have
Self-cleaning performance.And transparent hydrophobic surface is due to high transparency energy, being expected in glass outer wall, vehicle glass, photovoltaic group
Automobile can be improved so that above-mentioned surface has self-cleaning performance using its excellent hydrophobicity performance in the acquisitions application such as part surface
The degree of getting a clear view of windshield, the cleaning amount for reducing glass outer wall, raising photovoltaic module surface cleaning in driving process
Degree is to improve generating efficiency.
The preparation of super hydrophobic surface needs to form the bulge-structure of micro/nano level on surface, while using the change of low-surface-energy
Learn the free energy that reagent carries out modification reduction surface.Research points out that film to be made has excellent light transmission, needs stringent
Surface bump sizes are controlled, so that its roughness is no more than the 1/4 of visible wavelength.Therefore, it is necessary to strictly control in preparation process
Make the size of surface bulge structure.On the one hand, the formation of ultra-hydrophobicity needs to form biggish roughness on surface, still
Biggish roughness can reduce light transmittance again, therefore, effectively control the size of surface bulge-structure during the preparation process, regulate and control table
Surface roughness is most important.
Traditional method for preparing transparent hydrophobic surface has sol-gel method, template, sedimentation etc..Collosol and gel
Method and sedimentation preparation process are complicated, and microscopic protrusions structure is often uncontrollable, and film-substrate cohesion is poor.Template needs preset
Template, it is difficult to large-area applications.The existing method for preparing super hydrophobic surface has the problem that 1, preparation process complexity, process
Control is harsh, and film uniformity is poor；2, film-substrate cohesion is not strong, it is difficult to be applied to the families such as external wall, vehicle glass surface
On outer matrix.
Summary of the invention
In view of the above-mentioned problems existing in the prior art, the first purpose of the invention is to provide a kind of transparent hydrophobic is thin
Film.
A second object of the present invention is to provide a kind of methods for preparing transparent hydrophobic film based on magnetron sputtering technique.
Third object of the present invention is to provide the applications of transparent hydrophobic film.
To realize above-mentioned first purpose, the present invention adopts the following technical scheme: a kind of transparent hydrophobic film, described
Bright based superhydrophobic thin films include zinc-oxide film and be supported on the zinc oxide films film surface hexadecyl trimethoxy silane it is thin
Film；The thickness of the transparent hydrophobic film in 500 ~ 1000nm, can choose 500nm, 530nm, 550nm, 580nm,
600nm、630nm、650nm、680nm、700nm、730nm、750nm、780nm、800nm、830nm、850nm、870nm、
900nm, 930nm, 950nm, 970nm or 1000nm, it is seen that light transmittance is 50 ~ 90%, can choose 50%, 60%, 62%, 65%,
68%, 70%, 72%, 75%, 78%, 80%, 82%, 85% or 90% with the contact angle of water at 165 ° or more, can select 165 °, 168 °,
170 °, 172 °, 175 ° or 178 °, with the roll angle of water at 2 ° hereinafter, specifically can choose 2 °, 1.8 °, 1.5 °, 1.2 °, 1.0 °,
0.8 ° or 0.5 °.
Hexadecyl trimethoxy silane film plays chemical modification, reduces the energy on surface, thickness is in nanoscale.
As an improvement, the thickness of the zinc-oxide film in 500 ~ 1000nm, specifically can choose 500nm, 530nm,
550nm、580nm、600nm、630nm、650nm、680nm、700nm、730nm、750nm、780nm、800nm、830nm、
850nm, 870nm, 900nm, 930nm, 950nm, 970nm or 1000nm.Inventor analyzes by test of many times and data, discovery
For thickness in the zinc-oxide film of 800-1000nm, the bulge-structure height on surface is higher, thus its cementability, wearability and
Antifog anti-icing property is more preferable, in addition, the zinc-oxide film roll angle of the restriction in the present invention is at 2 ° or less, that is to say, that water droplet is rising
Surface is easier to roll, and dynamic ultra-hydrophobicity is more preferable, and self-cleaning is more preferable.
To realize above-mentioned second purpose, the present invention adopts the following technical scheme: a kind of transparent hydrophobic film for preparing
Method, the transparent hydrophobic film are transparent hydrophobic film among the above；
Preparation step includes:
S1: zinc film preparation is carried out using rf magnetron sputtering system, the processing of zinc Thin-film anneal is then carried out, obtains zinc oxide films
Film；
S2: moditied processing is carried out to the zinc-oxide film that S1 is obtained, obtains transparent hydrophobic film.
Preferably, the step of carrying out zinc film preparation using rf magnetron sputtering system in S1 includes:
S1a: it after substrate successively to be used to acetone, deionized water and dehydrated alcohol ultrasonic cleaning, is then dried；
S1b: under normal temperature condition, clean substrate being fixed in magnetron sputtering plating chamber, opens magnetron sputtering apparatus, is taken out true
Sky, using zinc target as sputtering source, argon gas does not add other reaction gas as working gas, after target pre-sputtering, opens baffle
Plated film is carried out, deposition obtains the zinc film for being supported on upper surface of substrate.Substrate can choose simple glass, k9 glass, be coated with increasing
Any one in the transparent bases such as the glass of permeable membrane, the glass for being coated with conductive film, the simple glass for being coated with electro-conductive glass.
As an improvement, successively vacuum degree is taken out down to 4 × 10 using mechanical pump and molecular pump in the S1b-3Pa, work gas
Body pressure specifically can choose 0.5Pa, 0.8Pa, 1.0Pa, 1.1Pa, 1.2Pa or 1.5Pa to 0.5 ~ 1.5Pa, and radio-frequency power is
150 ~ 170w specifically can choose 150W, 152W, 155W, 158W, 160W, 162W, 165W, 168W or 170W, sputtering time
(or sedimentation time) 1 ~ 15min, specifically can choose 1min, 2min, 3min, 4min, 5min, 6min, 7min, 7.5min,
8min, 9min, 10min, 11min, 12min, 13min, 14min or 15min,.That is sputtering condition, vacuum degree are extracted into 4x10-3Pa
Hereinafter, Ar is sputter gas, 0.5 ~ 1.5Pa of sputtering pressure, 1 ~ 15min of sputtering time.It is subsequently passed nitrogen, takes out sample after cooling
Product.Inventor analyzes by test of many times and data, and discovery is only when vacuum degree is taken out down to 4 × 10-3When Pa or less, could to the greatest extent may be used
Reduce influence of the remaining air plankton to transparent hydrophobic film in magnetron sputtering plating chamber in energy ground.
The present invention does not need to heat during preparing zinc film, while not needing to be passed through oxygen yet and be aoxidized, because
Sedimentation time in this present invention is very short, as long as 1-5min.
As an improvement, the step of zinc Thin-film anneal is handled in S1 is S1c: will be using the zinc of rf magnetron sputtering system preparation
It after film sample takes out, is put into Muffle furnace by room temperature to 400 DEG C of annealing 30min or more, so that the Thin-film anneal of sputtering
It is oxidized to stable oxide, then natural cooling.
As an improvement, the Muffle furnace is 10 DEG C/min by the heating rate of room temperature to 400 DEG C.The present invention is in Muffle
It disposably anneals in furnace to zinc film, zinc is all oxidized to stable zinc oxide.
The present invention is not heated in zinc film preparation, obstructed oxygen, directly zinc target is used to be sputtered as sputtering source,
Therefore the sedimentation time needed is short；In annealing, the present invention is directly heated zinc film sample to 400 DEG C by room temperature, is being annealed
Zinc is disposably oxidized to stable zinc oxide in the process, annealing process is easier to control, and zinc oxidation is more thorough.
As an improvement, the S2 carries out moditied processing process to zinc-oxide film are as follows: by obtained zinc-oxide film normal
Under temperature, condition of normal pressure, 30min is modified using the alcohol solution dipping of the hexadecyl trimethoxy silane of 2wt.%.It spontaneously dries
Afterwards.Decorating liquid is also an option that other fluorination class dressing agents.
The zinc-oxide film modification step that the present invention limits is very simple, and modification condition is room temperature and normal pressure, does not need to take out
Vacuum does not need to heat yet, it is only necessary to which then the hexadecyl trimethoxy silane solution for configuring 2wt.% soaks zinc-oxide film
Bubble modification 30min, modification step control is simple, and the quality of end product more preferably guarantees.
To realize above-mentioned third purpose, the present invention adopts the following technical scheme: above-mentioned transparent hydrophobic film is for building
Build exterior wall, glass for vehicle window, photoelectric device or optical device.
Compared with the existing technology, the present invention at least has the advantages that
1, the surface of transparent hydrophobic film provided by the invention has nano bar-shape structure, with excellent ultra-hydrophobicity and
Light transmission, while also there is excellent anti-fog performance, the light transmission of the glass surface under sleet, foggy weather can be significantly improved
Property.
2, transparent hydrophobic film provided by the invention has excellent acid-alkali-corrosive-resisting characteristic, to the acid & alkali liquid of pH1 ~ 13
Body all has excellent ultra-hydrophobicity.
3, transparent hydrophobic surface provided by the invention has excellent height temperature stability, in -20 DEG C ~ 100 DEG C situations
Under all have excellent super-hydrophobic stability.
4, the present invention, which provides transparent hydrophobic surface, has the excellent impact characteristics of resistance to high velocity water droplets, impacts in high velocity water droplets
Under still maintain ultra-hydrophobicity.
5, the method that present invention offer prepares transparent hydrophobic film based on magnetron sputtering technique is reliable, simple, while magnetic
Control sputtering method can large-area applications, have promotional value.
Detailed description of the invention
Fig. 1 is shape of the water droplet on different surfaces.
Fig. 2 is the pattern of transparent hydrophobic film prepared by embodiment 1, and (a) and (b) is the saturating of the preparation of embodiment 1 respectively
Surface topography map of the bright based superhydrophobic thin films under different amplification, (c) and (d) is that transparent hydrophobic prepared by embodiment 1 is thin
Cross-section diagram of the film under different amplification.
Fig. 3 is the self-cleaning performance test of transparent hydrophobic film prepared by embodiment 1.
Fig. 4 is different pH value water droplets form on the surface of transparent hydrophobic film attachment prepared by embodiment 1.
Fig. 5 is the surface of transparent hydrophobic film attachment prepared by embodiment 1 under different conditions of storage, the change of performance
Change.
When Fig. 6 is the surface of transparent hydrophobic film attachment prepared by friction speed droplets impact embodiment 1, the shape of water droplet
State.
Fig. 7 is that the translucency that the transparent hydrophobic film prepared to embodiment 1 carries out is tested.
Fig. 8 is influence of the sputtering time to transparent hydrophobic film contacts angle and roll angle.
Fig. 9 is influence of the sputtering time to transparent hydrophobic film thickness and roughness.
Figure 10 is influence of the sputtering time to the light transmittance in transparent hydrophobic film visible-range.
Specific embodiment
Invention is further described in detail below.
The present invention uses magnetron sputtering technique, due to being covalently bonded between atom between the substrates such as the particle of sputtering and glass
Conjunction mode, higher than the hydrogen bond and Van der Waals force between general coating and substrate, therefore, the film that magnetron sputtering is prepared has
Excellent film-substrate cohesion.In addition, magnetron sputtering preparation method is simple, preparation process is reliable, reproducible.And it is splashed by control
Emanating atmosphere, sputtering pressure and sputtering power can be with the size and length of the bulge-structure size of Effective Regulation coating surface, in turn
Any regulation surface roughness, may be implemented the Effective Regulation to coating ultra-hydrophobicity and translucency.
For the present invention using metal targets such as magnetron sputtering Zn, deposition rate is high, can quickly sputter acquisition film, lead to simultaneously
The hexagonal wurtzite structure zinc oxide being preferentially inclined to c-axis is formd after crossing annealing, advantageously forms surface roughness.
This method can solve the problem of the film-substrate cohesion difference on transparent hydrophobic surface, while pass through regulation preparation parameter, Ke Yiyou
Effect adjusts surface roughness, convenient to regulate and control to ultra-hydrophobicity and light transmission.Preparation method has reliable, simple, easy
In the advantage of large-area applications.
Embodiment 1: a method of transparent hydrophobic film being prepared, preparation step includes:
S1: zinc film preparation is carried out using rf magnetron sputtering system, the processing of zinc Thin-film anneal is then carried out, obtains zinc oxide
Film；
S1a: it after substrate successively to be used to acetone, deionized water and dehydrated alcohol ultrasonic cleaning, is then dried；
S1b: under normal temperature condition, clean substrate being fixed in magnetron sputtering plating chamber, opens magnetron sputtering apparatus, is taken out true
Sky, using zinc target as sputtering source, argon gas does not add other reaction gas as working gas, after target pre-sputtering, opens baffle
Plated film is carried out, deposition obtains the zinc film for being supported on upper surface of substrate；Sputtering condition are as follows: vacuum degree is taken out down to 4 × 10-3Pa, work
Make gas pressure intensity 1.5Pa, radio-frequency power 150w, sputtering time 2min.
S1c: it after being taken out using the zinc film sample of rf magnetron sputtering system preparation, is put into Muffle furnace by room temperature liter
Temperature is to 400 DEG C of annealing 30min or more, so that the Thin-film anneal of sputtering is oxidized to stable oxide, then natural cooling.
S2: moditied processing is carried out to the zinc-oxide film that S1 is obtained, the zinc-oxide film that S1c is obtained is in room temperature, normal pressure
Under the conditions of, 30min is modified using the alcohol solution dipping of the hexadecyl trimethoxy silane of 2wt.%, obtains transparent hydrophobic
Film.
Referring to Fig. 1, the pore in figure in a-quadrant indicates water droplet when on the transparent hydrophobic film that embodiment 1 obtains
Form, the pore in B area indicates form when water droplet only passes through on the glass surface of moditied processing, small in the region C
Point indicates form of water droplet when on untreated glass surface.It is not difficult to find out that water droplet in a-quadrant in spherical, illustrates transparent
The super-hydrophobic effect of based superhydrophobic thin films is very good, and is clear that the text of super hydrophobic surface bottom, and light transmittance is very
It is good.Spherical crown shape is presented in water droplet on the glass surface for only passing through moditied processing, and contact angle is about 95o.And water droplet is in untreated glass
Hydrophily is presented in glass surface, and adherency is on the glass surface.
Figure (a) and figure (b) in referring to fig. 2, from surface topography as can be seen that foring nano bar-shape under magnification at high multiple
Structure protrusion, effectively increases the roughness on surface, and conducive to ultra-hydrophobicity is formed, the nano bar-shape structure that is formed simultaneously can be with
Significantly improve the frosting resistance/anti-icing performance on the transparent hydrophobic surface.Figure (c) and figure (d) in referring to fig. 2, from cross-section diagram
As can be seen that the thickness of coating is about in 700 ~ 900nm, nano particle is piled up on the glass surface, coating bottom and substrate of glass
Fine and close adhesive layer is formed, there is excellent film-substrate cohesion.Simultaneously it can be seen that a spherical (Fig. 2 is presented on surface in water droplet
The upper right corner of middle figure (a)), show excellent ultra-hydrophobicity.
Self-cleaning performance test:
It is sprinkled upon on sample surfaces with pollutants pavings such as nano carbon black simulation dust.10 microlitres of water droplet is dropped into super-hydrophobic sample
When surface, water droplet can roll on super hydrophobic surface, while take away the carbon black impurity on rolling path, show excellent surpass
Hydrophobic performance and self-cleaning performance
Referring to Fig. 3, tilted-putted sample, in the small figure in the lower right corner, left side half is simple glass, and right side half be to prepare
Super-hydrophobic sample, it can be seen that when being tilted a certain angle, when 10 microlitres of water droplets drop onto left side surface of ordinary glass, water droplet
It cannot roll, can only be immersed in carbon black impurity layer, not have self-cleaning performance.And water droplet rolls down to the super-hydrophobic sample table in right side
When face, water droplet can tumble easily and take away the impurity such as carbon black, show excellent water droplet spring dynamic property and self-cleaning property
Energy.Make in this way the super hydrophobic surface application outdoors when, can outdoors raindrop the effects of under clean surface, have it is excellent
Self-cleaning performance.
Referring to fig. 4, it can be seen that water droplet pH value in 1 ~ 13(be acid water droplet and alkaline water droplet) under, with embodiment 1
The contact angle on the surface of the transparent hydrophobic film attachment of preparation is all larger than 155 °, and it is excellent to illustrate that transparent hydrophobic film has
Acid-alkali-corrosive-resisting stability.
Referring to Fig. 5, it can be seen that the surface of transparent hydrophobic film attachment prepared by embodiment 1 is at -20 DEG C ~ 100 DEG C
After storage for 24 hours, the contact angle on water droplet and based superhydrophobic thin films surface is still greater than 165 °, and it is excellent to illustrate that transparent hydrophobic film has
High temperature resistant and low-temperature stability.
Referring to Fig. 6, it can be seen that speed is respectively the saturating of the preparation of droplets impact embodiment 1 of 0.44,1.98 and 2.8m/s
When the surface of bright based superhydrophobic thin films attachment, it can rebound and leave super hydrophobic surface, it is excellent to illustrate that transparent hydrophobic film has
Resistance to high velocity water droplets impact stability.
Referring to Fig. 7, with the glass surface and common glass of transparent hydrophobic film attachment prepared by humidifier sprinkling embodiment 1
Glass surface, the glass surface that discovery vapor will not adhere in transparent hydrophobic film condense, the attachment of transparent hydrophobic film
Text below glass surface is still clear, and the glass surface of transparent hydrophobic film attachment has excellent light transmission；And
Surface of ordinary glass has adhered to many droplets, affects the translucency of glass surface, cannot see that the text below glass.
Embodiment 2-4 is identical as the preparation process of embodiment 1, the difference is that only the selection of sputtering condition, specifically such as
Table 1
Table 1
| Sputtering time (min) | Vacuum degree (pa) | Working gas pressure (Pa) | Radio-frequency power (w) | |
| Embodiment 2 | 0 | 4×10-3Pa | 1.5 | 150 |
| Embodiment 3 | 7.5 | 4×10-3Pa | 1.5 | 150 |
| Embodiment 4 | 15 | 4×10-3Pa | 1.5 | 150 |
In order to save length, the performance test data of transparent hydrophobic film prepared by embodiment 2-4 are not included in.
The transparent good hydrophobic surface of this method preparation, in addition to being had with excellent ultra-hydrophobicity and light transmission
Excellent film-substrate cohesion make it have an outdoor application condition, excellent acid-proof alkaline, resistance to height cryogenic property and resistance to
High velocity water droplets impact equistability makes its excellent enduring quality with outdoor application.
It prepared transparent hydrophobic surface can be with large-area applications in external wall, lathe glass, photovoltaic group
Part etc., has broad application prospects.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to skill of the invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered at this
In the scope of the claims of invention.
Claims (9)
1. a kind of transparent hydrophobic film, it is characterised in that: the transparent hydrophobic film includes zinc-oxide film and is supported on
The hexadecyl trimethoxy silane film of the zinc oxide films film surface
The thickness of the transparent hydrophobic film is in 500 ~ 1000nm, it is seen that light transmittance is 50 ~ 90%, is existed with the contact angle of water
165°
More than, the roll angle with water is at 2 ° or less.
2. transparent hydrophobic film as described in claim 1, it is characterised in that: the thickness of the zinc-oxide film 500 ~
1000nm 。
3. a kind of method for preparing transparent hydrophobic film, it is characterised in that: the transparent hydrophobic film be claim 1 or
Transparent hydrophobic film in 2；Preparation step includes:
S1: zinc film preparation is carried out using rf magnetron sputtering system, the processing of zinc Thin-film anneal is then carried out, obtains zinc oxide
Film；
S2: moditied processing is carried out to the zinc-oxide film that S1 is obtained, obtains transparent hydrophobic film.
4. the method for preparing transparent hydrophobic film as claimed in claim 3, it is characterised in that: splashed in S1 using radio frequency magnetron
Penetrating the step of system carries out zinc film preparation includes:
S1a: it after substrate successively to be used to acetone, deionized water and dehydrated alcohol ultrasonic cleaning, is then dried；
S1b: under normal temperature condition, clean substrate being fixed in magnetron sputtering plating chamber, opens magnetron sputtering apparatus, is taken out
Vacuum, using zinc target as sputtering source, argon gas does not add other reaction gas as working gas, after target pre-sputtering, beats
It opens baffle and carries out plated film, deposition obtains the zinc film for being supported on upper surface of substrate.
5. the method for preparing transparent hydrophobic film as described in claim 3 or 4, it is characterised in that: successively adopted in the S1b
Vacuum degree is taken out down to 4 × 10 with mechanical pump and molecular pump-3Pa, working gas pressure to 0.5 ~ 1.5Pa, radio-frequency power be 150 ~
170w, 1 ~ 15min of sputtering time.
6. the method for preparing transparent hydrophobic film as claimed in claim 5, it is characterised in that: zinc Thin-film anneal is handled in S1
The step of be S1c: by using rf magnetron sputtering system preparation zinc film sample take out after, be put into Muffle furnace by room temperature liter
Temperature is to 400 DEG C of annealing 30min or more, so that the Thin-film anneal of sputtering is oxidized to stable oxide, then natural cooling.
7. the method for preparing transparent hydrophobic film as claimed in claim 6, it is characterised in that: the Muffle furnace is by room temperature liter
The heating rate of temperature to 400 DEG C is 10 DEG C/min.
8. the method for preparing transparent hydrophobic film as claimed in claim 7, it is characterised in that: the S2 is to zinc-oxide film
Carry out moditied processing process are as follows: by obtained zinc-oxide film under room temperature, condition of normal pressure, using the cetyl three of 2wt.%
The alcohol solution dipping of methoxy silane modifies 30min.
9. the application of transparent hydrophobic film as claimed in claim 1 or 2, it is characterised in that: the transparent hydrophobic film
For external wall, glass for vehicle window, photoelectric device or optical device.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112067604A (en) * | 2019-08-01 | 2020-12-11 | 杭州博拓生物科技股份有限公司 | Detection device |
| CN114408852A (en) * | 2020-10-13 | 2022-04-29 | 天津工业大学 | Hydrophobic antireflection novel micro-nano structure CaF2Film and preparation method thereof |
-
2018
- 2018-11-01 CN CN201811297045.4A patent/CN109338304A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112067604A (en) * | 2019-08-01 | 2020-12-11 | 杭州博拓生物科技股份有限公司 | Detection device |
| CN114408852A (en) * | 2020-10-13 | 2022-04-29 | 天津工业大学 | Hydrophobic antireflection novel micro-nano structure CaF2Film and preparation method thereof |
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