CN109320097A - A kind of preparation method on the novel oiling superslide surface based on sol-gel method - Google Patents
A kind of preparation method on the novel oiling superslide surface based on sol-gel method Download PDFInfo
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- CN109320097A CN109320097A CN201811000850.6A CN201811000850A CN109320097A CN 109320097 A CN109320097 A CN 109320097A CN 201811000850 A CN201811000850 A CN 201811000850A CN 109320097 A CN109320097 A CN 109320097A
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- 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
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- 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
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
-
- 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
-
- 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
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention belongs to porous oiling superslide coat preparing technology field, in particular to the preparation method on a kind of novel oiling superslide surface based on sol-gel method.The present invention include on glass slide spin coating by colloidal sol that silane and silica are formed to construct the porous rough surface of reticular structure covering, then perfluoropolyether is added dropwise, prepares the superslide surface with lyophoby property.The superslide surface exhibits go out excellent lyophoby property, and water droplet and various organic matter drops all have minimum slide angle and contact angle hysteresis on the surface.In addition the magnetic droplet being added dropwise on the surface can clear up the spot for being scattered in surface in the case where adding field drives outside during moving freely.The surface also has the characteristics that good freezing, the anti-fog, high grade of transparency during lyophoby in addition to the automatically cleaning on achievable surface.
Description
Technical field
The invention belongs to porous oiling superslide coat preparing technology field, in particular to prepare with automatically cleaning, freezing,
The method of the coating suitable for various substrates of the features such as anti-fog.
Background technique
The preparation on the superslide surface of porous oiling is the row for being inspired and eating meat type common nepenthes catching small animal in the Nature
For.The colored ligule of this kind of plant is made of the hydrophilic component with micro-rough structure, and surface is easily spontaneously wet out by water and stores up
It deposits liquid water and forms water membrane, the toy for resting on surface is made to slide into the digestive system of bottom.It is constructed on matrix surface
The coarse structure similar with common nepenthes surface texture simultaneously pours into suitable lubricating oil and can prepare superslide surface.Prepared by artificial
Superslide surface has very wide application prospect in the fields such as liquid transporting, anti-pollution, anticorrosive, freezing.
The good lyophoby characteristic in surface can be realized by injecting organic lubricating oil in artificial superslide surface.The characteristic can make
From the pollution of greasy filth, surface can be applied to the fields such as liquid transporting, food packaging by this on superslide surface；The characteristic is also assigned
Giving the characteristics such as surface freezing, anti-fog allows surface by prolonged application in low temperature environment.Based on sol-gal process preparation
Superslide surface can improve the service life on surface very firmly by lubricating oil lock in the coarse structure on surface.Ultraviolet no shadow
The gel formed by colloidal sol is adhere strongly on matrix by the introducing of glue, this can not only increase substantially the resistance to of superslide surface
The translucency on superslide surface is not influenced also with property.
Summary of the invention
The object of the present invention is to provide the preparations that a kind of easy, efficient preparation has the superslide surface of good lyophoby property
Method.Ultraviolet shadowless glue and three-dimensional netted sol solution are spun on matrix using simple and easy spin coating method.Drop
All there is lesser slide angle and contact angle hysteresis on the surface filled after oil, and surface has preferable automatically cleaning, freezing
Etc. characteristics.
Realizing the technical solution of the object of the invention is: a kind of system on the novel oiling superslide surface based on sol-gel method
Preparation Method, which comprises the steps of:
A. early-stage preparations are tested: when glass slide being cropped to suitable size and being cleaned by ultrasonic one section inside organic solvent
Between, it is subsequently placed into baking oven and is dried for standby；
B. prepared by colloidal sol: by a certain amount of tetraethoxysilane TEOS, vinyltriethoxysilane VTES, perfluoro capryl
Triethoxysilane PFAS, silica SiO2It is scattered in a certain amount of normal propyl alcohol NPA, then dripped during magnetic agitation
Add a certain amount of distilled water and acetum HAc, hydrolysis for a period of time after, sol solution can be obtained and save stand-by；
The tetraethoxysilane TEOS, vinyltriethoxysilane VTES, perfluoro capryl triethoxysilane PFAS, titanium dioxide
Silicon SiO2, normal propyl alcohol NPA, distilled water and acetum HAc use mass percent match are as follows: 4.5%:7.6%:3%:
1.2%:30.2%:51.8%:1.7%；
C. prepared by superslide surface: loaded on spin coater clean glass slide and a certain amount of ultraviolet shadowless glue of spin coating,
Sol solution simultaneously carries out ultraviolet light and heat treatment to glass slide, then, a certain amount of perfluoropolyether is circulated into prepared
The glass slide containing gel on, superslide surface can be obtained.
Further, the long and wide size of the glass slide is 25 × 20cm.
Further, the hydrolysis forms the reaction time of colloidal sol as 12h.
Further, ultraviolet shadowless glue and the dosage of sol solution are all 1ml when the spin coating.
Further, the ultraviolet light processing time is 5min.
Further, the heat treatment temperature and time are respectively as follows: 100 DEG C, 30min.
Further, the method also includes step D. lyophoby performance tests: prepared superslide surface is placed in contact
On angle tester, the various drops of certain volume are added dropwise respectively to measure the contact angle and slide angle of various liquids, in addition,
Different spot drops is dripped to the automatically cleaning process on surface and recording and analyzing surface；For testing superslide surface lyophoby characteristic
Various dropping liquids include: one or more of distilled water, ethylene glycol, dimethyl sulfoxide, toluene, chlorotoluene, isooctane.
Further, the method also includes step D: the magnetic particle surface of Magnetic driving decontaminates experiment: will be by ethylene glycol
The magnetic droplet for dispersing ferroso-ferric oxide and being formed is added drop-wise on superslide surface, and is spilt on some powdered graphites to surface at random,
Then powdered graphite is wrapped in inside drop during surface moves freely in the driving magnetic drop of externally-applied magnetic field,
Achieve the purpose that clean surface.
The beneficial effects of the present invention are: compared with the prior art, the advantages of the present invention are as follows:
1. preparation method is simple, easy.
2. the superslide surface of preparation has preferable lyophoby characteristic.
3. the colloidal sol of preparation is suitable for various clean matrixes.
4. surface mechanical strength is big, adhesive force is strong, long service life.
5. superslide surface has both anti-pollution, freezing, anti-fog characteristic simultaneously.
Detailed description of the invention
Fig. 1 is the Fourier transform infrared spectroscopy (a) and x-ray photoelectron spectroscopy of gained colloidal sol in the embodiment of the present invention 1
(b)。
Fig. 2 is the atom grain microscope figure of gained hydrophobic surface electron microscope and oiling front and rear surfaces in the embodiment of the present invention 1,
(a) it is amplification 10000 times and 1000 times of electron microscopes, is (b) three-dimensional surface shape figure before oiling, (c) is the rear surface of oiling
Three-dimensional appearance figure.
Fig. 3 is contact angle of the water droplet in the slide surface before and after oiling in the embodiment of the present invention 1, and (a) water droplet is pure
Contact angle on glass, (b) water droplet has the contact angle of sol surface in spin coating, and (c) water droplet is in the contact angle on superslide surface, (d) water
Drip advancing angle and receding angle on superslide skewed surface.
Fig. 4 is contact angle and roll angle of the various organic matters on superslide surface in the embodiment of the present invention 1, (a) various drops
Contact angle and slide angle histogram on superslide surface, (b) contact angle of the various drops on superslide surface.
Fig. 5 is the automatically cleaning pictorial diagram on superslide surface in the embodiment of the present invention 2, (a) oiling surface and non-oiling surface point
It is not dipped vertically into 1-60 rear surface automatically cleaning figure of milk soln, (b) milk droplets on the superslide surface that inclination angle is 3 °
Sliding figure, (c) oiling surface and non-oiling surface, which are respectively perpendicular, is immersed in honey, coffee, the automatically cleaning in tomato juice solution
Comparison diagram.
Fig. 6 is the reality that magnetic droplet voluntarily removes superslide surface blot under extraneous field drives in the embodiment of the present invention 3
Object figure.
Fig. 7 is the pictorial diagram of surface freezing under -10 DEG C of low temperature in the embodiment of the present invention 4, and (a) water droplet is on oiling surface
The icing pictorial diagram on non-oiling surface, (b) histogram on oiling surface and non-oiling surface icing delay time.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.Those skilled in the art can make various modifications or changes to the present invention, these
Within the scope of equivalent form equally claims listed by the application limit.
Embodiment 1
(1) tests early-stage preparations:
Glass slide is cropped to 25 × 20cm size and is cleaned by ultrasonic a period of time inside ethyl alcohol and acetone mixture, with
After be put into baking oven and be dried for standby.
(2) prepared by colloidal sol:
By 2.25g tetraethoxysilane (TEOS), 3.8g vinyltriethoxysilane (VTES), 1.5g perfluoro capryl
Triethoxysilane (PFAS), 0.6g silica (SiO2) be scattered in 15.1g normal propyl alcohol (NPA), then in magnetic agitation
25.9g distilled water and 0.85g acetum (HAc) are added dropwise in the process.After hydrolysis 12h, sol solution can be obtained and protect
It deposits stand-by.
(3) prepared by superslide surface:
Clean glass slide and the ultraviolet shadowless glue of spin coating 1ml, 1ml sol solution and to glass slide are loaded on spin coater
Carry out ultraviolet light 5min and 100 DEG C of heat treatment 30min.Then, the perfluoropolyether of 6 μ l prepared containing is circulated into coagulate
On the glass slide of glue, superslide surface can be obtained.
(4) lyophoby performance:
Prepared superslide surface is placed in contact angle tester, distilled water, ethylene glycol, the diformazan of 5 μ l are added dropwise respectively
Base sulfoxide, toluene, chlorotoluene, isooctane measure the contact angle and slide angle of various drops.The water droplet as shown in Fig. 3 is in pure glass
Surface, hydrophobic surface, the contact angle on superslide surface are respectively 35 ± 1 °, and 123 ± 1 °, 112 ± 1 °, water droplet is 3 ° at inclination angle
Superslide surface on advancing angle and receding angle be respectively 112 ± 1 ° and 109 ± 1 °.Ethylene glycol, dimethyl sulfoxide, toluene, chlorine
The contact angle and roll angle of toluene, isooctane on superslide surface are as shown in Figure 4.Various drops are ok on inclined superslide surface
It freely slides, but since organic drop and the polar difference of surface lubrication oil are different, so organic drop is in surface contact angle
It is had a certain difference with slide angle.
Embodiment 2
(1) tests early-stage preparations:
Glass slide is cropped to 25 × 20cm size and is cleaned by ultrasonic a period of time inside ethyl alcohol and acetone mixture, with
After be put into baking oven and be dried for standby.
(2) prepared by colloidal sol:
By 2.25g tetraethoxysilane (TEOS), 3.8g vinyltriethoxysilane (VTES), 1.5g perfluoro capryl
Triethoxysilane (PFAS), 0.6g silica (SiO2) are scattered in 15.1g normal propyl alcohol (NPA), then in magnetic agitation
25.9g distilled water and 0.85g acetum (HAc) are added dropwise in the process.After hydrolysis 12h, sol solution can be obtained and protect
It deposits stand-by.
(3) prepared by superslide surface:
Clean glass slide and the ultraviolet shadowless glue of spin coating 1ml, 1ml sol solution and to glass slide are loaded on spin coater
Carry out ultraviolet light 5min and 100 DEG C of heat treatment 30min.Then, the perfluoropolyether of 6 μ l prepared containing is circulated into coagulate
On the glass slide of glue, superslide surface can be obtained.
(4) superslide self-cleaning surface is tested:
Oiling surface and non-oiling surface are respectively perpendicular the automatically cleaning for being immersed in milk soln 1-60 times and observing surface
Ability；5 μ l milk droplets are added dropwise on the superslide surface that inclination angle is 3 ° and observe the sliding condition of drop；Oiling surface and not
Oiling surface is respectively perpendicular and is immersed in honey, coffee, in tomato juice solution and observes self-cleaning surface situation.As shown in Figure 5 a,
With pure glass phase ratio, superslide surface can keep clean surface in being immersed in milk after 60 times.The superslide surface is vertical
It is immersed in honey, catsup, the performance (5b) that lyophoby can be still played in coffee.The 5 μ l when surface is tilted 3 ° of placements
Milk droplets still can freely slide (5c) from surface.
Embodiment 3
(1) tests early-stage preparations:
Glass slide is cropped to 25 × 20cm size and is cleaned by ultrasonic a period of time inside ethyl alcohol and acetone mixture, with
After be put into baking oven and be dried for standby.
(2) prepared by colloidal sol:
By 2.25g tetraethoxysilane (TEOS), 3.8g vinyltriethoxysilane (VTES), 1.5g perfluoro capryl
Triethoxysilane (PFAS), 0.6g silica (SiO2) are scattered in 15.1g normal propyl alcohol (NPA), then in magnetic agitation
25.9g distilled water and 0.85g acetum (HAc) are added dropwise in the process.After hydrolysis 12h, sol solution can be obtained and protect
It deposits stand-by.
(3) prepared by superslide surface:
Clean glass slide and the ultraviolet shadowless glue of spin coating 1ml, 1ml sol solution and to glass slide are loaded on spin coater
Carry out ultraviolet light 5min and 100 DEG C of heat treatment 30min.Then, the perfluoropolyether of 6 μ l prepared containing is circulated into coagulate
On the glass slide of glue, superslide surface can be obtained.
(4) the magnetic particle surface of Magnetic driving decontaminates experiment:
The magnetic droplet that 10 μ l are dispersed ferroso-ferric oxide by ethylene glycol and are formed is added drop-wise on superslide surface, and is spilt at random
On some powdered graphites to surface, then in the driving magnetic drop of externally-applied magnetic field during surface moves freely by stone
Ink powder end is wrapped in inside drop, achievees the purpose that clean surface.Experimental result is as shown in Fig. 6, and magnetic droplet is in externally-applied magnetic field
Driving under can freely be moved back and forth on surface, and the graphite spot on surface is wrapped in drop in the process of moving
Face, entire cleaning process can be completed in 31s.
Embodiment 4
(1) tests early-stage preparations:
Glass slide is cropped to 25 × 20cm size and is cleaned by ultrasonic a period of time inside ethyl alcohol and acetone mixture, with
After be put into baking oven and be dried for standby.
(2) prepared by colloidal sol:
By 2.25g tetraethoxysilane (TEOS), 3.8g vinyltriethoxysilane (VTES), 1.5g perfluoro capryl
Triethoxysilane (PFAS), 0.6g silica (SiO2) are scattered in 15.1g normal propyl alcohol (NPA), then in magnetic agitation
25.9g distilled water and 0.85g acetum (HAc) are added dropwise in the process.After hydrolysis 12h, sol solution can be obtained and protect
It deposits stand-by.
(3) prepared by superslide surface:
Clean glass slide and the ultraviolet shadowless glue of spin coating 1ml, 1ml sol solution and to glass slide are loaded on spin coater
Carry out ultraviolet light 5min and 100 DEG C of heat treatment 30min.Then, the perfluoropolyether of 6 μ l prepared containing is circulated into coagulate
On the glass slide of glue, superslide surface can be obtained.
(4) superslide surface freezing is tested:
It is clapped in the environment for thering is the non-oiling surface of 10 μ l water droplets and superslide surface to be put into -10 DEG C drop and in different time sections
That takes the photograph drop freezes figure.The freezing performance on hydrophobic surface and superslide surface is as shown in fig. 7, water droplet is on two surfaces when to freeze
It is rendered as colorless and transparent state, the drop to freeze completely is rendered as milky state.The water droplet of hydrophobic surface is in 605s
When will all freeze, and the drop on superslide surface can then postpone to freeze to 1220s.
The present invention include on glass slide spin coating by colloidal sol that silane and silica are formed to construct reticular structure covering
Porous rough surface, then perfluoropolyether is added dropwise, prepares the superslide surface with lyophoby property.The superslide surface exhibits are excellent out
Good lyophoby property, water droplet and various organic matter drops all have minimum slide angle and contact angle hysteresis on the surface.In addition
The magnetic droplet being added dropwise on the surface can be cleared up during moving freely in the case where adding field drives outside and be scattered in surface
Spot.The surface also has good freezing, anti-fog, high transparency during lyophoby in addition to the automatically cleaning on achievable surface
The features such as spending.
Finally it should be noted that the above content is merely illustrative of the technical solution of the present invention, rather than the present invention is protected
The limitation of range, the simple modification or equivalent replacement that those skilled in the art carry out technical solution of the present invention,
All without departing from the spirit and scope of technical solution of the present invention.
Claims (8)
1. a kind of preparation method on the novel oiling superslide surface based on sol-gel method, which is characterized in that including walking as follows
It is rapid:
A. early-stage preparations are tested: glass slide being cropped to suitable size and is cleaned by ultrasonic a period of time inside organic solvent, with
After be put into baking oven and be dried for standby；
B. prepared by colloidal sol: by a certain amount of tetraethoxysilane TEOS, vinyltriethoxysilane VTES, three second of perfluoro capryl
Oxysilane PFAS, silica SiO2It is scattered in a certain amount of normal propyl alcohol NPA, then be added dropwise one during magnetic agitation
Quantitative distilled water and acetum HAc, hydrolysis for a period of time after, sol solution can be obtained and save stand-by；It is described
Tetraethoxysilane TEOS, vinyltriethoxysilane VTES, perfluoro capryl triethoxysilane PFAS, silica
SiO2, normal propyl alcohol NPA, distilled water and acetum HAc use mass percent match are as follows: 4.5%:7.6%:3%:
1.2%:30.2%:51.8%:1.7%；
C. prepared by superslide surface: clean glass slide and a certain amount of ultraviolet shadowless glue of spin coating, colloidal sol are loaded on spin coater
Solution simultaneously carries out ultraviolet light and heat treatment to glass slide, then, a certain amount of perfluoropolyether is circulated into prepared contain
Have on the glass slide of gel, superslide surface can be obtained.
2. the preparation method on the novel oiling superslide surface based on sol-gel method, feature exist as described in claim 1
In: the long and wide size of glass slide is 25 × 20cm.
3. the preparation method on the novel oiling superslide surface based on sol-gel method, feature exist as described in claim 1
It polymerize that form the reaction time of colloidal sol be 12h in: silane hydrolyzate.
4. the preparation method on the novel oiling superslide surface based on sol-gel method, feature exist as described in claim 1
In: ultraviolet shadowless glue and the dosage of sol solution are all 1ml when spin coating.
5. the preparation method on the novel oiling superslide surface based on sol-gel method, feature exist as described in claim 1
In: ultraviolet lighting handles the time as 5min.
6. the preparation method on the novel oiling superslide surface based on sol-gel method, feature exist as described in claim 1
In: heat treatment temperature and time are respectively as follows: 100 DEG C, 30min.
7. the preparation method on the novel oiling superslide surface based on sol-gel method, feature exist as described in claim 1
In: the method also includes step D. lyophoby performances: prepared superslide surface being placed in contact angle tester, is added dropwise respectively
The various drops of certain volume are to measure the contact angle and slide angle of various liquids, in addition, different spot drops is dripped
On to surface and record and analyze the automatically cleaning process on surface；Various dropping liquids for testing superslide surface lyophoby characteristic include: to steam
One or more of distilled water, ethylene glycol, dimethyl sulfoxide, toluene, chlorotoluene, isooctane.
8. the preparation method on the novel oiling superslide surface based on sol-gel method, feature exist as described in claim 1
In: the method also includes step D: the magnetic particle surface of Magnetic driving decontaminates experiment: will disperse ferroso-ferric oxide by ethylene glycol
And the magnetic droplet formed is added drop-wise on superslide surface, and is spilt on some powdered graphites to surface at random, then in externally-applied magnetic field
Driving magnetic drop powdered graphite is wrapped in inside drop during surface moves freely, reach clean surface
Purpose.
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| CN111266277B (en) * | 2020-02-21 | 2022-10-28 | 福建师范大学 | Lubricating fluid injection type super-smooth silicone rubber/nano inorganic matter dynamic hydrophobic-oleophobic hybrid coating and construction method and application thereof |
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