CN107502875A - It is a kind of that there is non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect and preparation method thereof - Google Patents

It is a kind of that there is non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect and preparation method thereof Download PDF

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CN107502875A
CN107502875A CN201710592318.7A CN201710592318A CN107502875A CN 107502875 A CN107502875 A CN 107502875A CN 201710592318 A CN201710592318 A CN 201710592318A CN 107502875 A CN107502875 A CN 107502875A
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CN107502875B (en
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张友法
汪希奎
张静
余新泉
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Southeast University
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
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    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208Oxides, e.g. ceramics
    • C23C18/1212Zeolites, glasses
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    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125Process of deposition of the inorganic material
    • C23C18/1295Process of deposition of the inorganic material with after-treatment of the deposited inorganic material

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Abstract

It is a kind of that there is non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect and preparation method thereof, by the way that butyl titanate and Ludox are disperseed in absolute ethyl alcohol respectively, then by after the mixed solution ultrasonic disperse of butyl titanate and absolute ethyl alcohol, it is added in the mixed solution of Ludox and absolute ethyl alcohol, add silicon fluoride and by solution in 50 DEG C of 65 DEG C of stirred in water bath 12h 24h, prepare super-hydrophobic coat finish paint solution;By super-hydrophobic coat coated in substrate, then by photocatalysis by TiO2The silicon fluoride catalytic decomposition on surface is fallen, and SiO2The silicon fluoride on surface can not then be catalytically decomposed, so as to realize prepared by the hydrophilic super hydrophobic surface of sample surfaces.The present invention sample surfaces dew condensation desorption efficiency high, catchment, antifog and heat transfer effect it is preferable, there is preferable promotional value and application prospect.

Description

It is a kind of that there is the non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect and its preparation Method
Technical field
The invention belongs to super-hydrophobic coat surface preparation technology field, and in particular to one kind, which has, strengthens dropwise condensation effect Non-homogeneous super-hydrophobic coat and preparation method thereof.
Background technology
Super hydrophobic material refers to that material surface water droplet roll angle is more than 150 °, and contact angle is less than 10 ° of novel bionic material. Currently, there is super-hydrophobic, self-cleaning performance super hydrophobic material technology of preparing, developed faster, and start in work Industry and sphere of life carry out application.Superhydrophobic characteristic is presented in macroscopic view, microcosmic that the super-hydrophobic of the non-homogeneous wetability of hydrophilic-hydrophobic is presented Material surface, due to it possesses preferable dew condensation desorption effect and catchment, antifog, heat exchange etc. have it is more wide Application prospect.And at present in super hydrophobic surface preparation field, the preparation of complete super hydrophobic surface is concentrated mainly on, for non-equal The preparation research of even wetability super hydrophobic surface is then relatively fewer.Meanwhile in terms of existing non-homogeneous super hydrophobic surface preparation, it is main The technological means to be used has following several ways:
1st, the super-hydrophobic finish paint of preparing titanium dioxide, gone forward side by side line mask photocatalysis coated in sample surfaces, by mask plate Design configuration, super hydrophobic surface realize it is hydrophilic-super-hydrophobic it is non-homogeneous wetting surface preparation;
2nd, default patterned film is first pasted in sample surfaces, then coats super-hydrophobic coat in sample surfaces, treat Sample surfaces are prepared into after hypervelocity water coating, and film is taken off, realizes hydrophilic-super-hydrophobic non-homogeneous wetting table of sample surfaces It is prepared by face;
3rd, in the patterning cylinder of sample surfaces processing micro-nano structure, sample surfaces are integrally prepared into super-hydrophobic coat, Then again by rubbing off or by Hydrophilic modification, realizing hydrophilic-hydrophobic or hydrophilic-super thin the hydrophobic coating of damaged surface The preparation of the non-homogeneous wettable surfaces of water.
4th, existing non-homogeneous super-hydrophobic layer mainly carries out hydridization using hydrophilic granules and hydrophobic granule, required with acquisition Non-homogeneous wettability, if desired change the wetability of hybrid coating, mainly matched by the hydridization of hydrophilic/hydrophobic particle to enter Row regulation and control.
But the above method, there is also following problem, is characterized in particular in during specifically used:
On the one hand, the method that the non-homogeneous wetting surface of titanium dioxide is prepared by mask photocatalysis, by the shadow of mask plate Sound is larger, and the hydrophilic area accounting of sample surfaces needs to be controlled by the design of mask plate, and by designing hydrophilic area The method on the non-homogeneous wetting surface of accounting control is then cumbersome, and preparation cost is also of a relatively high, and processing dimension is also restrained, It is difficult to the requirement for meeting that mass prepares production.
On the other hand, by the film in sample surfaces pasting patterns, the non-homogeneous profit of Hydrophobic coating preparation is then sprayed The method of wet structure, the patterned dimension that it can be realized are larger, it is difficult to meet the fabrication design of micro-nano size pattern, and generally It can only meet prepared by the other hydrophilic pattern of some grades, prepared by the other pattern of micro/nano level realizes that difficulty is larger, and cost is higher, Also it is difficult to the preparation demand for meeting the non-homogeneous wetting surface of large area.
Another further aspect, by preparing the method on non-homogeneous wetting surface in substrate surface (such as silicon chip, metal), it is necessary to logical The cylinder pattern that high-precision precision instrument prepares micro-nano size is crossed, equipment is expensive, and process technology requires higher, processing charges It is more expensive, it can only meet that current scientific research uses, it is difficult to realize the preparation on the non-homogeneous wetting surface of large area.
Finally, the method for non-homogeneous super-hydrophobic coat being prepared by hydrophilic granules/hydrophobic granule progress hydridization, due to its profit Moist regulation and control are mainly realized by changing the proportioning of hydrophilic/hydrophobic hybrid particulates, and regulation and control and operation need to pay larger The work of repeatability, operate it is cumbersome time-consuming, be unfavorable for the wetability of coating quickly the large area of regulation and control and coating prepare and Using.
Therefore, prepare non-equal by further investigation, a kind of photocatalysis of present invention offer based on above-mentioned technical problem, inventor The method of even wetability super hydrophobic surface, to solve existing for prior art, non-homogeneous wetting surface preparation cost is higher, processes Difficulty is larger, is difficult to the deficiency and defect of large-scale surface preparation.
The content of the invention
The technical problem of solution:The present invention provide it is a kind of have strengthen dropwise condensation effect non-homogeneous super-hydrophobic coat and Its preparation method, to solve existing for prior art, non-homogeneous wetting surface preparation cost is higher, difficulty of processing is larger, is difficult to reality Deficiency and defect prepared by existing large-scale surface.
Technical scheme:A kind of preparation method with the non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect, the system Preparation Method comprises the following steps:(1) deionized water is contained in a reservoir, concentrated nitric acid is added dropwise into container, prepares aqueous solution of nitric acid, And container is placed in ultrasonic disperse in ultrasonic cleaning machine, making nitric acid, dispersion mixing is uniform in deionized water;(2) it is water-soluble to nitric acid Ludox is added dropwise in liquid, prepares the mixed solution of aqueous solution of nitric acid and Ludox, and is well mixed;(3) absolute ethyl alcohol is contained In a reservoir, the container is placed in water-bath magnetic stirring apparatus, be then added dropwise to the mixed solution of ultrasonic disperse in step (2) In absolute ethyl alcohol, and it is well mixed;(4) measure again with the isometric absolute ethyl alcohol of step (3), be placed in ultrasonic cleaning machine surpass Sound disperses, and adds solution of tetrabutyl titanate thereto, and is well mixed;(5) solution that step (4) is prepared is added completely into step Suddenly in the solution that (3) are prepared, the silicon fluoride that then adds is uniformly mixed under condition of water bath heating, obtains TiO2- SiO2Super-hydrophobic coat finish paint solution is blended;(6) by the finish paint solution that step (5) is prepared using spraying, Best-Effort request or spin coating Substrate is placed in baking oven and dried, be prepared into surface and possess super-hydrophobicity coated in substrate by least one of film plating process The sample of energy;(7) sample in step (6) is subjected to ultraviolet catalytic, you can obtain with the non-of reinforcing dropwise condensation effect Uniform super-hydrophobic coat.
In above-mentioned steps (1), the concentration of concentrated nitric acid is 65wt.%-68wt.%, and the pH value for preparing aqueous solution of nitric acid is 2.0-4.0, and the deionized water in container and the absolute ethyl alcohol volume ratio in step (4) they are 1:7-1:5.
The Ludox and the mass ratio of aqueous solution of nitric acid being added dropwise in above-mentioned steps (2) are 1:20-1:4, hybrid mode is to stir Mix or ultrasonic mixing, incorporation time 5min-10min.
The absolute ethyl alcohol volume added in above-mentioned steps (3) and step (4) is equal, and hybrid mode is using stirring or super Sound dispersing mode, incorporation time are 5min-10min;The butyl titanate and the quality of Ludox added in the step (4) Than for 1:2-3:1.
The silicon fluoride and the volume ratio of butyl titanate added in above-mentioned steps (5) is 1:5-1:1, hybrid mode is stirring Or ultrasonic disperse mode, and incorporation time is 5min-10min;The heating-up temperature of mixed solution stirring in water bath is 50 DEG C -65 DEG C, Mixing time is 12h-24h.
Substrate drying temperature in above-mentioned steps (6) is 60 DEG C -80 DEG C, drying time 0.5h-1h.
The sample ultraviolet catalytic time in above-mentioned steps (7) is 50s-300s, and the power for being catalyzed light source is 1500W- 2000W, and it is 10cm-15cm to be catalyzed the distance between light source and sample upper surface.
Above-mentioned preparation method is obtained to have the non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect.
Beneficial effect:1st, technical scheme, there is TiO simultaneously by preparing2And SiO2The hydridization of nano particle is mixed Solution is closed, and the face coat with superhydrophobic characteristic is prepared by using the solution, by realizing sample without mask photocatalysis method Product surface portion particle is hydrophilic, and partial particulate is hydrophobic, for existing mask photocatalysis mode, technical side of the invention For case using being catalyzed without mask mode, its preparation technology is fairly simple, and preparation cost is relatively low, while is easier to realize the non-of large area The preparation on uniform wet surface.
2nd, technical scheme, due to the TiO of preparation2And SiO2It is the particle of Nano grade, face coat is in light After catalysis, pass through TiO2The catalytic action of particle, makes TiO2The silicon fluoride on surface obtains fast decoupled, makes hydrophilic TiO2Particle Presentation water-wet behavior, and SiO2The surface of particle then remains in that superhydrophobic characteristic, so as to realize sample coatings surface in micro-nano Hydrophilic-super-hydrophobic non-homogeneous wetting characteristics in rank, for current patterned film concealing technique, energy of the present invention The hydrophilic area size class enough realized is smaller, and the condensation desorption efficiency of drop is more preferable, while it is non-homogeneous to be also more suitable for large area Soak the preparation and application on surface.
3rd, the present invention by the cylinder or pattern in substrate surface processing micro-nano structure due to that need not cause system of the present invention Standby non-homogeneous wettable surfaces' manufacture craft is simpler, and cost of manufacture is not only cheap for prior art, And easily operate and realize, there is preferable promotion and application prospect.
4th, technical scheme, after surface super hydrophobic coating passes through photocatalysis, sample surfaces macroscopic view is still in Existing super-hydrophobic state, and it is hydrophilic to be then presented part on sample is microcosmic, the hydrophobic non-homogeneous wetting state in part, in this way, making sample The hydrophilic area on surface can effectively adsorb the steam in air, make vapor when sample surface temperature reaches dew point, form water Pearl condenses in sample surfaces, and by the forming core growth process of condensation, condensing drip is constantly grown up, and by between adjacent water droplet Merging releases energy and the desorption that bounces, so as to realize that the property of sample surfaces and rate and drop desorption efficiency effectively improve.
5th, the non-homogeneous wetting surface prepared by technical scheme, due to the presence of microcosmic hydrophilic granules, makes Sample surfaces are more favorable for formation and the desorption of big drop, and for existing water-wetted surface, its drop desorption efficiency obtains To effectively improving, while causing the sample surfaces to possess freezing, antifog, automatically cleaning characteristic, the heat exchange of sample surfaces is additionally favorable for Efficiency improves, and is constantly grown up by the drop of sample surfaces to bounce or roll desorption, reaches the purpose of energy-conservation;And present invention system Standby non-homogeneous wetability coating surface, for existing conventional super hydrophobic surface, its macroscopical performance disclosure satisfy that The hydrophobic performance of super hydrophobic surface, and on microcosmic for, the forming core of non-homogeneous wettable surfaces of the invention, more conducively drop With growing up for water droplet, catchmenting, in terms of antifog and heat exchange efficiency, the super hydrophobic surface performance than routine is more preferable, thus possesses Preferable promotional value and application prospect.
6th, non-homogeneous super-hydrophobic coat of the present invention, by changing ultraviolet lighting intensity or light application time, coating Overall wetability i.e. can be achieved regulation and control and change, easy to operate, cost is low, is easy to large-area applications, air-conditioning, heat pump, generating, There is important application prospect on the condensation heat transfer associated components such as desalinization.
Brief description of the drawings
Fig. 1 is the super-hydrophobic coat surface preparation flow figure of the present invention;
Fig. 2 is condensing state stereoscopic take pictures figure of the sample of the embodiment of the present invention 1 in 5min38s;
Fig. 3 is condensing state stereoscopic take pictures figure of the sample of the embodiment of the present invention 1 in 5min54s;
Fig. 4 be the embodiment of the present invention 1 coating in copper sheet substrate stereoscopic taking pictures after photocatalysis 250s, condensation 1min Figure;
Fig. 5 is stereoscopic bat of the coating of the embodiment of the present invention 1 in copper sheet substrate after photocatalysis 250s, condensation 20min According to figure;
Fig. 6 is the sample surfaces microscopic appearance SEM scanned pictures of the embodiment of the present invention 2.
Embodiment
Following examples only technical concepts and features to illustrate the invention, its object is to allow person skilled in the art It is that can understand present disclosure and implement according to this, it is not intended to limit the scope of the present invention.It is all according to the present invention The equivalent transformation or modification that Spirit Essence is done, should all be included within the scope of the present invention.
Embodiment 1
As Figure 1-5, it is a kind of that there is the non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect, the super-hydrophobic coat Surface is by TiO2And SiO2Nano particle mixing self assembly accumulation forms, and has nano-porous structure.
A kind of above-mentioned preparation method with the non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect, the preparation side Method comprises the following steps:
(1) 10mL deionized water is contained first in beaker, 1- is added dropwise into beaker by the dropper of 2mL normal capacities The concentrated nitric acid that 2 drop concentration are 65wt.%, is measured using pH test paper or pH meter, and the pH value of water solution adjusted in beaker is 2.0, and beaker is placed in ultrasonic disperse in ultrasonic cleaning machine, making nitric acid, dispersion mixing is uniform in deionized water;
(2) 0.5g Ludox is added dropwise into the beaker of step (1) using dropper, and continues ultrasonic disperse 5min;
(3) absolute ethyl alcohol for measuring 50mL is contained in beaker, and the beaker is placed in water-bath magnetic stirring apparatus, then will The solution of ultrasonic disperse is added dropwise in absolute ethyl alcohol in step (2), continues magnetic agitation 5min;
(4) 50mL ethanol solution is measured again, is placed in ultrasonic disperse in ultrasonic cleaning machine, and add thereto 0.5mL solution of tetrabutyl titanate, continue ultrasonic disperse 5min;
(5) solution for preparing step (4) is added in the solution that step (3) is prepared, and then adds 0.5mL fluorine silicon Alkane, the stirring in water bath 12h under 50 DEG C of bath temperature, obtain TiO2-SiO2The preparation of super-hydrophobic coat finish paint is blended;
(6) by the solution that step (5) is prepared is using one kind in spraying, Best-Effort request or spin coating film plating process or this is several Method combination coating on the glass substrate, substrate is placed in 60 DEG C of baking oven and dries 1h, be prepared into surface possess it is super-hydrophobic The sample of performance;
(7) sample in step (6) is subjected to ultraviolet catalytic 50s, the distance for being catalyzed ultraviolet source and sample surfaces is 10cm, and the power for being catalyzed light source is 1500W, makes the TiO on sample super-hydrophobic coat surface2Particle ultraviolet lighting effect under, Catalytic action is played, by TiO2The silicon fluoride catalytic decomposition of particle surface, exposes hydrophilic TiO2Particle;And SiO2Particle table The silicon fluoride in face can not be then catalytically decomposed, so as to realize that hydrophilic-super-hydrophobic non-homogeneous wetting characteristics is presented in sample surfaces, Strengthen the dropwise condensation effect of sample surfaces.
Table 1 counted contact angle of the coating surface after ultraviolet catalytic 50s-10min of the present invention, roll angle and Condense bounce.It can be found that sample surfaces are after photocatalysis 50s-300s from table, measurement contact angle declines from 163 ° To 156 °, roll angle rises to 1 ° from 0.8 °, and sample surfaces remain in that superhydrophobic characteristic;As sample surfaces photocatalysis 10min Afterwards, the adhesiveness of water is increased better than the increase of catalytic surface hydrophilic segment accounting, sample surfaces, makes sample surfaces contact angle low In 150 °, and contact angle is gradually reduced with the extension of catalysis time.And pass through condensation test, find sample in catalysis 50s- In 250s time ranges, it can occur to condense bounce, so as to beneficial to the condensation of sample surfaces water droplet spring desorption.
The sample of table 1 passes through the contact angle of different catalysis times, roll angle and bounce statistical form
Catalysis time 50s 100s 150s 200s 250s 300s 10min 20min 30min
Contact angle (°) 163 162 162 160 156 156 140 120 118
Roll angle (°) 0.8 0.8 1 1 1 1 > 90 > 90 > 90
Whether spring is had Have Have Have Have Have Nothing Nothing Nothing Nothing
From Fig. 2 and Fig. 3, glass substrate sample surface still has water droplet after 250s is catalyzed in condensation process Merge bounce.
The super-hydrophobic coat that Fig. 4 is the present invention after photocatalysis 250s, is carried out in copper sheet substrate under stereomicroscope The figure of taking pictures after 1min is condensed, by the way that in figure, due to photocatalysis, it is hydrophilic and partly thin that part is presented in sample surfaces The state of water, cause water droplet preferentially to condense forming core in hydrophilic area, form the condensing drip of comparatively dense, the water droplet of hydrophobic region is then relative Distribution is relatively thin smaller, and sharp contrast is formed with hydrophilic area;After 20min condensation tests, as shown in figure 5, in hydrophilic area Drop is grown up to form larger drop, and these big drops are present in the hydrophilic area shown in Fig. 4, and the small water droplet of hydrophobic region is merged into Hydrophilic area, illustrate to pass through after photocatalysis, hydrophilic area enhances the Drop Condensation effect of sample surfaces.
Embodiment 2
A kind of to have the non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect, the super-hydrophobic coat surface is by TiO2With SiO2Nano particle mixing self assembly accumulation forms, and has nano-porous structure.
A kind of above-mentioned preparation method with the non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect, the preparation side Method comprises the following steps:
(1) 10mL deionized water is contained first in beaker, 1- is added dropwise into beaker by the dropper of 2mL normal capacities The concentrated nitric acid that 2 drop concentration are 68wt.%, is measured using pH test paper or pH meter, and the pH value of water solution adjusted in beaker is 2.5, and beaker is placed in ultrasonic disperse in ultrasonic cleaning machine, making nitric acid, dispersion mixing is uniform in deionized water;
(2) 1.0g Ludox is added dropwise into the beaker of step (1) using dropper, and continues ultrasonic disperse 8min;
(3) absolute ethyl alcohol for measuring 60mL is contained in beaker, and the beaker is placed in water-bath magnetic stirring apparatus, then will The solution of ultrasonic disperse is added dropwise in absolute ethyl alcohol in step (2), continues magnetic agitation 8min;
(4) 60mL ethanol solution is measured again, is placed in ultrasonic disperse in ultrasonic cleaning machine, and add thereto 0.8mL solution of tetrabutyl titanate, continue ultrasonic disperse 8min;
(5) solution for preparing step (4) is added in the solution that step (3) is prepared, and then adds 0.5mL fluorine silicon Alkane, the stirring in water bath 20h under 60 DEG C of bath temperature, obtain TiO2-SiO2The preparation of super-hydrophobic coat finish paint is blended;
(6) by the solution that step (5) is prepared is using one kind in spraying, Best-Effort request or spin coating film plating process or this is several Substrate is placed in 70 DEG C of baking oven coated in copper sheet substrate and dries 45min by the combination of method, be prepared into surface possess it is super thin The sample of water-based energy;
(7) sample in step (6) is subjected to ultraviolet catalytic 250s, the distance for being catalyzed ultraviolet source and sample surfaces is 12cm, and the power for being catalyzed light source is 1800W, makes the TiO on sample super-hydrophobic coat surface2Particle ultraviolet lighting effect under, Catalytic action is played, by TiO2The silicon fluoride catalytic decomposition of particle surface, exposes hydrophilic TiO2Particle;And SiO2Particle table The silicon fluoride in face can not be then catalytically decomposed, so as to realize that hydrophilic-super-hydrophobic non-homogeneous wetting characteristics is presented in sample surfaces, Strengthen the dropwise condensation effect of sample surfaces.
As shown in fig. 6, being taken pictures by the way that hydridization super-hydrophobic coat surface is carried out into SEM scannings, sample coatings surface is obtained Microscopic appearance picture.By picture amplifying observation, sample surfaces are that hybrid particulates assemble the porous rough surface knot to be formed Structure.
As the table statistics result in table 2 understand, by sample surfaces by different photocatalysis treatments after, catchmented Experiment, inlet time 2h;For the super-hydrophobic sample surfaces of hydridization after photocatalysis, overall collecting water from runoff is above uncatalyzed hydridization Super-hydrophobic coat and SiO2Super-hydrophobic coat, after sample surfaces are catalyzed 200s and 250s, collecting water from runoff is relatively higher than other Comparative sample, respectively 23.135g and 22.817g, after photocatalysis 50s-250s, sample collecting water from runoff is all higher than 20g, hence it is evident that high In the 17.447g and SiO of uncatalyzed sample collecting water from runoff2The 19.022g of super hydrophobic surface, after illustrating photocatalysis, sample surfaces Condensation and desorption effect strengthened.
Collecting water from runoff statistical form of the sample of table 2 after different catalysis times, the experiment 2h that catchments
Embodiment 3
A kind of to have the non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect, the super-hydrophobic coat surface is by TiO2With SiO2Nano particle mixing self assembly accumulation forms, and has nano-porous structure, the preparation side of the non-homogeneous super-hydrophobic coat Method comprises the following steps:
(1) 10mL deionized water is contained first in beaker, 1- is added dropwise into beaker by the dropper of 2mL normal capacities The concentrated nitric acid that 2 drop concentration are 65wt.%, is measured using pH test paper or pH meter, and the pH value of water solution adjusted in beaker is 4.0, and beaker is placed in ultrasonic disperse in ultrasonic cleaning machine, making nitric acid, dispersion mixing is uniform in deionized water;
(2) 1.5g Ludox is added dropwise into the beaker of step (1) using dropper, and continues ultrasonic disperse 10min;
(3) absolute ethyl alcohol for measuring 70mL is contained in beaker, and the beaker is placed in water-bath magnetic stirring apparatus, then will The solution of ultrasonic disperse is added dropwise in absolute ethyl alcohol in step (2), continues magnetic agitation 10min;
(4) 70mL ethanol solution is measured again, is placed in ultrasonic disperse in ultrasonic cleaning machine, and add thereto 1.0mL solution of tetrabutyl titanate, continue ultrasonic disperse 10min;
(5) solution for preparing step (4) is added in the solution that step (3) is prepared, and then adds 0.5mL fluorine silicon Alkane, the stirring in water bath 24h under 65 DEG C of bath temperature, obtain TiO2-SiO2The preparation of super-hydrophobic coat finish paint is blended;
(6) by the solution that step (5) is prepared is using one kind in spraying, Best-Effort request or spin coating film plating process or this is several Substrate is placed in 80 DEG C of baking oven coated in substrate and dries 0.5h, be prepared into surface and possess super-hydrophobicity by the combination of method The sample of energy;
(7) sample in step (6) is subjected to ultraviolet catalytic 300s, the distance for being catalyzed ultraviolet source and sample surfaces is 15cm, and the power for being catalyzed light source is 2000W.
Sample through catalysis is tested by condensation, and its surface nucleation rate is significantly increased, meanwhile, its dropwise condensation effect Fruit has also obtained larger raising.Tested through contact angle and roll angle, as shown in table 1, after sample catalysis 300s, contact angle is 156 °, roll angle is 1 °, and the sample surfaces of non-uniform coating have reached the performance and requirement of super hydrophobic surface.

Claims (8)

  1. A kind of 1. preparation method with the non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect, it is characterised in that the preparation Method comprises the following steps:
    (1)Deionized water is contained in a reservoir, is added dropwise concentrated nitric acid into container, prepares aqueous solution of nitric acid, and container is placed in super Ultrasonic disperse in sound washer, making nitric acid, dispersion mixing is uniform in deionized water;
    (2)Ludox is added dropwise into aqueous solution of nitric acid, prepares the mixed solution of aqueous solution of nitric acid and Ludox, and is well mixed; (3)Absolute ethyl alcohol is contained in a reservoir, the container is placed in water-bath magnetic stirring apparatus, then by step(2)Middle ultrasound point Scattered mixed solution is added dropwise in absolute ethyl alcohol, and is well mixed;
    (4)Measure again and step(3)Isometric absolute ethyl alcohol, ultrasonic disperse in ultrasonic cleaning machine is placed in, and added thereto Enter solution of tetrabutyl titanate, and be well mixed;
    (5)By step(4)The solution of preparation is added completely into step(3)In the solution of preparation, the silicon fluoride that then adds, in water It is uniformly mixed under bath heating condition, obtains TiO2-SiO2Super-hydrophobic coat finish paint solution is blended;
    (6)By step(5)The finish paint solution of preparation is using the coating of at least one of spraying, Best-Effort request or spin coating film plating process In substrate, substrate is placed in baking oven and dried, be prepared into the sample that surface possesses ultra-hydrophobicity;
    (7)By step(6)In sample carry out ultraviolet catalytic, you can obtain with strengthening the non-homogeneous super of dropwise condensation effect Hydrophobic coating.
  2. 2. a kind of preparation method with the non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect according to claim 1, It is characterized in that:The step(1)In, the concentration of concentrated nitric acid is 65wt.%-68wt.%, and the pH value for preparing aqueous solution of nitric acid is 2.0-4.0, and deionized water and step in container(4)In absolute ethyl alcohol volume ratio be 1:7-1:5.
  3. 3. a kind of preparation method with the non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect according to claim 1, It is characterized in that:The step(2)The Ludox of middle dropwise addition and the mass ratio of aqueous solution of nitric acid are 1:20-1:4, hybrid mode is Stirring or ultrasonic mixing, incorporation time 5min-10min.
  4. 4. a kind of preparation method with the non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect according to claim 1, It is characterized in that:The step(3)And step(4)The absolute ethyl alcohol volume of middle addition is equal, and hybrid mode is using stirring Or ultrasonic disperse mode, incorporation time are 5min-10min;The step(4)The butyl titanate of middle addition and Ludox Mass ratio is 1:2-3:1.
  5. 5. a kind of preparation method with the non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect according to claim 1, It is characterized in that:The step(5)The silicon fluoride of middle addition and the volume ratio of butyl titanate are 1:5-1:1, hybrid mode is Stirring or ultrasonic disperse mode, and incorporation time is 5min-10min;The heating-up temperature of mixed solution stirring in water bath is 50 DEG C -65 DEG C, mixing time 12h-24h.
  6. 6. a kind of preparation method with the non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect according to claim 1, It is characterized in that:The step(6)In substrate drying temperature be 60 DEG C -80 DEG C, drying time 0.5h-1h.
  7. 7. a kind of preparation method with the non-homogeneous super-hydrophobic coat for strengthening dropwise condensation effect according to claim 1, It is characterized in that:The step(7)In the sample ultraviolet catalytic time be 50s-300s, the power for being catalyzed light source is 1500W- 2000W, and it is 10cm-15cm to be catalyzed the distance between light source and sample upper surface.
  8. 8. any preparation methods of claim 1-7 are obtained to have the non-homogeneous super-hydrophobic painting for strengthening dropwise condensation effect Layer.
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CN115387154B (en) * 2022-08-26 2023-10-10 中国科学院长春应用化学研究所 Passive radiation refrigeration paper and preparation method thereof

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