CN101845242A - Super-hydrophobic nano-composite coating and preparation method thereof - Google Patents
Super-hydrophobic nano-composite coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a super-hydrophobic nano-composite coating comprising the following components in percentage by weight: 0.5-10.5 percent of hydrophobic silicon dioxide, 0.2-5.4 percent of hydrophobic polymer material and 86.5-99.3 percent of solvent, wherein a contact angle of a water drop on a membrane surface prepared by the coating is 152-169 degrees, and a rolling angle is 1-9 degrees. When the coating is transparent, the visible light transmission of the membrane prepared from the coating is 80-94 percent. The invention also discloses a preparation method of the super-hydrophobic nano-composite coating. The nano-composite coating not only has excellent super-hydrophobicity and low cost of products, but also can obtain higher transparency by reducing the contents of the hydrophobic silicon dioxide and the hydrophobic polymer material and has simple preparation processing equipment and high production efficiency.
Description
Technical field
The invention belongs to super hydrophobic coating and preparing technical field thereof, be specifically related to a kind of super-hydrophobic nano-composite coating and preparation method thereof.
Background technology
Super hydrophobic material makes it become the focus of scientific research recent years because of it has actual using value in fields such as waterproof, automatically cleaning, hull drag reduction, micro-drop free of losses transmission, micro-fluidic system.
Super hydrophobic material need reach two requirements usually: the one, and water droplet need reach more than 150 ° at the contact angle of material surface, and the 2nd, water droplet needs less than 10 ° in the roll angle of material surface.And reaching such requirement, the super hydrophobic material that will make preparation need satisfy two key conditions: the one, and material surface has enough roughness, particularly has micro-nano dual yardstick structure, the 2nd, material is a hydrophobic material, has enough low surface energy, generally promptly, water droplet can reach more than 90 ° at the contact angle on the level and smooth surface mass.In order to realize this two conditions, present main method is the surfaceness of constructing earlier to a certain degree, and then at the material of uneven surface physics or chemical lamination one deck low surface energy, perhaps directly makes the low surface energy material have to a certain degree surfaceness.For last class methods, as Dutch scientist just utilize particle diameter for 70nm through the silicon dioxide granule after the ammonification and particle diameter reacting to each other between the silicon dioxide granule that epoxidation is handled for 700nm, at first obtained having the roughness structure of many short grained dual yardsticks at large particle surface, thereby the polydimethylsiloxane after its finishing ammonification obtains having super-hydrophobic low surface energy surface (Ming then, W., D.Wu, et al. (2005). " Superhydrophobic films fromraspberry-like particles. " Nano Letters 5 (11): 2298-2301.).And the Korea S scientist is first carbon nano tube modified above the individual layer colloid crystal of the polystyrene with micro-meter scale with nanoscale by the wet-chemical self-assembling technique, modify the super hydrophobic surface (Li that obtains low surface energy with silicon fluoride then, Y., X.J.Huang, et al. (2007). " Superhydrophobic bionic surfaces with hierarchical microsphere/SWCNT compositearrays. " Langmuir 23 (4): 2169-2174.).French scientist then is to obtain the ZnO nano-wire array by the growth of electrochemistry lamination earlier, then it is carried out having obtained super hydrophobic surface (Pauporte after stearic acid is modified, T., G.Bataille, et al. (2010). " Well-Aligned ZnO Nanowire Arrays Prepared by Seed-Layer-FreeElectrodeposition and Their Cassie-Wenzel Transition after Hydrophobization. " Journal ofPhysical Chemistry C 114 (1): 194-202.).But these methods need two technological processs at least, thereby operating process is many, produce line length, are unfavorable for improving industrial work efficiency.For one class methods of back, pass through at CF as Italian scientist
4In the atmosphere, the roughness and the low-energy super hydrophobic surface (Cortese that are had different micro-nano-scales with the way of plasma etching at dimethyl silicone polymer surface simultaneously, B., S.D ' Amone, et al. (2008). " Superhydrophobicity due to the hierarchical scale roughness of PDMS surfaces. " Langmuir24 (6): 2712-2718.); U.S. scientist with the aperture is
Polycarbonate be template, on hydrophobic polypropylene matrix, heat-treat impression, obtained the super-hydrophobic polypropylene surface (Hsu, S.H.and W.M.Sigmund (2010). " Artificial Hairy Surfaces with a Nearly Perfect Hydrophobic Response. " Langmuir26 (3): 1504-1506.); The Turkey scientist is by being separated polypropylene at its good solvent and poor solvent the inside, directly obtained the polypropylene super-hydrophobic surface (Erbil of porous surface, H.Y., A.L.Demirel, et al. (2003). " Transformation of a simple plastic into a superhydrophobic surface. " Science 299 (5611): 1377-1380.); The TaiWan, China scientist obtains hydrophobic surface (Sheen by the sol-gel method of triethoxy methyl silicane and tetraethoxysilane, Y.C., W.H.Chang, et al. (2009). " Non-fluorinatedsuperamphiphobic surfaces through sol-gel processing of methyltriethoxysilane andtetraethoxysilane. " Materials Chemistry and Physics 114 (1): 63-68.).Because these methods or need complex apparatus instrument (plasma treatment, electrospinning silk, template etc.) or complicated technology means (being separated sol-gel method etc.) to realize, thereby limitation is too big, is difficult to wide popularization and application.
In addition, when super hydrophobic material uses as the surfacing of transparent base material, the transparency of super hydrophobic material itself can directly influence the transparency of body material on the one hand, preparation because of super hydrophobic material needs material surface to have certain roughness on the other hand, and the increase of roughness can make material that the reflection-absorption of visible light is increased, thereby cause the reduction of the material transparency, therefore also limited the surfacing use of super hydrophobic material as the transparent use occasion of the whole material of needs.
Summary of the invention
The objective of the invention is the problem at the prior art existence, a kind of new super-hydrophobic nano-composite coating is provided, this composite coating is the hydrophobic performance excellence not only, and with low cost.
Another object of the present invention provides a kind of method for preparing above-mentioned super-hydrophobic nano-composite coating, and this method prescription is simple, preparation is easy, and production cost is low.
Super-hydrophobic nano-composite coating provided by the invention, it is characterized in that each set of dispense than by mass percentage is in this coating: hydrophobically modified silicon-dioxide 0.5～10.5%, hydrophobic polymeric material 0.2～5.4%, solvent 86.5～99.3%, and water droplet is 152～169 ° at the lip-deep contact angle of the film made from this coating, and roll angle is 1～9 °.
And the proportioning of each component is by mass percentage in the transparent super-hydrophobic nano-composite coating: hydrophobically modified silicon-dioxide 0.5～3.1%, hydrophobic polymeric material 0.2～0.8%, solvent 96.1～99.3%, and the film forming visible light transmissivity of this coating system of usefulness that is obtained can reach 80～94%.
The particle diameter of the water drain silica in the above-mentioned coating is 10～100nm.
Hydrophobic polymeric material in the above-mentioned coating is any in polydimethylsiloxane, polystyrene or the fluorinated polyurethane.Wherein fluorinated polyurethane can be by document Tan, H., X.Y.Xie, et al. (2004). " Synthesis and surfacemobility of segmented polyurethanes with fluorinated side chains attached to hard blocks. " Polymer 45 (5): 1495-1502. disclosed method synthetic.
Solvent in the above-mentioned coating is to make dewatering nano silicon-dioxide and hydrophobic polymeric material obtain the solvent of homodisperse (dissolving or swelling) simultaneously, specifically can select toluene, dimethylbenzene, tetrahydrofuran (THF), N for use, N-N,N-DIMETHYLACETAMIDE or N, any in the dinethylformamide.
The method of the super-hydrophobic nano-composite coating that preparation provided by the invention is above-mentioned, this method is with hydrophobically modified silicon-dioxide 0.5～10.5%, hydrophobic polymeric material 0.2～5.4%, solvent 86.5～99.3%, mechanical stirring or sonic oscillation dispersion at normal temperatures or Ball milling are uniformly dispersed it and get final product, and wherein the add-on of each component is mass percent.
In order to obtain transparent super-hydrophobic nano-composite coating the time, the present invention is adjusted into the proportioning of each component in the aforesaid method by mass percentage: hydrophobically modified silicon-dioxide 0.5～3.1%, hydrophobic polymeric material 0.2～0.8%, solvent 96.1～99.3%.
The particle diameter of used water drain silica is 10～100nm in the aforesaid method.
Used hydrophobic polymeric material is any in polydimethylsiloxane, polystyrene or the fluorinated polyurethane in the aforesaid method.Wherein fluorinated polyurethane can be by document Tan, H., X.Y.Xie, et al. (2004). " Synthesis andsurface mobility of segmented polyurethanes with fluorinated side chains atached to hardblocks. " Polymer 45 (5): 1495-1502. disclosed method synthetic.
Used solvent is to make hydrophobically modified nano silicon and hydrophobic polymeric material obtain the solvent of homodisperse (dissolving or swelling) simultaneously in the aforesaid method, specifically can select toluene, dimethylbenzene, tetrahydrofuran (THF), N for use, N-N,N-DIMETHYLACETAMIDE or N, any in the dinethylformamide.
Time with mechanical stirring, sonic oscillation or Ball milling in the aforesaid method is 30～300min.
The present invention compared with prior art has following positively effect:
1, since water droplet making the lip-deep contact angle of film and can reach 152～169 ° with super-hydrophobic nano-composite coating provided by the invention, roll angle can reach 1～9 °, thereby the super-hydrophobicity excellence of nano composite dope provided by the invention, water droplet can roll on the film surface that coating forms easily, realize the automatic cleaning action of similar lotus leaf, see Fig. 2,3.
2, because the employed three kinds of raw materials of super-hydrophobic nano-composite coating provided by the invention not only are cheap general goods, and the water drain silica and the hydrophobic polymeric material content that wherein play super-hydrophobic main effect are low, thereby not only raw material sources are extensive, and product price is cheap, avoid the common hydrophobic and super hydrophobic coating of preparation need add various auxiliary agents, increased the problem of product cost greatly.
3, since the present invention by after reducing water drain silica and the content of hydrophobic polymeric material in composite coating, use the film of this coating brushing to obtain very high transparent (see figure 4), thereby enlarged the scope of application of this composite coating, having avoided prior art because of needs add various auxiliary agents in the coating the inside, all is opaque or translucent problem and make the product film of acquisition basically.
4, contain inorganic nano-particle owing in the composite coating provided by the present invention, thereby make this coating have certain weathering resistance and stability.
5, because prescription provided by the invention is simple, do not need to add any auxiliary agent, and preparation technology's equipment is all very simple and easy, thereby production cost is low, the efficient height, both avoided common hydrophobic and general super hydrophobic coating need add promotor, stablizer, mould inhibitor, anti-sedimentation agent, defoamer, the prescription complicated problems that auxiliary agent caused such as wetting agent, avoid prior art again or needed the complex apparatus instrument, maybe need to adopt the complicated technology means, or need the technological operation flow process many, produce problems such as line length.
Description of drawings
Fig. 1 be the water droplet of one 3 μ L in the level and smooth lip-deep form of polydimethylsiloxane film, its contact angle is 108.2 °;
Fig. 2 be the water droplet of one 10 μ L in the lip-deep form of composite coating film that is obtained with embodiment 10, its contact angle is 167 °;
Fig. 3 be the water droplet of one 10 μ L in the lip-deep roll angle of composite coating film that is obtained with embodiment 10, be～1 °;
Fig. 4 is a common lid slide (Glass, left side) and the transparency that scribbles the transparent hydrophobic coating (Sample A, right side) that embodiment 7 obtained on common lid slide matrix photo relatively;
Fig. 5 is the light transmittance curve figure of two slide visible lights about Fig. 4, as can be seen from the figure (91～94%) do not significantly decrease before surperficial spin coating has the transparency (86～94%) and the spin coating of common lid slide of transparent hydrophobic coating, illustrate that this super hydrophobic coating can be used as Clear paint and uses.
Embodiment
Provide embodiment below; so that the present invention will be described in more detail; it is important to point out that following examples can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field must belong to protection scope of the present invention according to the invention described above content to some nonessential improvement and the adjustment that the present invention did.
In addition, what deserves to be explained is: 1. in order to carry out performance test, below the film of making of each embodiment coating all on common lid slide matrix, carry out spin coating and obtain, spin coating proceeding is 3000r/min, 20s; The back dry 1h in 80 ℃ baking oven that films with solvent flashing, takes out postcooling to room temperature and promptly obtains the cover glass item for disposal that the surface has the ultra-hydrophobicity rete, carries out performance test then.2. German Kr ü ss DSA100 instrument is adopted in the test of contact angle and roll angle; 3. ultra-violet and visible spectrophotometer (UV-1800PC) is adopted in the visible light transmissivity test.
Adding the 2.63g particle diameter earlier in 496.31g toluene is the silicon-dioxide and the 1.06g polydimethylsiloxane of the hydrophobically modified of 10～30nm, and mechanical stirring disperses to obtain transparent hydrophobic coating behind the 30min at normal temperatures then.
The contact angle of this transparent hydrophobic coating is 152～154 °; Roll angle is 7～9 °; Transmittance is 88～94%.
Embodiment 2
Adding the 3.97g particle diameter earlier in 494.47g toluene is the silicon-dioxide and the 1.56g polystyrene of the hydrophobically modified of 10～30nm, and sonic oscillation disperses to obtain transparent hydrophobic coating behind the 30min at normal temperatures then.
The contact angle of this transparent hydrophobic coating is 153～157 °; Roll angle is 3～5 °; Transmittance is 88～94%.
Embodiment 3
Adding the 4.925g particle diameter earlier in 492.61g dimethylbenzene is the silicon-dioxide and the 2.465g fluorinated polyurethane of the hydrophobically modified of 20～50nm, obtains transparent hydrophobic coating behind the Ball milling 50min at normal temperatures then.
The contact angle of this transparent hydrophobic coating is 153～155 °; Roll angle is 1～3 °; Transmittance is 88～94%.
Embodiment 4
Adding the 7.355g particle diameter earlier in 490.195g dimethylbenzene is the silicon-dioxide and the 2.45g polydimethylsiloxane of the hydrophobically modified of 20～50nm, and mechanical stirring disperses to obtain transparent hydrophobic coating behind the 100min at normal temperatures then.
The contact angle of this transparent hydrophobic coating is 156～158 °; Roll angle is 1～3 °; Transmittance is 87～94%.
Embodiment 5
Adding the 7.815g particle diameter earlier in the 488.28g tetrahydrofuran (THF) is the silicon-dioxide and the 3.905g polystyrene of the hydrophobically modified of 40～60nm, and sonic oscillation disperses to obtain transparent hydrophobic coating behind the 150min at normal temperatures then.
The contact angle of this transparent hydrophobic coating is 158～161 °; Roll angle is 1～3 °; Transmittance is 87～94%.
Embodiment 6
Adding the 9.755g particle diameter earlier in the 487.805g tetrahydrofuran (THF) is the silicon-dioxide and the 2.44g fluorinated polyurethane of the hydrophobically modified of 40～60nm, obtains transparent hydrophobic coating behind the Ball milling 100min at normal temperatures then.
The contact angle of this transparent hydrophobic coating is 157～160 °; Roll angle is 1～3 °; Transmittance is 87～94%.
Embodiment 7
At 484.495g N, adding the 11.63g particle diameter in the dinethylformamide is the silicon-dioxide and the 3.875g polystyrene of the hydrophobically modified of 60～85nm earlier, and mechanical stirring disperses to obtain transparent hydrophobic coating behind the 230min at normal temperatures then.
The contact angle of this transparent hydrophobic coating is 158～162 °; Roll angle is 1～3 °; Transmittance is 86～94%.
Embodiment 8
Adding the 15.385g particle diameter earlier in the 480.77g N,N-dimethylacetamide is the silicon-dioxide and the 3.845g fluorinated polyurethane of the hydrophobically modified of 60～85nm, and sonic oscillation disperses to obtain transparent hydrophobic coating behind the 200min at normal temperatures then.
The contact angle of this transparent hydrophobic coating is 160～165 °; Roll angle is 1～3 °; Transmittance is 80～91%.
Embodiment 9
Adding the 26.785g particle diameter earlier in 446.43g toluene is the silicon-dioxide and the 26.785g polydimethylsiloxane of the laboratory drains modification of 60～85nm, obtains opaque super hydrophobic coating behind the Ball milling 200min at normal temperatures then.
The contact angle of this opaque super hydrophobic coating is 154～156 °; Roll angle is 3～5 °.
Embodiment 10
At 444.445g N, adding the 44.445g particle diameter in the dinethylformamide is the silicon-dioxide and the 11.11g polystyrene of the hydrophobically modified of 80～100nm earlier, and sonic oscillation disperses to obtain opaque super hydrophobic coating behind the 280min at normal temperatures then.
The contact angle of this opaque super hydrophobic coating is 165～169 °; Roll angle is 1～3 °.
Embodiment 11
Adding the 52.175g particle diameter earlier in the 434.78g N,N-dimethylacetamide is the silicon-dioxide and the 13.045g fluorinated polyurethane of the hydrophobically modified of 80～100nm, obtains opaque super hydrophobic coating behind the Ball milling 300min at normal temperatures then.
The contact angle of this opaque super hydrophobic coating is 164～168 °; Roll angle is 1～3 °.
Claims (10)
1. super-hydrophobic nano-composite coating, it is characterized in that each set of dispense than by mass percentage is in this coating: hydrophobically modified silicon-dioxide 0.5～10.5%, hydrophobic polymeric material 0.2～5.4%, solvent 86.5～99.3%, and water droplet is 152～169 ° at the lip-deep contact angle of the film made from this coating, and roll angle is 1～9 °.
2. super-hydrophobic nano-composite coating according to claim 1, it is characterized in that each set of dispense than by mass percentage is in this coating: hydrophobically modified silicon-dioxide 0.5～3.1%, hydrophobic polymeric material 0.2～0.8%, solvent 96.1～99.3%, and the visible light transmissivity of the film made from this coating is 80～94%.
3. super-hydrophobic nano-composite coating according to claim 1 and 2 is characterized in that hydrophobic polymeric material in this coating is any in polydimethylsiloxane, polystyrene or the fluorinated polyurethane.
4. super-hydrophobic nano-composite coating according to claim 1 and 2 is characterized in that the solvent in this coating is toluene, dimethylbenzene, tetrahydrofuran (THF), N,N-dimethylacetamide or N, any in the dinethylformamide.
5. super-hydrophobic nano-composite coating according to claim 3 is characterized in that the solvent in this coating is toluene, dimethylbenzene, tetrahydrofuran (THF), N, N-methylacetamide or N, any in the dinethylformamide.
6. method for preparing each described super-hydrophobic nano-composite coating among the claim 1-5, it is characterized in that this method is with hydrophobically modified silicon-dioxide 0.5～10.5%, hydrophobic polymeric material 0.2～5.4%, solvent 86.5～99.3%, mechanical stirring or sonic oscillation dispersion at normal temperatures or Ball milling are uniformly dispersed it and get final product, and wherein the add-on of each component is mass percent.
7. the method for preparing super-hydrophobic nano-composite coating according to claim 6 is characterized in that hydrophobically modified silicon-dioxide used in this method is 0.5～3.1%, and hydrophobic polymeric material is 0.2～0.8%, and solvent is 96.1～99.3%.
8. according to claim 6 or the 7 described methods that prepare super-hydrophobic nano-composite coating, it is characterized in that hydrophobic polymeric material used in this method is any in polydimethylsiloxane, polystyrene or the fluorinated polyurethane.
9. according to claim 6 or the 7 described methods that prepare super-hydrophobic nano-composite coating, it is characterized in that solvent used in this method is toluene, dimethylbenzene, tetrahydrofuran (THF), N,N-dimethylacetamide or N, any in the dinethylformamide; Time with mechanical stirring, sonic oscillation or Ball milling is 30～300min.
10. the method for preparing super-hydrophobic nano-composite coating according to claim 8 is characterized in that solvent used in this method is toluene, dimethylbenzene, tetrahydrofuran (THF), N,N-dimethylacetamide or N, any in the dinethylformamide; Time with mechanical stirring, sonic oscillation or Ball milling is 30～300min.
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