CN101723601A - Method for preparing super-hydrophobic surface - Google Patents
Method for preparing super-hydrophobic surface Download PDFInfo
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- CN101723601A CN101723601A CN200810225360A CN200810225360A CN101723601A CN 101723601 A CN101723601 A CN 101723601A CN 200810225360 A CN200810225360 A CN 200810225360A CN 200810225360 A CN200810225360 A CN 200810225360A CN 101723601 A CN101723601 A CN 101723601A
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Abstract
The invention provides a method for preparing a super-hydrophobic surface. Firstly, mixed solution of polystyrene and polymethyl methacrylate is dip-coated on a substrate material, a settled layer is formed on the surface of the substrate after a solvent is volatilized, then the substrate material and the settled layer are soaked in cyclohexane, and a super-hydrophobic film with a coarse microstructure is formed on the surface of the substrate material through drying. A contact angle between the film and the water is more than 150 degrees, so the super-hydrophobic performance is achieved. The preparation method has the advantages of simple and convenient operation, simple equipment and cheap raw materials; the prepared super-hydrophobic surface film has excellent hydrophobic performance and stable property; and the preparation method can prepare the large-area super-hydrophobic film and perform scale production.
Description
Technical field
The present invention relates to a kind of preparation method of function interface, more particularly, relate to a kind of preparation method of super hydrophobic surface.
Background technology
Surface wettability is the very common surface phenomenon of a class, and it not only directly influences the various vital movements of occurring in nature biology, and also plays an important role in Human's production and life.Super hydrophobic surface brings great convenience for people's life as having a kind of form on special wetting property surface, for example can be used for the waterproof of waterproof, anti-caking mist and the outdoor radar of tiles in toilet, antifog, snow defence, dustproof etc.
At present, several different methods being arranged, adopts different materials, comprising: inorganic, organic and inorganic--the organic hybrid material prepares and has special infiltrating surface.Wherein superpolymer is a kind of important material of preparation super hydrophobic surface.
The method that adopts superpolymer to prepare super hydrophobic surface has a variety of.As: template synthesis method (L.Feng, Y.Song, J.Zhai, B.Liu, J.Xu, L.Jiang, D.Zhu, Angew.Chem.2003,115,824), electrospinning method (L.Jiang, Y.Zhao, J.Zhai, Angew.Chem.Int.Ed.2004,43,4338), solution methods (H.Y.Erbil, A.L.Demirel, Y.Avci, O.Mert, Science 2003,299,1377), silicon fluoride modifying method (A.Nakajima, A.Fujishima, K.Hashimoto, T.Watanabe, Adv.Mater.1999,11,1365) etc.But these methods or used raw material costliness, or the preparation condition harshness, waste time and energy, or be difficult to prepare even, large-area based superhydrophobic thin films, limited the practical application of aforesaid method.
In the prior art, Chinese patent CN1611305A adopts noncrystalline polymer to be separated into membrane technique in the solvent evaporates process, and preparation is coated in the super-hydrophobic polymeric coating layer on the solid surface; This method is simple, cost is low, but can't prepare uniform large-area super hydrophobic surface.Chinese patent CN 1613565A adopts inorganic materials to prepare the zinc oxide super-hydrophobic surface with wet chemistry method; This method technology is simple, raw material is easy to get, but making is more time-consuming, required time is long.Chinese patent CN 1621434A, the phase inversion process of employing solvent-precipitation agent is prepared super-hydrophobic cellular PVC film; This method is easy and simple to handle, equipment is simple, but adopts hydrophobic material to prepare super hydrophobic surface, and cost is higher.
Summary of the invention
In order to overcome when preparing based superhydrophobic thin films, material cost is higher, preparation process is complicated, preparation time is long, use the problem that is restricted, the invention provides a kind of preparation method of based superhydrophobic thin films, this method with the polymkeric substance that cheaply is easy to get as starting material, making processes is simple, Production Time is short, and practical application is convenient.
Preparation method of the present invention is achieved in that
A. preparation contains the mixing solutions of polystyrene and polymethylmethacrylate, and the solvent of described mixing solutions is: benzene, chloroform or pimelinketone;
B. clean the surface of super hydrophobic surface base material;
C. the mixing solutions dip-coating that step a is obtained is on the base material that cleans through step b;
D. dip-coating is at the mixing solutions of substrate material surface, at first pass through solvent evaporates, make deposition of solute in the mixing solutions at substrate material surface, to volatilize then settled layer that the back forms or with this settled layer together with base material immersion treatment in hexanaphthene, through super-dry, form based superhydrophobic thin films with coarse microtexture on the surface of base material.
In the specific implementation, at step a, the concentration of polystyrene (PS) and polymethylmethacrylate (PMMA) mixing solutions is 10~50wt%, and the weight ratio of polystyrene and polymethylmethacrylate is 40/60~60/40.At step b, described base material is glass, ceramic tile or metal.When step b cleaned, ultrasonic cleaning was adopted in described cleaning, generally can clean about 2 hours; Or at first use daily clean-out system to clean, adopt ultrasonic cleaning equipment to clean then.When the steps d immersion treatment, soaking temperature is 40~60 ℃, and soak time is 30~40min.
The microscopic appearance of the based superhydrophobic thin films that aforesaid method obtains adopts scanning electron microscope to characterize, and at room temperature measures the contact angle of film with video optics contact angle measurement.By scanning electron microscope, can be observed film surface and be the porous microtexture, the bird's nest that likeness in form is barricaded as by the ball and the branch of different sizes.The contact angle of film and water surpasses 150 ° (drop size is 2 μ l), shows good super-hydrophobicity (being called super hydrophobic surface greater than 150 ° surface with the contact angle of water).
The present invention is dissolved in a kind of solvent with two kinds of incompatible polymers and forms solution, the dip-coating film forming, two components are separated after the solvent evaporates, adopt then the selective solvent general wherein a kind of components dissolved fall, stay another kind of component and in substrate, form based superhydrophobic thin films.
This preparation method is simple, preparation time is short, cost is low, need not any complex apparatus, can prepare the big area based superhydrophobic thin films.The super-hydrophobicity film of preparation, surface are the bird's nest shape vesicular structure of micron and nano composite structure, and microtexture is coarse.And its super-hydrophobicity is still constant after the several months, shows good stability.
Description of drawings
Fig. 1. the stereoscan photograph of the based superhydrophobic thin films of embodiment 1 gained.
Fig. 2. the based superhydrophobic thin films of embodiment 1 gained and water contact angle photo.
Fig. 3. the stereoscan photograph of the based superhydrophobic thin films of embodiment 2 gained.
Fig. 4. the based superhydrophobic thin films of embodiment 2 gained and water contact angle photo.
Fig. 5. the stereoscan photograph of the based superhydrophobic thin films of embodiment 4 gained.
Fig. 6. the based superhydrophobic thin films of embodiment 4 gained and water contact angle photo.
Embodiment
Be described in further detail technical scheme of the present invention below in conjunction with embodiment, protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Compound concentration is the polystyrene (PS) of 10% (weight) and the solution of polymethylmethacrylate (PMMA), and the proportioning of PS and PMMA is 40/60 (weight), and solvent is a benzene.With the ceramic tile is base material, thoroughly cleans with washing composition before the preparation based superhydrophobic thin films, and ultrasonic cleaning is 2 hours then, water cleaning again, drying.With the polymers soln dip-coating film forming in substrate for preparing.After treating that solvent in the film fully volatilizees, place 50 ℃ hexanaphthene to soak 40min, take out the back and dries naturally, obtain based superhydrophobic thin films in clean room together with substrate.
The microscopic appearance of film adopts field emission scanning electron microscope (FE-SEM) to characterize.At room temperature measure the contact angle of film with video optics contact angle measurement.Measure take off data average (drop size is 2 μ l) respectively at 5 different positionss.
The contact angle of gained film and water is 155~165 degree.Survey its hydrophobicity after three months again, still constant.
The sem photograph and the water contact angle photo of preparation film are seen accompanying drawing 1 and accompanying drawing 2 under this condition.
Embodiment 2
Compound concentration is the polystyrene (PS) of 20% (weight) and the solution of polymethylmethacrylate (PMMA), and the proportioning of PS and PMMA is 50/50 (weight), and solvent is a benzene.Glass is base material, thoroughly cleans with washing composition before the preparation based superhydrophobic thin films, handles 2 hours in ultrasonic, cleans.With the polymers soln dip-coating film forming in substrate for preparing.After treating that solvent in the film fully volatilizees, place 55 ℃ hexanaphthene to soak 40min, take out the back and dries naturally, obtain based superhydrophobic thin films in clean room together with substrate.
The microscopic appearance of film adopts scanning electron microscope to characterize.At room temperature measure the contact angle of film with video optics contact angle measurement.Measure at 5 different positionss respectively, take off data is averaged, and wherein drop size is 2 μ l.
The contact angle of gained film and water is 150~160 degree.Survey its hydrophobicity after three months again, still constant.
The sem photograph and the water contact angle photo of preparation film are seen accompanying drawing 3 and accompanying drawing 4 under this condition.
Embodiment 3
Compound concentration is the polystyrene (PS) of 50% (weight) and the solution of polymethylmethacrylate (PMMA), and the proportioning of PS and PMMA is 50/50 (weight), and solvent is a chloroform.Metal is a base material, thoroughly cleans with washing composition before the preparation based superhydrophobic thin films, handles 2 hours in ultrasonic, cleans.With the polymers soln dip-coating film forming in substrate for preparing.After treating that solvent in the film fully volatilizees, place 60 ℃ hexanaphthene to soak 35min, take out the back and dries naturally, then obtain based superhydrophobic thin films in clean room together with substrate.
The microscopic appearance of film adopts scanning electron microscope to characterize, and at room temperature measures the contact angle of film with video optics contact angle measurement.Measure at 5 different positionss respectively, take off data is averaged, and wherein drop size is 2 μ l.
The contact angle of gained film and water is 150~155 degree.Survey its hydrophobicity after three months again, still constant.
Embodiment 4
Compound concentration is the polystyrene (PS) of 40% (weight) and the solution of polymethylmethacrylate (PMMA), and the proportioning of PS and PMMA is 60/40 (weight), and solvent is a pimelinketone.Glass is base material, thoroughly cleans with washing composition before the preparation based superhydrophobic thin films, handles 2 hours in ultrasonic, cleans.With the polymers soln dip-coating film forming in substrate for preparing.After treating that solvent in the film fully volatilizees, place 40 ℃ hexanaphthene to soak 40min, take out the back and dries naturally, then obtain based superhydrophobic thin films in clean room together with substrate.
The microscopic appearance of film adopts scanning electron microscope to characterize, and at room temperature measures the contact angle of film with video optics contact angle measurement.Measure at 5 different positionss respectively, take off data is averaged, and wherein drop size is 2 μ l.
The contact angle of gained film and water is 150~160 degree.Survey its hydrophobicity after three months again, still constant.
The sem photograph and the water contact angle photo of preparation film are seen accompanying drawing 5 and accompanying drawing 6 under this condition.
Embodiment 5
Compound concentration is the polystyrene (PS) of 30% (weight) and the solution of polymethylmethacrylate (PMMA), and the proportioning of PS and PMMA is 55/45 (weight), and solvent is a chloroform.Ceramic tile is a base material, thoroughly cleans with washing composition before the preparation based superhydrophobic thin films, handles 2 hours in ultrasonic, cleans.With the polymers soln dip-coating film forming in substrate for preparing.After treating that solvent in the film fully volatilizees, place 60 ℃ hexanaphthene to soak 30min, take out the back and dries naturally, then obtain based superhydrophobic thin films in clean room together with substrate.
The microscopic appearance of film adopts scanning electron microscope to characterize, and at room temperature measures the contact angle of film with video optics contact angle measurement.Measure at 5 different positionss respectively, take off data is averaged, and wherein drop size is 2 μ l.
The contact angle of gained film and water is 155~165 degree.Survey its hydrophobicity after three months again, still constant.
Table 1 is implementation condition and the contact angle summary sheet of embodiment 1~5.
Table 1
Embodiment | Strength of solution (weight %) | PS/PMMA (weight ratio) | Solvent | Substrate | The hexanaphthene temperature (℃) | The hexanaphthene treatment time (min) | The contact angle of film and water (degree) |
??1 | ??10 | ??40/60 | Benzene | Ceramic tile | ??50 | ??40 | ??155~165 |
??2 | ??20 | ??50/50 | Benzene | Glass | ??55 | ??40 | ??150~160 |
??3 | ??50 | ??50/50 | Chloroform | Metal | ??60 | ??35 | ??150~155 |
??4 | ??40 | ??60/40 | Pimelinketone | Glass | ??40 | ??40 | ??150~160 |
??5 | ??30 | ??55/45 | Chloroform | Ceramic tile | ??60 | ??30 | ??155~165 |
Claims (5)
1. the preparation method of a super hydrophobic surface, this preparation method may further comprise the steps:
A. preparation contains the mixing solutions of polystyrene and polymethylmethacrylate, and the solvent of described mixing solutions is: benzene, chloroform or pimelinketone;
B. clean the surface of super hydrophobic surface base material;
C. the mixing solutions dip-coating that step a is obtained is on the base material that cleans through step b;
D. dip-coating is at the mixing solutions of substrate material surface, at first pass through solvent evaporates, make deposition of solute in the mixing solutions at substrate material surface, the settled layer immersion treatment in hexanaphthene that will form after will volatilizing then, through super-dry, form based superhydrophobic thin films with coarse microtexture on the surface of base material.
2. preparation method according to claim 1 is characterized in that:
At step a, the concentration of polystyrene and polymethylmethacrylate mixing solutions is 10~50wt%, and the weight ratio of polystyrene and polymethylmethacrylate is 40/60~60/40.
3. preparation method according to claim 1 is characterized in that:
At step b, described base material is glass, ceramic tile or metal.
4. preparation method according to claim 3 is characterized in that:
When step b cleaned, ultrasonic cleaning was adopted in described cleaning.
5. preparation method according to claim 1 is characterized in that:
When the steps d immersion treatment, soaking temperature is 40~60 ℃, and soak time is 30~40min.
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Cited By (13)
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CN102174239A (en) * | 2011-02-24 | 2011-09-07 | 南京师范大学 | Polymethyl methacrylate with micro-nano topological structure and preparation method and application thereof |
CN102794113A (en) * | 2012-08-24 | 2012-11-28 | 中国科学院苏州纳米技术与纳米仿生研究所 | Super hydrophobic-supper lipophilic polymer porous film, preparation method and application thereof |
CN103066217A (en) * | 2013-01-18 | 2013-04-24 | 南京邮电大学 | Method for preparing super-hydrophobic film for encapsulating flexible organic luminescent device |
CN103700450A (en) * | 2012-09-27 | 2014-04-02 | 中国石油化工股份有限公司 | Method and equipment for manufacturing anti-icing metal high-voltage power line |
CN103728675A (en) * | 2013-12-31 | 2014-04-16 | 江苏大学 | Super-hydrophobic self-cleaning resin lens and manufacturing method thereof |
CN104228337A (en) * | 2013-06-20 | 2014-12-24 | 珠海纳思达企业管理有限公司 | Liquid ejecting head and liquid ejecting device |
CN109265719A (en) * | 2018-09-28 | 2019-01-25 | 蔡菁菁 | It is a kind of with super-hydrophobic, self-cleaning function fluorescent glass and preparation method |
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CN111440337A (en) * | 2020-04-22 | 2020-07-24 | 无锡嘉弘塑料科技有限公司 | Preparation method of hydrophobic polyvinyl chloride granules |
CN114105684A (en) * | 2021-09-11 | 2022-03-01 | 景德镇陶瓷大学 | Super-hydrophobic building ceramic tile and preparation method thereof |
CN114504954A (en) * | 2020-11-16 | 2022-05-17 | 中国石油化工股份有限公司 | Multilayer super-hydrophobic composite membrane and preparation method thereof |
CN115403977A (en) * | 2022-09-19 | 2022-11-29 | 青岛石创科技有限公司 | Surface material and super-hydrophobic composite application method |
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CN102174239A (en) * | 2011-02-24 | 2011-09-07 | 南京师范大学 | Polymethyl methacrylate with micro-nano topological structure and preparation method and application thereof |
CN102794113A (en) * | 2012-08-24 | 2012-11-28 | 中国科学院苏州纳米技术与纳米仿生研究所 | Super hydrophobic-supper lipophilic polymer porous film, preparation method and application thereof |
CN103700450B (en) * | 2012-09-27 | 2016-12-21 | 中国石油化工股份有限公司 | The preparation method of a kind of ice-covering-proof metal high voltage line and equipment |
CN103700450A (en) * | 2012-09-27 | 2014-04-02 | 中国石油化工股份有限公司 | Method and equipment for manufacturing anti-icing metal high-voltage power line |
CN103066217A (en) * | 2013-01-18 | 2013-04-24 | 南京邮电大学 | Method for preparing super-hydrophobic film for encapsulating flexible organic luminescent device |
CN103066217B (en) * | 2013-01-18 | 2015-05-06 | 南京邮电大学 | Method for preparing super-hydrophobic film for encapsulating flexible organic luminescent device |
CN104228337A (en) * | 2013-06-20 | 2014-12-24 | 珠海纳思达企业管理有限公司 | Liquid ejecting head and liquid ejecting device |
CN104228337B (en) * | 2013-06-20 | 2017-02-08 | 珠海赛纳打印科技股份有限公司 | Liquid ejecting head and liquid ejecting device |
CN103728675A (en) * | 2013-12-31 | 2014-04-16 | 江苏大学 | Super-hydrophobic self-cleaning resin lens and manufacturing method thereof |
CN103728675B (en) * | 2013-12-31 | 2015-08-26 | 江苏大学 | A kind of preparation method of super-hydrophobic automatic cleaning resin lens |
CN110577687A (en) * | 2018-06-08 | 2019-12-17 | 康美包(苏州)有限公司 | lyophobic film and preparation method and application thereof |
CN109265719A (en) * | 2018-09-28 | 2019-01-25 | 蔡菁菁 | It is a kind of with super-hydrophobic, self-cleaning function fluorescent glass and preparation method |
CN110384953A (en) * | 2019-07-26 | 2019-10-29 | 山东大学 | A kind of carbon dots modification sponge oil absorption material and preparation method thereof |
CN111440337A (en) * | 2020-04-22 | 2020-07-24 | 无锡嘉弘塑料科技有限公司 | Preparation method of hydrophobic polyvinyl chloride granules |
CN114504954A (en) * | 2020-11-16 | 2022-05-17 | 中国石油化工股份有限公司 | Multilayer super-hydrophobic composite membrane and preparation method thereof |
CN114504954B (en) * | 2020-11-16 | 2023-03-28 | 中国石油化工股份有限公司 | Multilayer super-hydrophobic composite membrane and preparation method thereof |
CN114105684A (en) * | 2021-09-11 | 2022-03-01 | 景德镇陶瓷大学 | Super-hydrophobic building ceramic tile and preparation method thereof |
CN115403977A (en) * | 2022-09-19 | 2022-11-29 | 青岛石创科技有限公司 | Surface material and super-hydrophobic composite application method |
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Application publication date: 20100609 |