CN101519278A - Method for preparing transparent super-hydrophobic automatic cleaning coating - Google Patents
Method for preparing transparent super-hydrophobic automatic cleaning coating Download PDFInfo
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- CN101519278A CN101519278A CN200910066706A CN200910066706A CN101519278A CN 101519278 A CN101519278 A CN 101519278A CN 200910066706 A CN200910066706 A CN 200910066706A CN 200910066706 A CN200910066706 A CN 200910066706A CN 101519278 A CN101519278 A CN 101519278A
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Abstract
The invention belongs to the technical field of preparing transparent super-hydrophobic coatings, in particular to a method for preparing a transparent, super-hydrophobic and automatic-cleaning coating on an arbitrary-shape substrate made of glass, quartz, and the like. The method for preparing a transparent super-hydrophobic automatic cleaning coating comprises the following steps: substrate processing, solution preparation, micro-nanometer composite structure assemblage, heat processing of the coating, modification of a hydrophobic substance, and the like. The method of the invention is not limited by the size and the shape of the substrate and is suitable for the substrates with flat surfaces, curve surfaces and irregular surfaces. The contact angle of the super-hydrophobic coating is larger than 150 DEG, and the rolling angle of the super-hydrophobic coating is smaller than 5 DEG. When falling on the glass, rain drops can rapidly roll off without being adhered to the glass and can take away the dust falling on the glass to keep the surface to be clean. The prepared coating has high transmission, and the average transmission is higher than 90 percent. The invention has simple technology and method, easy-obtained material and low cost, and is suitable for the occasions of windshields and lenses of automobiles and planes, curtain walls and glass of buildings, and the like.
Description
Technical field
The invention belongs to the transparent hydrophobic coating preparing technical field, particularly a kind of in arbitrary shape substrates such as glass, quartz the method for transparent, super-hydrophobic, the automatic cleaning coating of preparation.
Background technology
Super-hydrophobic phenomenon is very extensive at nature, and a lot of plants, animal, insect all have super-hydrophobic surface.Super hydrophobic surface refers generally to contact angle greater than 150 °, the roll angle surface less than 10 °.Super hydrophobic surface has the surface property of a lot of uniquenesses: as self-cleaning property, didirtresistance, hydrophobicity etc., make its in very life, production field all has great application prospect.
Transparent super-hydrophobic coat has good visible light permeability and hydrophobicity, and it is applied in glass surface, can prepare self-cleaning glass.This glass can be used as the windshield glass of automobile, aircraft, falls when on glass when rainwater, can tumble fast and does not stick on glass, take away simultaneously and drop on dust on glass, keep cleaning surfaces, guarantee the visual field in the rainy day driving procedure, improved drive safety; If transparent hydrophobic coating is applied in the surface of Highrise buildings and on glass, can reduce cleaning time, reduce the danger of cleaning cost and working aloft.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing the large-area transparent super-hydrophobic automatic cleaning coating simply and easily, this transparent super-hydrophobic automatic cleaning coating can be applied in complex surface, overcomes to prepare the shortcoming that transparent hydrophobic coating needs expensive instrument, preparation difficulty in the current techniques.
The step of the method for the invention is as follows:
1. the processing of substrate: the method for the invention is not subjected to the influence of the shape and the size of substrate, and the substrate of plane, curved surface or irregular surface is all applicable, and the typical substrate that suitable the present invention uses is glass and quartz.At first, substrate is cleaned by polarity of solvent from small to large with the different solvent of several polarity successively, as cleaning with toluene, acetone, chloroform, ethanol and distilled water successively; Then, again through H
2O
2And H
2SO
4Mixing solutions handle can be so that the surface of substrate has one deck silicon hydroxyl;
2. the preparation of coating solution: the inorganic nano-particle that will have negative charge is dissolved in the solvent, is made into the inorganic nano-particle solution that concentration is 1.0～10.0mg/mL in ultrasonic 20～60 minutes; Again cationic polymers is dissolved in the deionized water, is prepared into the solution that concentration is 1.0～10.0mg/mL;
3. the preparation of micro-nano compound surface: the substrate that step 1 was handled alternately is immersed in two kinds of prepared solution of step 2 each 3～20 minutes, after each the immersion substrate taken out and with deionized water rinsing, dry up, thereby finish the preparation of the layered assembling film of one-period; Repeat said process, thereby in substrate, utilize the stratiform package technique to prepare the multilayer micro-nano compound structure coating of different roughness;
4. the thermal treatment of coating: will have the substrate of multilayer micro-nano compound structure coating to put into retort furnace by the preparation that step 3 obtains and under 400 ℃～600 ℃ temperature condition, heat 1～3 hour, remove organic components, and make inorganic nano-particle crosslinked to increase the stability of coating;
5. the modification of hydrophobic substance: the substrate that step 4 obtains is carried out chemical vapour deposition again under 100 ℃～150 ℃ temperature condition, the molecular modification that will contain hydrophobic chain is at coatingsurface, thereby obtains transparent super-hydrophobic automatic cleaning coating in substrate.
The inorganic nano-particle that has negative charge of the present invention is TiO
2, CaCO
3Or SiO
2Deng, particle diameter is between 10～50nm;
The solvent that is used for dissolving inorganic nano-particle of the present invention is the mixed solvent of a kind of and deionized water of acetone, ethanol, methyl alcohol or Virahol, and by volume the usage ratio of acetone, ethanol, methyl alcohol or Virahol and deionized water is 1:1～1:8;
The used cationic polymers of the present invention is polydimethyl diallyl amine hydrochlorate or polypropylene amine;
The used molecule that contains hydrophobic chain of the present invention is tetrahydrochysene perfluor C
4～C
16Alkyl trimethyl silane or tetrahydrochysene perfluor C
4～C
16Alkyltrialkoxysilaneand.
Compared with prior art, the invention has the advantages that:
1. technology is simple, and raw material is easy to get, and cost is low;
2. can in the substrate of on-plane surface complex construction, prepare transparent hydrophobic coating;
3. Zhi Bei transparent hydrophobic, contact angle is greater than 150 °, and roll angle has good self-cleaning property less than 5 °;
4. Zhi Bei super-hydrophobic glass has good visible light permeability, and average visible light transmissivity is up to more than 90%.
Description of drawings
Fig. 1: embodiment 1 gained transparent hydrophobic surface field emission scanning electron microscope figure;
Fig. 2: embodiment 1 gained transparent hydrophobic surface contact angle state graph;
The transmittance curve figure (dotted line) of the glass of Fig. 3: embodiment 1 gained transparent hydrophobic glass transmitance (solid line) and unmodified transparent hydrophobic coating;
Fig. 4: embodiment 1 gained transparent hydrophobic glass pictorial diagram;
Fig. 5: embodiment 2 gained transparent hydrophobic surface contact angle state graphs;
Fig. 6: embodiment 3 gained transparent hydrophobic surface contact angle state graphs.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Field emission scanning electron microscope figure is obtained by XL30 ESEM FEG type field emission scanning electron microscope.
Contact angle is recorded by Dataphysics OCA20 type contact angle measurement.
Visible light transmissivity is recorded by Shimadzu UV-3600 UV, visible light optical measuring instrument.
Embodiment 1:
(1) processing of substrate:
The sheet glass of surface level is used toluene, acetone, chloroform, ethanol and distilled water supersound process 10min respectively successively, to remove the various impurity that substrate surface adheres to, is 98% H in mass concentration then
2SO
4With mass concentration be 30% H
2O
2(v:v=7:3) heated and boiled 20min does not overflow to there being bubble in the mixing solutions, and a large amount of distilled water flushings are used in the cooling back, dry up with nitrogen again, and are stand-by.
(2) preparation of solution:
With the 0.3g particle diameter is the SiO of the Sigma-Al drich company production of 10nm
2Inorganic nano-particle is dissolved in the mixing solutions of 100mL Virahol and deionized water, and the volume ratio of Virahol and deionized water is 1:4, makes SiO in ultrasonic 30 minutes
2Nanoparticle is uniformly dispersed, and is stand-by; 0.2g polydimethyl diallyl amine hydrochlorate is dissolved in the 100mL deionized water, dissolving evenly back is stand-by again.
(3) preparation of micro-nano compound surface:
Soaked 20 minutes in the polydimethyl diallyl amide hydrochloride that the substrate of glass of handling well in the step (1) is prepared in step (2), take out washing and dry up; And then the SiO of preparation in step (2)
2Soaked 10 minutes in the solution, take out washing and dry up; Dry up stand-by after above process repeats 4 times.
(4) thermal treatment of coating:
To put into retort furnace by the glass that deposits 4 layers of micro-nano compound structure coating that step (3) obtains and under 400 ℃ of temperature condition, heat 3 hours, remove organic components, as shown in Figure 1, obtain SiO
2Sintering micro-nano compound structure together, its dimensional structure is between 400nm～800nm.
(5) decorating hydrophobic substances:
The glass that step (4) obtains is put into baking oven, carried out chemical vapour deposition 1 hour under 100 ℃ of temperature condition, the tetrahydrochysene perfluor dodecyl trimethyl silane that Degussa company is produced is modified at the micro-nano compound structure surface, obtains transparent hydrophobic glass.
As shown in Figure 2, prepared transparent hydrophobic glass, its contact angle are 157 °, and have good perviousness.As shown in Figure 3, not modified glass, its transmitance is (dotted line) about 93%.Be modified with the glass of transparent hydrophobic coating, in the visible-range more than the 500nm wavelength, its transmitance is all than simple glass height; Scope below 500nm because micro-nano compound structure is more serious to the scattering of light of this wave band, has caused transmitance to reduce slightly.(solid line) carries out integration to curve, obtains its average transmittances up to more than 93%, can not influence the transmitance of original glass.Transparent hydrophobic glass pictorial diagram is placed on resulting transparent hydrophobic glass 2 on the paper 1 of literal 4 as shown in Figure 4, and following literal 4 is high-visible, and water droplet 3 do not soak into from the teeth outwards, and slight vibrations will tumble from the surface.
Embodiment 2:
(1) processing of substrate:
With the sheet glass of surface level successively with the ultrasonic 10min that handles respectively of toluene, acetone, chloroform, ethanol and distilled water, to remove the various impurity that substrate surface adheres to, then at the H of mass concentration 98%
2SO
4H with mass concentration 30%
2O
2Heated and boiled in the mixing solutions (v:v=7:3) (～20min) do not overflow to there being bubble.A large amount of distilled water flushings are used in the cooling back, dry up with nitrogen again, and are stand-by.
(2) formulations prepared from solutions:
With the 0.4g particle diameter is the TiO of the Sigma-Aldrich company production of 20nm
2Nanoparticle is dissolved in the mixture of 100mL acetone and deionized water, and the volume ratio of acetone and deionized water is 1:2, makes TiO in ultrasonic 20 minutes
2Nanoparticle is uniformly dispersed, and is stand-by; The 0.3g polypropylene amine is dissolved in the 100mL water, and dissolving evenly back is stand-by.
(3) micro-nano compound surface preparation:
The substrate of glass of handling well in the step (1) was soaked 20 minutes in the polypropylene amine solution of step (2) preparation, take out washing and dry up; And then at the TiO of step (2) preparation
2Soaked 10 minutes in the solution, take out washing and dry up.Dry up stand-by after above process repeats 3 times.
(4) coating thermal treatment:
The glass of the micro-nano compound structure coating that will have three layers by the deposition that step (3) obtains is put into retort furnace and was heated 3 hours under 450 ℃ of temperature condition, removes organic components, and makes TiO
2Sintering together.
(5) decorating hydrophobic substances:
The glass that step (4) was handled is put into baking oven, under 130 ℃ of temperature condition, carried out chemical vapour deposition 1 hour, tetrahydrochysene perfluor ten alkyl trimethyls that Degussa company produces are hydride modified on the micro-nano compound structure surface, obtain transparent hydrophobic glass.As shown in Figure 5, prepared transparent hydrophobic glass, its contact angle are 156 °, and average transmittances is 90%.
Embodiment 3:
(1) processing of substrate:
With the quartz plate of surface level successively with the ultrasonic 10min that handles respectively of toluene, acetone, chloroform, ethanol and distilled water, to remove the various impurity that substrate surface adheres to, then at the H of mass concentration 98%
2SO
4H with mass concentration 30%
2O
2Heated and boiled in the mixing solutions (v:v=7:3) (～20min) do not overflow to there being bubble.A large amount of distilled water flushings are used in the cooling back, dry up with nitrogen again, and are stand-by.
(2) formulations prepared from solutions:
With the 0.4g particle diameter is the SiO of the Sigma-Aldrich company production of 14nm
2Nanoparticle is dissolved in the mixture of 100mL ethanol and deionized water, and the volume ratio of ethanol and deionized water is 1; 2, made SiO in ultrasonic 40 minutes
2Nanoparticle is uniformly dispersed, and is stand-by; The 0.5g polypropylene amine is dissolved in the 100mL water, and dissolving evenly back is stand-by.
(3) micro-nano compound surface preparation:
The quartz plate substrate of handling well in the step (1) was soaked 20 minutes in the polypropylene amine solution of step (2) preparation, take out washing and dry up; And then at the SiO of step (2) preparation
2Soaked 10 minutes in the solution, take out washing and dry up.Dry up stand-by after above process repeats 5 times.
(4) coating thermal treatment:
The quartz plate of the micro-nano compound structure coating that will be of five storeys by the deposition that step (3) obtains is put into retort furnace and was heated 2 hours under 500 ℃ of temperature condition, removes organic components, and makes SiO
2Sintering together.
(5) decorating hydrophobic substances:
The quartz plate that step (4) was handled is put into baking oven, under 120 ℃ of temperature condition, carried out chemical vapour deposition 2 hours, the tetrahydrochysene perfluor undecyl triethoxyl silane that Degussa company is produced is modified at the micro-nano compound structure surface, obtains the transparent hydrophobic quartz plate.As shown in Figure 6, prepared transparent hydrophobic quartz plate, its contact angle are 158 °, and average transmittances is 91%.
Claims (9)
1, a kind of method for preparing transparent super-hydrophobic automatic cleaning coating, its step is as follows:
A. the processing of substrate: substrate is cleaned by polarity of solvent from small to large with the different solvent of several polarity successively, and then through H
2O
2And H
2SO
4Mixing solutions handle, make the surface of substrate have one deck silicon hydroxyl;
B. the preparation of coating solution: electronegative inorganic nano-particle is dissolved in the solvent, was made into the inorganic nano-particle solution that concentration is 1.0～10.0mg/mL in ultrasonic 20～60 minutes; Again cationic polymers is dissolved in the deionized water, is prepared into the solution that concentration is 1.0～10.0mg/mL;
C. the preparation of micro-nano compound surface: the substrate that processing of step A is crossed alternately is immersed in two kinds of prepared solution of step B each 3～20 minutes, after each the immersion substrate taken out and with deionized water rinsing, dry up, thereby finish the preparation of the layered assembling film of one-period; Repeat said process, thereby in substrate, utilize the stratiform package technique to prepare the multilayer micro-nano compound structure coating of different roughness;
D. the thermal treatment of coating: will have the substrate of multilayer micro-nano compound structure coating to put into retort furnace by the preparation that step C obtains and under 400 ℃～600 ℃ temperature condition, heat 1～3 hour, remove organic components, and make inorganic nano-particle crosslinked to increase the stability of coating;
E. the modification of hydrophobic substance: the substrate that step D obtains is carried out chemical vapour deposition again under 100 ℃～150 ℃ temperature condition, the molecular modification that will contain hydrophobic chain is at coatingsurface, thereby obtains transparent super-hydrophobic automatic cleaning coating in substrate.
2, a kind of method for preparing transparent super-hydrophobic automatic cleaning coating as claimed in claim 1, it is characterized in that: inorganic nano-particle is TiO
2, CaCO
3Or SiO
2
3, a kind of method for preparing transparent super-hydrophobic automatic cleaning coating as claimed in claim 1 or 2, it is characterized in that: the particle diameter of inorganic nano-particle is between 10～50nm.
4, a kind of method for preparing transparent super-hydrophobic automatic cleaning coating as claimed in claim 1, it is characterized in that: the solvent of dissolving inorganic nano-particle is the mixed solvent of a kind of and deionized water in acetone, ethanol, methyl alcohol or the Virahol, and the usage ratio with deionized water is 1:1～1:8 by volume.
5, a kind of method for preparing transparent super-hydrophobic automatic cleaning coating as claimed in claim 1, it is characterized in that: cationic polymers is polydimethyl diallyl amine hydrochlorate or polypropylene amine.
6, a kind of method for preparing transparent super-hydrophobic automatic cleaning coating as claimed in claim 1 is characterized in that: the molecule that contains hydrophobic chain is tetrahydrochysene perfluor C
4～C
16Alkyl trimethyl silane or tetrahydrochysene perfluor C
4～C
16Alkyltrialkoxysilaneand.
7, a kind of method for preparing transparent super-hydrophobic automatic cleaning coating as claimed in claim 1, it is characterized in that: substrate is the substrate of plane, curved surface or irregular surface.
8, a kind of method for preparing transparent super-hydrophobic automatic cleaning coating as claimed in claim 1, it is characterized in that: substrate is glass or quartz.
9, a kind of method for preparing transparent super-hydrophobic automatic cleaning coating as claimed in claim 1, it is characterized in that: the solvent that several polarity are different is followed successively by with toluene, acetone, chloroform, ethanol and distilled water and cleans.
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|---|---|---|---|
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|---|---|---|---|
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| CN111944379A (en) * | 2020-08-25 | 2020-11-17 | 上海大学 | Application of carbohydrate-based block copolymer self-assembled micro-nano structure in anti-icing |
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| CN112744783B (en) * | 2021-01-06 | 2024-04-09 | 南京大学 | Preparation method of super-hydrophobic and super-oleophobic surface with micro-nano composite structure |
| CN114150312A (en) * | 2021-11-02 | 2022-03-08 | 四川艾庞机械科技有限公司 | Preparation method of super-hydrophobic aluminum alloy surface layer |
| CN115028372A (en) * | 2022-06-27 | 2022-09-09 | 四川大学 | Preparation method of self-cleaning crystal product |
| WO2024021971A1 (en) * | 2022-07-28 | 2024-02-01 | 华为技术有限公司 | Light-transmitting plate, structural member, and light sensing apparatus |
| CN115403276A (en) * | 2022-09-29 | 2022-11-29 | 南京信息职业技术学院 | Preparation method of transparent super-smooth surface based on glass matrix |
| CN115403276B (en) * | 2022-09-29 | 2023-09-22 | 南京信息职业技术学院 | Preparation method of transparent super-smooth surface based on glass matrix |
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