CN103951277B - A kind of super lyophoby anti-reflective glass upper layer and preparation method thereof - Google Patents
A kind of super lyophoby anti-reflective glass upper layer and preparation method thereof Download PDFInfo
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- CN103951277B CN103951277B CN201410182709.8A CN201410182709A CN103951277B CN 103951277 B CN103951277 B CN 103951277B CN 201410182709 A CN201410182709 A CN 201410182709A CN 103951277 B CN103951277 B CN 103951277B
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Abstract
A kind of super lyophoby anti-reflective glass upper layer and preparation method thereof, the invention belongs to field of novel, belongs to automatically cleaning optical material field especially.The present invention first passes through CF
3/ O
2plasma etching glass body surface, obtain the lower floor's submicron coarse structure in the surperficial micro-nano two-stage structure needed for super lyophoby, then one kettle way generates fluorine-containing hydridization SiO
2nano coating liquid, the twin-stage that a step dip-coating direct construction becomes to have overhung structure fluoridizes abrasive glass upper layer, while ensureing that upper layer surpasses lyophoby antireflection premium properties, avoids and fluoridizes aftertreatment, effectively simplify processing step.In addition, lower floor's submicrometer structure of twin-stage coarse structure is directly built by glass body to form, the then fluorine-containing hydridization SiO of chemical bonding one deck
2nanostructure, can avoid the double-deck short texture of prior art, substantially increase the physical strength of upper layer, obtains the glass surface that stability is high, wearing quality is strong, and technique is simple, is easy to industrialization.
Description
Technical field
A kind of super lyophoby anti-reflective glass upper layer and preparation method thereof, the invention belongs to field of novel, belongs to automatically cleaning optical material field especially.Be specifically related to the preparation of inorganic nano material, the preparation of optical coating film, technical field of surface.
Background technology
Taking lotus leaf as the self-cleaning surface effect of representative, be called as " lotus leaf effect ", is caused by the mastoid process of the micron-nanometer composite structure on uneven surface and the waxy substance acting in conjunction of surface hydrophobicity.These self-cleaning surfaces have good super-hydrophobicity, and stronger contamination resistance, and namely surface contaminant can be taken away by the water droplet tumbled as dust etc. and not leave any vestige.Automatic cleaning coating or lyophoby coating have the advantages such as water saving, energy-saving and environmental protection, more and more get more and more people's extensive concerning, and are one of focuses of current material subject research.
Surface wettability generally describes with contact angle, for a given system, has two basic methods to increase contact angle, improves the lyophobicity (not only hydrophobic but also oleophobic) on surface.One is reduce surface free energy by changing surface chemistry, is usually referred to as the method for chemically modified; Another kind is exactly increase surfaceness thus increase surface energy, is referred to as method of geometry.In order to obtain super lyophobic surface, the method that usual mating surface chemically modified and surfaceness strengthen.For chemical process, fluorine is the element effectively reducing surface free energy most, and therefore, conventional fluoropolymer is modified and obtained high performance lyophoby film and coating; But be only physical adsorption between the most base materials of prior art and fluorine-based hydrophobic coating, bonding force is very weak; On the other hand, also can change contact angle by building suitable surfaceness, improving the lyophobicity on surface.The increase of surfaceness can increase surface-area, thus increases apparent surface free energy, and according to Young's equation, in order to the surface energy increased between equilibrium solid base material and drop, contact angle must correspondingly increase.Although surfaceness is larger, hydrophobic performance is better, and roughness is larger, and surface reflection is stronger, causes transmittance to reduce.Therefore control surface roughness, to balance transmittance and these two factors of vying each other of roughness, preparing super lyophoby antireflecting coating is a technical barrier.Current bibliographical information mainly concentrates on super-hydrophobic coat, relate to super-hydrophobic transparent coating or super-hydrophobic super oleophobic coating on a small quantity, these artificial constructed two (many) heavy micro-nano compounds rough layer aggregated(particle) structures are while raising coatingsurface hydrophobic oleophobic performance, what have reduces transmittance, have due between base material and micro-nano compound coarse structure and micro-nano compound coarse structure internal bond strength mostly be physical adsorption, thus bonding force is weak, bad mechanical property, wearing quality is inadequate, unstable properties, What is more easily comes off, be difficult to use in severe environment, its practical value is had a greatly reduced quality.
Super lyophoby anti-reflective glass upper layer; there is frost prevention, antifog, antipollution, antibacterial self-cleaning performance; and have excellent light transmission concurrently; in rugged environment, the performance of optical element, optoelectronic component, solar cell and laser system effectively can be protected not by the impact of environment; greatly widen the use range of these equipment; ensure work reliability and increase the service life, thus improving the practical value of these equipment significantly.Therefore build that to have super lyophoby antireflecting, the surface layer of glass that high mechanical strength, high stability, wearing quality are strong, is a technical problem urgently to be resolved hurrily, has important actual application value.
Summary of the invention
The object of the invention is the defect existed to solve prior art, a kind of super lyophoby anti-reflective glass upper layer and preparation method thereof is provided, excellent transmittance and high mechanical strength is had concurrently while making gained surface layer of glass have super-hydrophobic super oleophobic self-cleaning performance, realize stability high, wearing quality is strong, there is the self-cleaning glass upper layer of actual application value, effectively optical element can be protected in rugged environment, optoelectronic component, the performance of solar cell and laser system is not by the impact of environment, greatly widen the use range of these equipment, ensure its work reliability and extend its work-ing life, thus improve the practical value of these equipment significantly.
Technical scheme of the present invention: a kind of super lyophoby anti-reflective glass upper layer and preparation method thereof, realizes by following technical scheme: first pass through CF
3/ O
2plasma etching glass body surface, to obtain the lower floor's submicron coarse structure in the twin-stage micro-nano structure needed for super lyophobic surface layer, then generates fluorine-containing hydridization SiO by one kettle way
2nano sol coating solution, what one step dip-coating direct construction became to have an overhung structure fluoridizes twin-stage abrasive glass upper layer, obtain described super lyophoby anti-reflective glass upper layer, liquid can be effectively stoped to enter in the hole of sub-surface, make air trapping in hole, the compound surface that formation solid and air form, improves lyophoby ability and the antireflection ability of upper layer greatly.
A preparation method for super lyophoby anti-reflective glass upper layer, specifically comprises the steps:
The preparation on submicron order abrasive glass surface: substrate of glass is ultrasonic 20min in deionized water and dehydrated alcohol respectively, obtains cleaning glass substrate; At radio frequency 13.56MHz, CHF
3: O
2volume ratio is 4:1, and mixture pressure is 80 ~ 100Pa, and power is 1.8 ~ 2.0W/cm
2condition under, plasma etching is carried out to cleaning glass surface, obtain submicron order abrasive glass surface;
Assemble fluorine-containing hydridization SiO
2nano coating: tetraethoxy: dimethyldiethoxysilane volume ratio is the mixing solutions 3mL of 2:1, joins in 60mL dehydrated alcohol, stirs; Then, by dimethyldiethoxysilane: fluorine containing silane mol ratio is that 17:3 adds fluorine containing silane, stirs, obtains mixed silanes solution; Then be added drop-wise in above-mentioned mixed silanes solution by strong aqua (25wt%) 1.0 ~ 1.5mL, stirring at room temperature 1 ~ 2h, places aging 48h; Before using, dilute by 1:1 volume ratio dehydrated alcohol, stir, obtain fluorine-containing hydridization SiO
2nano coating liquid; Fluorine-containing hydridization SiO is immersed with the speed of 50mm/min in gained submicron order abrasive glass surface
2in nano coating liquid, stop 15min, then at the uniform velocity lift plated film with the speed of 200mm/min, by the diaphragm of preparation in the loft drier of 50 DEG C after dry 1h, thermal treatment 1 ~ 2h at 110 DEG C, obtains described super lyophoby anti-reflective glass upper layer.
Described fluorine containing silane is preferably: 1H, 1H, 2H, 2H-perfluoro decyl Trimethoxy silane (CF
3(CF
2)
7cH
2cH
2si (OCH
3)
3) or 1H, 1H, 2H, 2H-perfluoro decyl triethoxyl silane (CF
3(CF
2)
7cH
2cH
2si (OCH
2cH
3)
3).
A kind of super lyophoby anti-reflective glass upper layer prepared according to above-mentioned preparation method.
Beneficial effect of the present invention is: compared with prior art, and the present invention first passes through CF
3/ O
2plasma etching glass body surface, to obtain the lower floor's submicron coarse structure in the surperficial twin-stage micro-nano structure needed for super-hydrophobic super oleophobic, then generates fluorine-containing hydridization SiO by one kettle way
2nano coating liquid, the twin-stage that one step dip-coating direct construction becomes to have overhung structure fluoridizes abrasive glass upper layer, the later stage eliminating employing usually in prior art fluoridizes modification with the step reducing surface free energy, while ensureing that upper layer surpasses lyophoby antireflection premium properties, effectively simplify processing step.Gained water contact angle >=157 °, roll angle≤7 °; Contact angle >=150 ° of sunflower seed oil, roll angle≤10 °, test fluid is 5 μ L; Average transmittance > 92%, peak value transmittance is maximum reaches 95.3%.In addition, lower floor's submicrometer structure of the micro-nano structure needed for super lyophoby is directly built by glass body to form, then chemical bonding one deck nanostructure, thus avoid the double-deck short texture of prior art, substantially increase the physical strength of upper layer, obtain the glass surface that stability is high, wearing quality is strong, hardness and sticking power reach best 6H and 5B level level respectively, and operating procedure is simple, is easy to industrialization.This super lyophoby anti-transmitting surface layer of glass and preparation method thereof all belongs to initiative work.
Accompanying drawing explanation
Fig. 1 is water contact angle (1) and the sunflower seed oil contact angle (2) that the embodiment of the present invention 2 gained surpasses lyophoby anti-reflective glass upper layer.
Fig. 2 is transmittance-wavelength graph that the embodiment of the present invention 2 gained surpasses lyophoby anti-reflective glass upper layer, and wherein 1 is super lyophoby anti-reflective glass upper layer, and 2 is substrate of glass.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but scope of the present invention is not limited thereto.
Embodiment 1
The present embodiment is the preparation of super lyophoby anti-reflective glass upper layer.Substrate of glass is ultrasonic 20min in deionized water and dehydrated alcohol respectively, obtains cleaning glass substrate; At radio frequency 13.56MHz, CHF
3: O
2volume ratio is 4:1, and mixture pressure is 80Pa, and power is 1.8W/cm
2condition under, plasma etching is carried out to cleaning glass surface, obtain submicron order abrasive glass surface; 2mL tetraethoxy (Si (OCH
2cH
3)
4) and 1mL dimethyldiethoxysilane ((CH
3)
2si (OCH
2cH
3)
2) mixing, join in 60mL dehydrated alcohol, stir; Then, add 1H, 1H, 2H, 2H-perfluoro decyl Trimethoxy silane 0.001mol, stirs, obtains mixed silanes solution; Then be added drop-wise in above-mentioned mixed silanes solution by strong aqua (25wt%) 1.0mL, stirring at room temperature 1h, places aging 48h; Before using, add the dilution of 64mL dehydrated alcohol, stir, obtain fluorine-containing hydridization SiO
2nano coating liquid; Fluorine-containing hydridization SiO is immersed with the speed of 50mm/min in described submicron order abrasive glass surface
2in nano coating liquid, stop 15min, then at the uniform velocity lift plated film with the speed of 200mm/min, by the diaphragm of preparation in the loft drier of 50 DEG C after dry 1h, thermal treatment 1h at 110 DEG C, i.e. obtained described super lyophoby anti-reflective glass upper layer on the glass substrate.The water contact angle (5 μ L) of gained surface layer of glass is: 157 °, roll angle is 5 °; Sunflower seed oil contact angle (5 μ L) is: 150 °, roll angle is: 9 °; Average transmittance is greater than 92%, and peak value transmittance is 94.7%.
Embodiment 2
The present embodiment is the preparation of super lyophoby anti-reflective glass upper layer.Substrate of glass is ultrasonic 20min in deionized water and dehydrated alcohol respectively, obtains cleaning glass substrate; At radio frequency 13.56MHz, CHF
3: O
2volume ratio is 4:1, and mixture pressure is 90Pa, and power is 1.9W/cm
2condition under, plasma etching is carried out to cleaning glass surface, obtain submicron order abrasive glass surface; 2mL tetraethoxy (Si (OCH
2cH
3)
4) and 1mL dimethyldiethoxysilane ((CH
3)
2si (OCH
2cH
3)
2) mixing, join in 60mL dehydrated alcohol, stir; Then, add 1H, 1H, 2H, 2H-perfluoro decyl triethoxyl silane 0.001mol, stirs, obtains mixed silanes solution; Then be added drop-wise in above-mentioned mixed silanes solution by strong aqua (25wt%) 1.2mL, stirring at room temperature 1.5h, places aging 48h; Before using, add the dilution of 64.2mL dehydrated alcohol, stir, obtain fluorine-containing hydridization SiO
2nano coating liquid; Fluorine-containing hydridization SiO is immersed with the speed of 50mm/min in described submicron order abrasive glass surface
2in nano coating liquid, stop 15min, then at the uniform velocity lift plated film with the speed of 200mm/min, by the diaphragm of preparation in the loft drier of 50 DEG C after dry 1h, thermal treatment 1.5h at 110 DEG C, namely obtains described super lyophoby anti-reflective glass upper layer on the glass substrate.The water contact angle (5 μ L) of gained surface layer of glass is: 158 °, roll angle is 7 °; Sunflower seed oil contact angle (5 μ L) is: 151 °, roll angle is: 7 °; Average transmittance is greater than 92%, and peak value transmittance is 95.0%.The water contact angle (1) of gained surface layer of glass and sunflower seed oil contact angle (2), be shown in Fig. 1; Transmittance-wavelength graph is shown in Fig. 2, and wherein 1 is super lyophoby anti-reflective glass upper layer, and 2 is substrate of glass.
Embodiment 3
The present embodiment is the preparation of super lyophoby anti-reflective glass upper layer.Substrate of glass is ultrasonic 20min in deionized water and dehydrated alcohol respectively, obtains cleaning glass substrate; At radio frequency 13.56MHz, CHF
3: O
2volume ratio is 4:1, and mixture pressure is 100Pa, and power is 2.0W/cm
2condition under, plasma etching is carried out to cleaning glass surface, obtain submicron order abrasive glass surface; 2mL tetraethoxy (Si (OCH
2cH
3)
4) and 1mL dimethyldiethoxysilane ((CH
3)
2si (OCH
2cH
3)
2) mixing, join in 60mL dehydrated alcohol, stir; Then, add 1H, 1H, 2H, 2H-perfluoro decyl Trimethoxy silane 0.001mol, stirs, obtains mixed silanes solution; Then be added drop-wise in above-mentioned mixed silanes solution by strong aqua (25wt%) 1.5mL, stirring at room temperature 2h, places aging 48h; Before using, add the dilution of 64.5mL dehydrated alcohol, stir, obtain fluorine-containing hydridization SiO
2nano coating liquid; Fluorine-containing hydridization SiO is immersed with the speed of 50mm/min in described submicron order abrasive glass surface
2in nano coating liquid, stop 15min, then at the uniform velocity lift plated film with the speed of 200mm/min, by the diaphragm of preparation in the loft drier of 50 DEG C after dry 1h, thermal treatment 2h at 110 DEG C, i.e. obtained described super lyophoby anti-reflective glass upper layer on the glass substrate.The water contact angle (5 μ L) of gained surface layer of glass is: 159 °, roll angle is 6 °; Sunflower seed oil contact angle (5 μ L) is: 152 °, roll angle is: 10 °; Average transmittance is greater than 92%, and peak value transmittance is 95.3%.
Embodiment 4
The present embodiment is hardness and the sticking power test of super lyophoby anti-reflective glass upper layer.According to standard A STMD3363-05 and D3359-09 standard operation method, adopt hardness and the sticking power of pencil hardness method and cross cut test method difference test chart surface layer, the results are shown in Table 1.
Table 1
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, without departing from the inventive concept of the premise; can also make some improvements and modifications, these improvements and modifications also should be considered within the scope of protection of the present invention.
Claims (3)
1. a preparation method for super lyophoby anti-reflective glass upper layer, is characterized in that, comprise the steps:
(1) preparation on submicron order abrasive glass surface: substrate of glass is ultrasonic 20min in deionized water and dehydrated alcohol respectively, obtains cleaning glass substrate; At radio frequency 13.56MHz, CHF
3: O
2volume ratio is 4:1, and mixture pressure is 80 ~ 100Pa, and power is 1.8 ~ 2.0W/cm
2condition under, plasma etching is carried out to cleaning glass surface, obtain submicron order abrasive glass surface;
(2) fluorine-containing hydridization SiO is assembled
2nano coating: tetraethoxy: dimethyldiethoxysilane volume ratio is the mixing solutions 3mL of 2:1, joins in 60mL dehydrated alcohol, stirs; Then, by dimethyldiethoxysilane: fluorine containing silane mol ratio is that 17:3 adds fluorine containing silane, stirs, obtains mixed silanes solution; Then be added drop-wise in above-mentioned mixed silanes solution by the strong aqua 1.0 ~ 1.5mL of 25wt%, stirring at room temperature 1 ~ 2h, places aging 48h; Before using, dilute by 1:1 volume ratio dehydrated alcohol, stir, obtain fluorine-containing hydridization SiO
2nano coating liquid; Fluorine-containing hydridization SiO is immersed with the speed of 50mm/min in gained submicron order abrasive glass surface
2in nano coating liquid, stop 15min, then at the uniform velocity lift plated film with the speed of 200mm/min, by the diaphragm of preparation in the loft drier of 50 DEG C after dry 1h, thermal treatment 1 ~ 2h at 110 DEG C, obtains described super lyophoby anti-reflective glass upper layer.
2. the preparation method of a kind of super lyophoby anti-reflective glass upper layer according to claim 1, is characterized in that described fluorine containing silane is preferably: 1H, 1H, 2H, 2H-perfluoro decyl Trimethoxy silane (CF
3(CF
2)
7cH
2cH
2si (OCH
3)
3) or 1H, 1H, 2H, 2H-perfluoro decyl triethoxyl silane (CF
3(CF
2)
7cH
2cH
2si (OCH
2cH
3)
3).
3. the super lyophoby anti-reflective glass upper layer that preparation method prepares according to any one of claim 1 ~ 2.
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| CN103951277B true CN103951277B (en) | 2015-11-25 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016082153A1 (en) * | 2014-11-27 | 2016-06-02 | Honeywell International Inc. | Omniphobic coating |
| CN106390764B (en) * | 2015-07-28 | 2018-10-12 | 北京工业大学 | A kind of super-hydrophobic oleophobic method of modifying of perforated membrane |
| CN105317422A (en) * | 2015-11-18 | 2016-02-10 | 中石化石油工程技术服务有限公司 | Underground visual probing equipment and method |
| CN105622975B (en) * | 2016-01-27 | 2019-01-15 | 复旦大学 | A kind of preparation method of super-hydrophobic dielectric material and its dielectric material of preparation |
| CN110590184A (en) * | 2019-09-30 | 2019-12-20 | 福耀玻璃(苏州)有限公司 | Glass surface hydrophobic treatment process |
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| JP2008105887A (en) * | 2006-10-25 | 2008-05-08 | National Institute Of Advanced Industrial & Technology | Super water-repellent glass substrate and its manufacturing method |
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| CN102774085A (en) * | 2012-06-29 | 2012-11-14 | 法国圣戈班玻璃公司 | Hydrophobic base plate and manufacturing method thereof |
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Patent Citations (5)
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|---|---|---|---|---|
| JP2008105887A (en) * | 2006-10-25 | 2008-05-08 | National Institute Of Advanced Industrial & Technology | Super water-repellent glass substrate and its manufacturing method |
| CN101092289A (en) * | 2007-05-18 | 2007-12-26 | 华东理工大学 | A super hydrophobic material with roughened surface |
| CN102272066A (en) * | 2009-01-09 | 2011-12-07 | 法国圣戈班玻璃厂 | Hydrophobic substrate including a plasma-activated silicon oxycarbide primer |
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