CN107500557A - A kind of preparation method of the hydrophilic antifogging surface of imitative May-fly nymph compound eye structural - Google Patents

A kind of preparation method of the hydrophilic antifogging surface of imitative May-fly nymph compound eye structural Download PDF

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Publication number
CN107500557A
CN107500557A CN201710803521.4A CN201710803521A CN107500557A CN 107500557 A CN107500557 A CN 107500557A CN 201710803521 A CN201710803521 A CN 201710803521A CN 107500557 A CN107500557 A CN 107500557A
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China
Prior art keywords
glass
substrate
compound eye
plate
negative norm
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CN201710803521.4A
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Chinese (zh)
Inventor
韩志武
冯晓明
牛士超
张俊秋
穆正知
李博
王泽�
焦志彬
王大凯
张斌杰
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Jilin University
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Jilin University
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Publication of CN107500557A publication Critical patent/CN107500557A/en
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/0035—Multiple processes, e.g. applying a further resist layer on an already in a previously step, processed pattern or textured surface
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/29—Mixtures
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Composite Materials (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

The present invention relates to a kind of preparation method of the hydrophilic antifogging surface of imitative May-fly nymph compound eye structural, belong to antifogging surface and water wetted material preparation field.The preparation of the hydrophilic antifogging surface combines a kind of ultraviolet photolithographic and sol-gal process.First using the photoresists of SU 8 2005 as base material, the negative norm plate of similar bowl-shape array structure is prepared using ultraviolet photolithographic technique, and the negative norm plate may be reused, and production cost be reduced, then with SiO2For structural material, duplication obtains a kind of hydrophilic antifogging surface of imitative May-fly nymph compound eye structural.May-fly nymph compound eye is micro-meter scale hydrophilic antifogging function surface, different from the mosquito compound eye of micro-nano compound structure, therefore prepare relatively easy, and structure is survivable, micro-meter scale hydrophilic antifogging function is obtained by the way that its microstructure is characterized and copied, the antifogging surface that this method is prepared shows good transmitance, hydrophily and anti-fog performance.

Description

A kind of preparation method of the hydrophilic antifogging surface of imitative May-fly nymph compound eye structural
Technical field
The present invention relates to a kind of preparation method of the hydrophilic antifogging surface of imitative May-fly nymph compound eye structural, belong to antifogging surface With micro-nano manufacturing technology field.
Background technology
Hydrophily refers to there is very big affinity to water, can attract hydrone.If drop spreads, larger face is soaked Product, contact angle are less than 90 degree, then claim surface to be hydrophilic.Ultra-hydrophilic surface is generally referred to the contact angle of water close to 0 degree, it Drop can be allowed to sprawl to form water membrane rapidly, so as to reduce the scattering of light, surface is kept good transmitance, realize more Good anti-fog effect.
The biology of nature is in order to adapt to the environment of surrounding, by the evolution of 1 years so that some biologies have closely Perfect surface texture, present charming surface wettability.The mosquito that has now been found that, fly compound eye antifogging surface are all micro- Nano composite structure, excellent hydrophobic anti-fog performance is demonstrated by, but preparation difficulty is big, is unfavorable for large area processing and prepares.
The May-fly nymph compound eye lived in the fog environment of waterside, not only possesses simple micron scale construction, and have Excellent hydrophilic antifogging function.The hydrophilic antifogging surface of a kind of imitative May-fly nymph compound eye structural prepared by this paper, applied to super The fields such as hydrophilic, automatically cleaning, antireflection, mechanical lubrication, microfluid, and can produce in batches.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the hydrophilic antifogging surface of imitative May-fly nymph compound eye structural.For Prepared by the production of hydrophilic antifogging material at present mainly passes through following two approach：First, smear anti-fog coating, examination in material surface Anti-fog thin film is pasted in agent, reaches antifog effect using the hydrophily of this coating or film, but because composition is organic For thing so structural instability, composition are easily lost in, some volatile antifoggants even pollute environment, life-threatening health；Two It is using the method for heating, body surface is heated up, reduces the temperature difference between steam in object and air, so as to prevent the production of mist It is raw, but the method needs that tyre firing equipment, device volume be big, short, restricted application of holding time.The present invention proposes A kind of preparation method of the hydrophilic antifogging surface of imitative May-fly nymph compound eye structural, antifogging surface prepared by this method not only structure Simply and need not outer carrying device.
The preparation method of the present invention comprises the following steps：
This method combines a kind of ultraviolet photolithographic and sol-gel process, using the photoresists of SU-8 2005 as base material.
First, the cleaning of substrate of glass：First, in order to improve attachment of the photoresist to substrate of glass and obtain more smooth Film；By substrate of glass, 10min is washed in ultrasound shake in acetone, removes the organic matter of glass basic surface；Secondly substrate of glass is existed 10min is washed in ultrasound shake in absolute ethyl alcohol, is removed the remaining acetone of glass basic surface；Then by substrate of glass in deionized water 10min is washed in middle shake, is removed the inorganic matter of glass basic surface；Then substrate of glass will be placed on 200 DEG C of warm table and dried Roasting 10min, for increase photoresist with by glass basic surface adhesive force.
2nd, the preparation of precursor solution：The concentrated hydrochloric acid of 100ml water and 1ml is well mixed, then takes 7.2ml to prepare Hydrochloric acid solution and 22.4ml TEOS (tetraethyl orthosilicate) put into closed container, pass through magnetic stirrer at room temperature 30-40min is reacted, until the transparent no muddiness of solution, obtains precursor solution；
3rd, the preparation of negative norm plate：
1), the design of mask plate：According to the size of the single ommatidium of May-fly nymph compound eye and distribution, devise a kind of such as Fig. 2 Shown array of circular apertures mask plate, the diameter of its single circular hole is 15um, and the interval between circular hole is 16um, due to mayfly The height of the single ommatidium of naiad compound eye is 6um, is calculated by accurate with experiment repeatedly, the spin coating thickness for drawing photoresist is 7um。
2), the coating of photoresist：The photoresists of SU-8 2005 are coated on the glass substrate.The coating of the photoresists of SU-8 2005 Parameter：Desk-top spin coating machine speed is set to 2500-3500r/min, is put into after 30s in hot drying-plate, 2-3min is toasted at 95 DEG C, so Substrate of glass naturally cools to room temperature afterwards；
3), ultraviolet light photoetching：Utilize ultraviolet light photoetching：If Fig. 2 mask plate is under 105-110mJ/cm2 ultraviolet source Vertical exposure 5-8s, hot drying-plate being moved into again, 8-10min being toasted at 100 DEG C, the substrate of glass after cooling is ultrasonic in development 30s is washed in shake, then cleans 10s with isopropanol, is finally dried up glass basic surface with nitrogen gun, has so far been obtained photoresist composition Similar bowl-shape array structure negative norm plate, as shown in Figure 3.
4th, the formation of hydrophilic antifogging surface：One layer of clean sheet glass is covered on negative norm plate, by negative norm plate and sheet glass Both ends clamped with clip, then with pipette by precursor solution add in negative norm plate surface, due to negative norm plate and glass Capillary force between piece be present, precursor solution can be naturally infiltrated in the micro-structural of negative norm plate, be then put into negative norm plate Be heating and curing 1h in 120 DEG C of drying box, finally in order to ensure the integrality of micro-structural, is carefully taken clip using tweezers Under, so as to obtain a kind of hydrophilic antifogging surface using SiO2 as the imitative May-fly nymph compound eye structural of structural material.
The beneficial effects of the invention are as follows：
1st, the size of the antifogging surface is micro-meter scale, therefore prepares relatively easy, and structure is survivable, The negative norm plate that ultraviolet photolithographic is prepared simultaneously may be reused, and reduce production cost, be advantageous to industrialize large area Production and application.
2nd, the transmitance for the antifogging surface that this method is prepared, hydrophily and anti-fog performance, which are compared in the past, more preferable effect Fruit, the research for material surface wetability provide new approaches.
Brief description of the drawings
Fig. 1 is a kind of preparation process schematic diagram of the hydrophilic antifogging surface of imitative May-fly nymph compound eye structural of the present invention.
Fig. 2 is the structural representation of array of circular apertures mask plate of the present invention.
Fig. 3 is the structural representation of negative norm plate of the present invention.
Fig. 4 is the structural representation of the hydrophilic antifogging surface of the imitative May-fly nymph compound eye structural of the present invention.
Fig. 5 is atom grain microphotograph stereogram prepared by the present invention.
Fig. 6 is atom grain microphotograph top view prepared by the present invention.
Embodiment
As shown in Figure 1 and Figure 4, preparation method of the invention comprises the following steps：
This method combines a kind of ultraviolet photolithographic and sol-gel process, using the photoresists of SU-8 2005 as base material.
First, the cleaning of substrate of glass：First, in order to improve attachment of the photoresist to substrate of glass and obtain more smooth Film；By substrate of glass, 10min is washed in ultrasound shake in acetone, removes the organic matter of glass basic surface；Secondly substrate of glass is existed 10min is washed in ultrasound shake in absolute ethyl alcohol, is removed the remaining acetone of glass basic surface；Then by substrate of glass in deionized water 10min is washed in middle shake, is removed the inorganic matter of glass basic surface；Then substrate of glass will be placed on 200 DEG C of warm table and dried Roasting 10min, for increase photoresist with by glass basic surface adhesive force.
2nd, the preparation of precursor solution：The concentrated hydrochloric acid of 100ml water and 1ml is well mixed, then takes 7.2ml to prepare Hydrochloric acid solution and 22.4ml TEOS (tetraethyl orthosilicate) put into closed container, pass through magnetic stirrer at room temperature 30-40min is reacted, until the transparent no muddiness of solution, obtains precursor solution；
3rd, the preparation of negative norm plate：
1), the design of mask plate：According to the size of the single ommatidium of May-fly nymph compound eye and distribution, devise a kind of such as Fig. 2 Shown array of circular apertures mask plate, the diameter of its single circular hole is 15um, and the interval between circular hole is 16um, due to mayfly The height of the single ommatidium of naiad compound eye is 6um, is calculated by accurate with experiment repeatedly, the spin coating thickness for drawing photoresist is 7um。
2), the coating of photoresist：The photoresists of SU-8 2005 are coated on the glass substrate.The coating of the photoresists of SU-8 2005 Parameter：Desk-top spin coating machine speed is set to 2500-3500r/min, is put into after 30s in hot drying-plate, 2-3min is toasted at 95 DEG C, so Substrate of glass naturally cools to room temperature afterwards；
3), ultraviolet light photoetching：Utilize ultraviolet light photoetching：If Fig. 2 mask plate is under 105-110mJ/cm2 ultraviolet source Vertical exposure 5-8s, hot drying-plate being moved into again, 8-10min being toasted at 100 DEG C, the substrate of glass after cooling is ultrasonic in development 30s is washed in shake, then cleans 10s with isopropanol, is finally dried up glass basic surface with nitrogen gun, has so far been obtained photoresist composition Similar bowl-shape array structure negative norm plate, as shown in Figure 3.
4th, the formation of hydrophilic antifogging surface：One layer of clean sheet glass is covered on negative norm plate, by negative norm plate and sheet glass Both ends clamped with clip, then with pipette by precursor solution add in negative norm plate surface, due to negative norm plate and glass Capillary force between piece be present, precursor solution can be naturally infiltrated in the micro-structural of negative norm plate, be then put into negative norm plate Be heating and curing 1h in 120 DEG C of drying box, finally in order to ensure the integrality of micro-structural, is carefully taken clip using tweezers Under, so as to obtain a kind of hydrophilic antifogging surface using SiO2 as the imitative May-fly nymph compound eye structural of structural material, such as Fig. 5 and Fig. 6 The atom grain microphotograph stereogram and top view prepared for the present invention.

Claims (1)

  1. A kind of 1. preparation method of the hydrophilic antifogging surface of imitative May-fly nymph compound eye structural, it is characterised in that：Comprise the following steps：
    First, the cleaning of substrate of glass：First, in order to improve attachment of the photoresist to substrate of glass and obtain more smooth film； By substrate of glass, 10min is washed in ultrasound shake in acetone, removes the organic matter of glass basic surface；Secondly by substrate of glass anhydrous 10min is washed in ultrasound shake in ethanol, is removed the remaining acetone of glass basic surface；Then substrate of glass is shaken in deionized water 10min is washed, is removed the inorganic matter of glass basic surface；Then substrate of glass will be placed on 200 DEG C of warm table and toasted 10min, for increase photoresist with by glass basic surface adhesive force；
    2nd, the preparation of precursor solution：The concentrated hydrochloric acid of 100ml water and 1ml is well mixed, the salt for then taking 7.2ml to prepare Acid solution and 22.4ml TEOS (tetraethyl orthosilicate) are put into closed container, are reacted at room temperature by magnetic stirrer 30-40min, until the transparent no muddiness of solution, obtain precursor solution；
    3rd, the preparation of negative norm plate：
    1), the design of mask plate：According to the size of the single ommatidium of May-fly nymph compound eye and distribution, devise a kind of array of circular apertures and cover Template, the diameter of its single circular hole is 15um, and the interval between circular hole is 16um, due to the single ommatidium of May-fly nymph compound eye Height be 6um, by it is accurate calculate with experiment repeatedly, the spin coating thickness for drawing photoresist is 7um；
    2), the coating of photoresist：The photoresists of SU-8 2005 are coated on the glass substrate.The coating ginseng of the photoresists of SU-8 2005 Number：Desk-top spin coating machine speed is set to 2500-3500r/min, is put into after 30s in hot drying-plate, 2-3min is toasted at 95 DEG C, then Substrate of glass naturally cools to room temperature；
    3), ultraviolet photolithographic：Utilize ultraviolet photolithographic：Mask plate vertical exposure 5-8s under 105-110mJ/cm2 ultraviolet source, then It is secondary to move into hot drying-plate, 8-10min is toasted at 100 DEG C, 30s is washed in the ultrasound shake in development of the substrate of glass after cooling, is then used Isopropanol cleans 10s, finally dries up glass basic surface with nitrogen gun, has so far obtained the similar bowl-shape array of photoresist composition The negative norm plate of structure；
    4th, the formation of hydrophilic antifogging surface：One layer of clean sheet glass is covered on negative norm plate, by the two of negative norm plate and sheet glass End is clamped with clip, is then added precursor solution in negative norm plate surface with pipette, due to negative norm plate and sheet glass it Between capillary force be present, precursor solution can be naturally infiltrated in the micro-structural of negative norm plate, and negative norm plate then is put into 120 DEG C Drying box in be heating and curing 1h, finally in order to ensure the integrality of micro-structural, carefully clip is removed using tweezers, so as to Obtain a kind of hydrophilic antifogging surface using SiO2 as the imitative May-fly nymph compound eye structural of structural material.
CN201710803521.4A 2017-09-08 2017-09-08 A kind of preparation method of the hydrophilic antifogging surface of imitative May-fly nymph compound eye structural Pending CN107500557A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103840038A (en) * 2012-11-21 2014-06-04 中国科学院物理研究所 Three-dimensional sphere-like structure for enhancing light extraction efficiency of LED sample, and method for preparing same
CN105932074A (en) * 2016-04-27 2016-09-07 安徽工程大学 Solar cell packaging glass having self-cleaning function and preparation method thereof and solar cell having same

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103840038A (en) * 2012-11-21 2014-06-04 中国科学院物理研究所 Three-dimensional sphere-like structure for enhancing light extraction efficiency of LED sample, and method for preparing same
CN105932074A (en) * 2016-04-27 2016-09-07 安徽工程大学 Solar cell packaging glass having self-cleaning function and preparation method thereof and solar cell having same

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
曹焱焱: "蜉蝣目昆虫复眼防雾结构设计与机理研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 *

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Application publication date: 20171222