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CN104955783A - Transparent base having stain-proof film attached thereto - Google Patents

Transparent base having stain-proof film attached thereto Download PDF

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Publication number
CN104955783A
CN104955783A CN201480006778.1A CN201480006778A CN104955783A CN 104955783 A CN104955783 A CN 104955783A CN 201480006778 A CN201480006778 A CN 201480006778A CN 104955783 A CN104955783 A CN 104955783A
Authority
CN
China
Prior art keywords
transparent base
film
interarea
soil
soil film
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201480006778.1A
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Chinese (zh)
Other versions
CN104955783B (en
Inventor
藤井健辅
宫村贤郎
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AGC Inc
Original Assignee
Asahi Glass Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by Asahi Glass Co Ltd filed Critical Asahi Glass Co Ltd
Priority to CN201711338071.2A priority Critical patent/CN108129032B/en
Publication of CN104955783A publication Critical patent/CN104955783A/en
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Classifications

    • 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
    • C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
    • C03C17/30—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with silicon-containing compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • 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
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/42—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating of an organic material and at least one non-metal coating
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16—Antifouling paints; Underwater paints
    • C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
    • C09D5/1662—Synthetic film-forming substance
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16—Antifouling paints; Underwater paints
    • C09D5/1681—Antifouling coatings characterised by surface structure, e.g. for roughness effect giving superhydrophobic coatings or Lotus effect
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/538—Roughness
    • 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
    • C03C2217/70—Properties of coatings
    • C03C2217/77—Coatings having a rough surface

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  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Surface Treatment Of Glass (AREA)
  • Laminated Bodies (AREA)
  • Surface Treatment Of Optical Elements (AREA)
  • Liquid Crystal (AREA)
  • Optical Elements Other Than Lenses (AREA)

Abstract

The present invention provides a transparent base having a stain-proof film attached thereto, which comprises a transparent base and a fluorine-containing organosilicon compound coating film, wherein the transparent base has a first main surface and a second main surface that faces the first main surface, an anti-glare treatment is applied to the surface of the first main surface, and the fluorine-containing organosilicon compound coating film is arranged on the first main surface side of the transparent base and serves as a stain-proof film, and wherein the stain-proof film has a surface roughness (RMS) of 0.05 to 0.25 [mu]m inclusive and the average length (RSm) of a roughness curve element is 10 to 40 [mu]m inclusive.

Description

With the transparent base of anti-soil film
Technical field
The present invention relates to the transparent base of band anti-soil film.
Background technology
In recent years, especially in mancarried device, vehicle-mounted equipment, use the various display unit such as liquid-crystal displays more.In such display unit, as its lid component, adopt the formation being configured with transparent base all the time.In addition, also the known contact panel by band transparency electrode is integrated with protective glass and substrate that is that obtain is formed.
For such display unit, the chance on the touching such as the finger of people transparent base surface is many, when the finger etc. of people is touched, easily adheres to grease etc. on the surface at transparent base.And, when the attachment such as grease, visuality can be affected, the surface being therefore used in transparent base implement the transparent base of antifouling process.
As the transparent base implementing antifouling process from the teeth outwards, such as Patent Document 1 discloses a kind of water repellency glass, it is provided with water repellent layer on the glass baseplate surface with concaveconvex shape.
In addition, for the water repellency glass being provided with water repellent layer, because the adhesive power of water repllents and glass is weak, thus be difficult to keep water repellency, therefore in order to improve its weather resistance, studying the method (the such as patent documentation 2) surface shape of glass substrate being made predetermined shape always.
Prior art document
Patent documentation
Patent documentation 1: Japanese Unexamined Patent Publication 07-126041 publication
Patent documentation 2: Japanese Unexamined Patent Publication 11-171594 publication
Summary of the invention
Invent problem to be solved
But the water repellency glass of patent documentation 2 is the glass of exploitation for the purpose of the purposes such as windshield glass, window glass plate, the transparent base not being intended to be display unit etc. uses.
Therefore; when using this water repellency glass to use as the lid component of the display unit such as liquid-crystal display or the protective glass integrated with the transparency electrode of contact panel; owing to almost there is no anti-dazzle characteristic, therefore exist and map light around thus the problem of the visuality of display section reduction.
In addition, as mentioned above, the water repellency glass of patent documentation 2 is the water repellency glass being designed for the few part of the chance of the staff such as window glass touching, when therefore using as the lid component likely touched by staff as display unit or the substrate integrated with contact panel, weather resistance is not enough upper frequency.
In view of the problem that above-mentioned prior art has, the object of the invention is to, provide a kind of and there is the transparent base that anti-dazzle characteristic improves the band anti-soil film of the weather resistance of anti-soil film simultaneously.
For the means of dealing with problems
In order to solve the problem, the invention provides a kind of transparent base with anti-soil film, it has:
Transparent base, described transparent base has the first interarea and second interarea relative with described first interarea, and implements anti-dazzle processing on the surface of described first interarea; With
Fluorine-containing organic silicon compound overlay film, described fluorine-containing organic silicon compound overlay film is the anti-soil film of the described first interarea side being arranged on described transparent base;
The surfaceness RMS of described anti-soil film is more than 0.05 μm and less than 0.25 μm, and the mean length RSm of roughness curve key element is more than 10 μm and less than 40 μm.
Invention effect
In the present invention, can provide a kind of and there is the transparent base that anti-dazzle characteristic improves the band anti-soil film of the weather resistance of anti-soil film simultaneously.
Accompanying drawing explanation
Fig. 1 is the explanatory view of the formation of the transparent base of the band anti-soil film of the 1st embodiment of the present invention.
Fig. 2 is the explanatory view of the formation of the transparent base of the band anti-soil film of the 2nd embodiment of the present invention.
Embodiment
Be described with reference to accompanying drawing for implementing mode of the present invention below, but the present invention is not limited to following embodiment, can impose various distortion and displacement without departing from the present invention to following embodiment.
1st embodiment
In the present embodiment, the transparent base of band anti-soil film of the present invention is described.
The transparent base of the band anti-soil film of present embodiment has transparent base and fluorine-containing organic silicon compound overlay film, described transparent base has the first interarea and second interarea relative with above-mentioned first interarea, and implementing anti-dazzle processing on the surface of above-mentioned first interarea, described fluorine-containing organic silicon compound overlay film is the anti-soil film of the above-mentioned first interarea side being arranged on above-mentioned transparent base.And the feature of the transparent base of above-mentioned band anti-soil film is: the surfaceness RMS of above-mentioned anti-soil film is more than 0.05 μm and less than 0.25 μm, and the mean length RSm of roughness curve key element is more than 10 μm and less than 40 μm.
Use Fig. 1 that the transparent base of the band anti-soil film of present embodiment is described.Fig. 1 schematically shows the sectional view of the transparent base of the band anti-soil film of present embodiment, has the formation being configured with anti-soil film 12 in the first interarea side of transparent base 11.Below each component of the transparent base forming band anti-soil film is described.
First, the material as transparent base 11 is not particularly limited, and can utilize at least through the various transparent bases of visible ray.Can enumerate such as: the various material such as plastic base, glass substrate.Wherein, from viewpoints such as the transparency, intensity, transparent base is preferably glass substrate.In this case, the kind of glass is not particularly limited, and can utilize the various glass such as non-alkali glass, soda-lime glass, alumina silicate glass.Wherein, from the adhering viewpoint with the layer (film) of disposed thereon, preferably soda-lime glass is used.
When transparent base 11 is glass substrate, from the view point of the intensity of transparent base itself, preferably use the hardened glass substrate (such as " Dragontrail (registered trademark) " etc.) obtained through chemical intensification treatment by alumina silicate glass.
Chemical intensification treatment refers to that the basic ion (such as sodium ion) by little for the ionic radius of glass surface is replaced as the process of the large basic ion of ionic radius (such as potassium ion).Such as, the fused salt of the glass containing sodium ion containing potassium ion is processed, can carry out chemical enhanced thus.The composition of the compressive stress layer of the glass baseplate surface after such chemical intensification treatment is slightly different from the composition before chemical intensification treatment, but the composition in substrate deep layer portion is roughly the same with the composition before chemical intensification treatment.
As chemical enhanced condition, be not particularly limited, can select according to for chemical enhanced glass types, required chemical enhanced degree etc.
As the fused salt for carrying out chemical intensification treatment, carry out selecting according to for chemical enhanced glass substrate.Can enumerate such as: alkali metal sulfates and the alkali metal chlorizated salts etc. such as saltpetre, sodium sulfate, potassium sulfate, sodium-chlor and Repone K.These fused salts can be used alone and also multiple combination can be used.
The Heating temperature of fused salt is preferably more than 350 DEG C, is more preferably more than 380 DEG C.In addition, be preferably less than 500 DEG C, be more preferably less than 480 DEG C.
Being more than 350 DEG C by setting the Heating temperature of fused salt, can preventing from being difficult to because ion-exchange speed reduces carrying out chemical enhanced.In addition, by being set as less than 500 DEG C, the decomposition of fused salt, deterioration can be suppressed.
In addition, in order to give sufficient stress, the time that glass substrate is contacted with fused salt is preferably more than 1 hour, is more preferably more than 2 hours.In addition, when long ion-exchange, productivity declines, and owing to relaxing, value of compressive stress is reduced, and is therefore preferably less than 24 hours, is more preferably less than 20 hours.
Shape about transparent base is also not particularly limited, and can utilize the transparent base of different shape.
Transparent base 11 has the first interarea 11A and the second interarea 11B corresponding thereto as mentioned above.And, the first interarea 11A implements the anti-dazzle processing forming the concaveconvex shape expected.Now, preferably the surfaceness RMS of the first interarea 11A is more than 0.05 μm and less than 0.25 μm, and the mean length RSm of the roughness curve key element of the first interarea 11A is more than 10 μm and less than 40 μm.By being this scope, can make the surfaceness RMS of the anti-soil film described later and mean length RSm of roughness curve key element in the scope expected.
Herein, surfaceness RMS refers to the concavo-convex mean depth apart from reference plane (being the substrate surface before surface treatment) herein.It should be noted that, also referred to as r.m.s. roughness, sometimes also represent with Rq.In addition, the mean length RSm of roughness curve key element refers in the roughness curve contained by datum length obtained on reference plane, the length on the concavo-convex reference plane in appearance one cycle is averaged and the length obtained.The mean length RSm of surfaceness RMS (μm) and roughness curve key element can by measuring based on the method for the method of regulation in JIS B 0601 (2001).
This is the result that the present inventor etc. finds in order to the weather resistance improving anti-soil film in the transparent base of band anti-soil film carries out studying, namely, by making the surface property of the first interarea 11A, there is above-mentioned characteristic, except anti-dazzle characteristic, compared with the transparent base of band anti-soil film in the past, especially the weather resistance of anti-soil film improves.
Anti-soil film is formed in the first interarea side of transparent base, and due to the surface shape of anti-soil film manifolding transparent base, thus anti-soil film surface also has the surface roughness characteristics roughly the same with transparent base.
This means to be greater than 0.25 μm with the RMS used in the past or RSm is greater than 40 μm and implements compared with the transparent base of anti-dazzle processing, afore mentioned rules is met by making the first interarea 11A of transparent base, in the micro concavo-convex of the first interarea of transparent base, pitch smaller between recess, and the area of protuberance increases.And as mentioned above, the surface of anti-soil film also has same surface shape.
When surface and the anti-soil film of the transparent base of this band anti-soil films of contact such as pointing, protuberance area increase compared with the transparent base of band anti-soil film in the past of the anti-soil film contacted with finger etc.Therefore, the power that finger etc. is applied to transparent base surface (anti-soil film) part of band anti-soil film is disperseed, and infers and can reduce the pressure being applied to anti-soil film thus, can suppress the stripping of anti-soil film, wearing and tearing.
Infer that the mean length RSm interval that is less, i.e. recess of roughness curve key element is less, then larger with the contact area of finger, weather resistance improves.But, in order to make RSm very little, needing embodiment as utilized the etch processes etc. of photomask, from the view point of cost, as long as RSm is more than 10 μm, just can preferably make.Therefore, for the face forming anti-soil film, preferably use the transparent base meeting above-mentioned RSm scope.
In addition, when transparent base in above-mentioned numerical range of RMS, RSm, the spacing of recess in suitable scope, therefore, it is possible to also had the transparent base of anti-dazzle characteristic.
In addition, the surfaceness RMS of the first interarea 11A is preferably more than 0.08 μm and less than 0.20 μm, and the mean length RSm of roughness curve key element is preferably more than 15 μm and less than 35 μm.By meeting these parameters, the weather resistance of anti-soil film can be made to improve further.
The anti-dazzle working method making the transparent base with above-mentioned surface property is not particularly limited, and can utilize and implements surface treatment to the first interarea and form the concavo-convex method of expectation.
Specifically, can enumerate: the first interarea for transparent base implements the method for frosted process.Frosted processing example is as can by will to be immersed in as the transparent base of treated object in the mixing solutions of hydrogen fluoride and Neutral ammonium fluoride thus to carry out chemical surface treatment to carry out to dipping face.
In addition, except above-mentioned chemically treated method, also can utilize the method for such as so-called sandblasting, by ground silica, carborundum powder etc. with compressed air spraying to transparent base on the surface; Or the method for physical treatment, by be attached with ground silica, carborundum powder etc. brush water-wet after, utilize this brush to grind etc.
Particularly the reagent solutions such as hydrogen fluoride are utilized to carry out in the method for frosted process of chemical surface treatment in enforcement, be not easy to produce tiny crack on the surface at treated object, and be not easy to produce physical strength reduction, therefore can preferably use as the surface-treated method implementing transparent base.
Make in the above described manner concavo-convex after, in order to refacing shape, generally can carry out chemical milling to glass surface.By etch quantity, mist degree can be adjusted to the value of expectation thus, can remove at middle crackles produced such as sandblastings, can also dazzle be suppressed.
As etching, the method that will be immersed in as the transparent base of treated object with hydrogen fluoride in the solution being main component preferably can be used.As the composition beyond hydrogen fluoride, hydrochloric acid, nitric acid, citric acid etc. can be contained.By containing these materials, can suppress to enter the alkali composition of glass and hydrogen fluoride reaction and the phenomenon of evolution reaction locally occurs, can make to be etched in face and evenly carry out.
For the second interarea 11B of transparent base, its characteristic is not particularly limited, and also can carry out the mean length RSm processing to make it have the surfaceness RMS same with the first interarea and roughness curve key element.
In addition, also contact panel transparency electrode can be made on the second interarea 11B of transparent base.Like this, by the formation that the transparency electrode of formation contact panel is integrated with the transparent base of band anti-soil film, further slim lightweight can be realized.It should be noted that, in this case, for the second interarea 11B, preferably do not carry out the above-mentioned anti-dazzle processing same with the first interarea 11A.
And, be formed with anti-soil film 12 as shown in Figure 1 in the first interarea 11A side of transparent base 11.Anti-soil film 12 can be made up of fluorine-containing organic silicon compound.
At this, fluorine-containing organic silicon compound is described.As the fluorine-containing organic silicon compound used in present embodiment, as long as the fluorine-containing organic silicon compound of imparting didirtresistance, water repellency, oil repellent just can be not particularly limited to use.
As such fluorine-containing organic silicon compound, can enumerate such as: the fluorine-containing organic silicon compound with more than one groups in the group being selected from and being made up of multi-fluoro polyether base, polyfluoro alkylidene group and Polyfluoroalkyl.It should be noted that, multi-fluoro polyether base refers to the divalent group with the structure that polyfluoro alkylidene group and etheric oxygen atom replace bonding and obtain.
There is as this concrete example of the fluorine-containing organic silicon compound of more than one groups in the group being selected from and being made up of multi-fluoro polyether base, polyfluoro alkylidene group and Polyfluoroalkyl, the compound etc. represented by following general formula (I) ~ (V) can be enumerated.
In formula, Rf is that the straight chain Polyfluoroalkyl of carbonatoms 1 ~ 16 is (as alkyl, such as: methyl, ethyl, n-propyl, sec.-propyl, normal-butyl etc.), X be the low alkyl group of hydrogen atom or carbonatoms 1 ~ 5 (such as: methyl, ethyl, n-propyl, sec.-propyl, normal-butyl etc.), R1 is that hydrolyzable group is (such as amino, alkoxyl group etc.) or halogen atom is (such as: fluorine, chlorine, bromine, iodine etc.), m is the integer of 1 ~ 50, be preferably the integer of 1 ~ 30, n is the integer of 0 ~ 2, be preferably the integer of 1 ~ 2, p is the integer of 1 ~ 10, be preferably the integer of 1 ~ 8.
C qF 2q+1CH 2CH 2Si(NH 2) 3(II)
At this, q be more than 1 integer, be preferably 2 ~ 20 integer.
As the compound represented by general formula (II), can enumerate such as: trifluoro (1,1,2,2-tetrahydrochysene) n-propyl silazane (n-CF 3cH 2cH 2si (NH 2) 3), seven fluorine (1,1,2,2-tetrahydrochysene) n-pentyl silazane (n-C 3f 7cH 2cH 2si (NH 2) 3) etc.
C q’F 2q’+1CH 2CH 2Si(OCH 3) 3(III)
At this, q ' be more than 1 integer, be preferably 1 ~ 20 integer.
As the compound represented by general formula (III), can enumerate such as: 2-(perfluoro capryl) ethyl trimethoxy silane (n-C 8f 17cH 2cH 2si (OCH 3) 3) etc.
In formula (IV), R f2serve as reasons-(OC 3f 6) s-(OC 2f 4) t-(OCF 2) uthe divalent straight chain multi-fluoro polyether base that-(s, t, u are the integer of 0 ~ 200 independently of one another) represents, R 2, R 3be the monovalent hydrocarbon (such as: methyl, ethyl, n-propyl, sec.-propyl, normal-butyl etc.) of carbonatoms 1 ~ 8 independently of one another.X 2, X 3be hydrolyzable group (such as amino, alkoxyl group, acyloxy, alkene oxygen base, isocyanate group etc.) or halogen atom (such as: fluorine atom, chlorine atom, bromine atoms, atomic iodine etc.) independently, d, e are the integer of 1 ~ 2 independently, c, f are the integer of 1 ~ 5 (being preferably 1 ~ 2) independently, a and b is 2 or 3 independently.
The R that compound (IV) has f2in, s+t+u is preferably 20 ~ 300, is more preferably 25 ~ 100.In addition, as R 2, R 3, be more preferably methyl, ethyl, butyl.As by X 2, X 3the hydrolysable group represented, is more preferably the alkoxyl group of carbonatoms 1 ~ 6, is particularly preferably methoxyl group, oxyethyl group.In addition, a and b is preferably 3 separately.
F-(CF 2) v-(OC 3F 6) w-(OC 2F 4) y-(OCF 2) z(CH 2) hO(CH 2) i-Si(X 4) 3-k(R 4) k(V)
In formula (V), v is the integer of 1 ~ 3, and w, y, z are the integer of 0 ~ 200 independently of one another, h be 1 or 2, i be the integer of 2 ~ 20, X 4for hydrolysable group, R 4for the straight or branched alkyl of carbonatoms 1 ~ 22, k is the integer of 0 ~ 2.W+y+z is preferably 20 ~ 300, is more preferably 25 ~ 100.In addition, i is preferably 2 ~ 10.X 4be preferably the alkoxyl group of carbonatoms 1 ~ 6, be more preferably methoxyl group, oxyethyl group.As R 4, be preferably the alkyl of carbonatoms 1 ~ 10.
In addition, be selected from the fluorine-containing organic silicon compound of more than one groups in the group be made up of multi-fluoro polyether base, polyfluoro alkylidene group and Polyfluoroalkyl as commercially available having, preferably can use KP-801 (trade(brand)name, chemical company of SHIN-ETSU HANTOTAI system), KY178 (trade(brand)name, chemical company of SHIN-ETSU HANTOTAI system), KY-130 (trade(brand)name, chemical company of SHIN-ETSU HANTOTAI system), KY-185 (trade(brand)name, chemical company of SHIN-ETSU HANTOTAI system), OPTOOL (registered trademark) DSX and OPTOOL AES (being trade(brand)name, large King Company system) etc.
It should be noted that, react and deterioration etc. to suppress the moisture in fluorine-containing organic silicon compound and air, generally it is mixed with containing fluorous solvent equal solvent and preserve, but time when containing these solvents directly for film formation process, sometimes detrimentally affect is caused to the weather resistance etc. of obtained film.
Therefore, in the present embodiment, the fluorine-containing organic silicon compound of solvent removing process or the fluorine-containing organic silicon compound without solvent cut (not adding solvent) has been carried out before preferably use utilizes heating container to heat in advance.Such as solvent strength contained in fluorine-containing organic silicon compound solution, be preferably less than 1 % by mole, be more preferably less than 0.2 % by mole.Particularly preferably use not solvent-laden fluorine-containing organic silicon compound.
It should be noted that, as the solvent used when preserving above-mentioned fluorine-containing organic silicon compound, can enumerate such as: perflexane, hexafluoro m-xylene (C 6h 4(CF 3) 2), (trade(brand)name, Sumitomo 3M Inc., HFE7200 are by C for hydrogen perfluoroalkyl polyether, HFE7200/7100 4f 9c 2h 5expression, HFE7100 are by C 4f 9oCH 3represent) etc.
Carry out from containing containing carrying out vacuum exhaust as passed through to the container being placed with fluorine-containing organic silicon compound solution except the processing example of desolventizing (solvent) the fluorine-containing organic silicon compound solution of fluorous solvent.
About the time of carrying out vacuum exhaust, change according to the exhaust capacity of vent line, vacuum pump etc., the amount of solution etc., so there is no limit, such as, can be more than about 10 hours.
The film of the anti-soil film of present embodiment is not particularly limited, and preferably uses above-mentioned materials to carry out film forming by vacuum evaporation.
In addition, the removing process of above-mentioned solvent also by fluorine-containing organic silicon compound solution being imported the heating container of the film deposition system forming anti-soil film, then at room temperature can be carried out carrying out vacuum exhaust in heating container before intensification.In addition, also can vaporizer etc. be utilized in advance to remove desolventizing before importing heating container.
But as mentioned above, solvent few or not solvent-laden fluorine-containing organic silicon compound, compared with the situation containing solvent, easily due to deteriorated with atmosphere.
Therefore, the preservation container of the fluorine-containing organic silicon compound of solvent few (or not containing solvent) preferably use by container with inert gas replacements such as nitrogen and airtight after container, and shorten when operating and be exposed to air, time with atmosphere.
Specifically, preferably the heating container immediately fluorine-containing organic silicon compound being imported the film deposition system forming anti-soil film after container breaks a seal will be preserved.And, preferably make after importing become vacuum in heating container or replace with the rare gas element such as nitrogen, rare gas, remove air (air) contained in heating container thus.In order to can when with when atmosphere not being directed into the heating container of this manufacturing installation from preserving container (storage container), such as preferred storage container to be connected by being with the pipe arrangement of valve with heating container.
And, after fluorine-containing organic silicon compound is imported heating container, in container, preferably form vacuum or with after inert gas replacement, start the heating for film forming immediately.
As the film of anti-soil film, describing the example of the fluorine-containing organic silicon compound using solution or stoste in description of the present embodiment, but be not limited thereto.As other method, such as: evaporation particle is (as an example to use commercially available being called, キ ャ ノ Application オ プ ト ロ Application Inc. サ ー Off Network リ ア) method, this evaporation particle is by making a certain amount of fluorine-containing organic silicon compound be infiltrated up in porous metal (such as tin or copper) or fibrous metal (such as stainless steel) and obtain in advance.In this case, also the particle of the amount according to evaporation coating device capacity, required film thickness can be formed anti-soil film simply as vapor deposition source.
As mentioned above, because anti-soil film directly makes carbon copies the surface shape of transparent base, thus its surface property is identical with the surfaceness RMS of transparent base and the mean length RSm of roughness curve key element.Therefore, its surfaceness RMS is more than 0.05 μm and less than 0.25 μm, and the mean length RSm of roughness curve key element is more than 10 μm and less than 40 μm.In addition, particularly, surfaceness RMS is more preferably more than 0.08 μm and less than 0.20 μm, and the mean length RSm of roughness curve key element is more preferably more than 15 μm and less than 35 μm.
In addition, in order to improve the adhesivity of transparent base and anti-soil film, adhesion layer can be inserted between transparent base and anti-soil film.When inserting adhesion layer, be formed in advance on the first interarea of transparent substrate before formation anti-soil film.As adhesion layer, preferably use silicon oxide film.As thickness, for more than 2nm and below 50nm, be preferably more than 5nm and below 20nm.
Each component above for the transparent base of the band anti-soil film of present embodiment is illustrated, and the mist degree of the transparent base of the band anti-soil film of present embodiment is preferably more than 2% and less than 30%.This is because, if mist degree is more than 2%, compared with not implementing the substrate of anti-dazzle processing, the mapping of light (reflecting り こ body) can be suppressed significantly through visual confirmation; If be greater than 30%, then causing light diffuse-reflectance, when using as the lid component of display unit or the substrate integrated with contact panel, the visuality of the display of display unit can be reduced.In addition, the mist degree of the transparent base of the band anti-soil film of present embodiment is preferably more than 15% and less than 27%.
Show: by mist degree in above-mentioned scope, the transparent base of the band anti-soil film of present embodiment has sufficient anti-dazzle characteristic, can more preferably as lid component or the substrate integrated with the contact panel utilization of display unit etc.
According to the transparent base of the band anti-soil film of present embodiment discussed above, can obtain that there is the transparent base that anti-dazzle characteristic improves the band anti-soil film of the weather resistance of anti-soil film simultaneously.
[the 2nd embodiment]
In the present embodiment, the formation being also provided with low-reflection film in the 1st embodiment is described.Other is formed, due to as illustrated in the 1st embodiment, therefore omits herein.
Low-reflection film can suppress the reflection of the light on the transparent base surface at band anti-soil film, therefore, it is possible to make anti-dazzle characteristic improve further.Such as, when the lid component as display unit uses, the mapping of the light of surrounding can be suppressed, improve the visuality of the display of display unit further.
The material of low-reflection film is not particularly limited, as long as can the material of inhibitory reflex, just can utilize various material.Such as, as low-reflection film, can be formed high refractive index layer and the stacked and formation obtained of low-index layer.
High refractive index layer and low-index layer can for the forms comprising 1 layer separately, also can for the formation comprising more than 2 layers separately.When the high refractive index layer of each self-contained more than 2 layers and low-index layer, be preferably high refractive index layer and the alternately laminated form of low-index layer.
In order to obtain sufficient antireflection property, low-reflection film is preferably laminated with the duplexer of multiple film (layer).Such as, this duplexer preferably amounts to and is laminated with more than 2 layers and the film of less than 6 layers, is more preferably laminated with more than 2 layers and the film of less than 4 layers.Duplexer is herein preferably as mentioned above by high refractive index layer and the stacked and duplexer that obtains of low-index layer, and preferably the total of the number of plies of high refractive index layer and low-index layer in above-mentioned scope.
The material of high refractive index layer, low-index layer is not particularly limited, and can consider that required antireflection degree, productivity etc. are selected.As the material forming high refractive index layer, such as, preferably can utilize and be selected from niobium oxides (Nb 2o 5), titanium oxide (TiO 2), zirconium white (ZrO 2), silicon nitride (SiN) and tantalum oxide (Ta 2o 5) more than one.As the material forming low-index layer, can preferably utilize silicon oxide (SiO 2).
As high refractive index layer, consider from productivity, specific refractory power degree, particularly preferably utilize niobium oxides.Therefore, above-mentioned low-reflection film is more preferably the duplexer of niobium oxides layer and silicon oxide layer.
In the transparent base of the band anti-soil film of present embodiment, the position arranging low-reflection film is not particularly limited, on the first interarea 11A that can be arranged on transparent base and/or the second interarea 11B.Particularly preferably be arranged on the first interarea 11A of transparent base.Such as shown in Fig. 2, sequentially laminated with the formation of low-reflection film 13, fluorine-containing organic silicon compound overlay film 12 on the surface (from the first interarea side) being more preferably formed in the first interarea 11A of transparent base 11.
As described above by the formation the first interarea 11A being formed in transparent base being laminated with low-reflection film 13, fluorine-containing organic silicon compound overlay film (anti-soil film) 12, also can prevent low-reflection film 13 from peeling off and improving weather resistance, therefore preferably.
In addition, when inserting the adhesion layer of the weather resistance improving anti-soil film, preferably put it between low-reflection film and anti-soil film.In this case, silicon oxide film is also the material preferably used, and when the superiors being shown in low-reflection film as above-mentioned example institute are also silicon oxide, can realize the effect of low reflectivity and adhesion layer, be therefore preferred formation simultaneously.
In fig. 2, low-reflection film 13 is formed as being laminated with 2 layer 131, the formation of 132, but is not limited to this form, also can be formed as the formation being laminated with multiple layers further as mentioned above.
In addition, for the transparent base of the band anti-soil film of present embodiment, based on illustrated same reasons in the 1st embodiment, mist degree is also preferably more than 2% and less than 30%, is more preferably more than 15% and less than 27%.
Above, in the present embodiment, the transparent base for the band anti-soil film with low-reflection film is illustrated, and by having this formation, can improve anti-dazzle characteristic further.Therefore, can more preferably use in the purposes of the special requirement such as the lid arrangement of display unit or the substrate integrated with contact panel anti-dazzle characteristic.
Embodiment
Below enumerate specific embodiment to be described, but the present invention is not limited to these embodiments.It should be noted that, example 1 ~ example 4 is embodiment, and example 5 ~ example 7 is comparative example.
(1) evaluation method
Evaluating characteristics for the transparent base of the band anti-soil film obtained in following example 1 ~ example 7 is described as follows.
(surface shape measuring)
For the surface shape of the anti-soil film of the sample after the anti-soil film film forming used in example 1 ~ example 7, laser microscope (Ji Ensi (キ ー エ Application ス) Inc., trade(brand)name: VK-9700) is used to measure face profile with the multiplying power of 50 times.Then, obtain the value of the mean length RSm of surfaceness RMS and roughness curve key element based on JIS B0601 (2001) from the face profile obtained.
In each example, the anti-soil film of film forming, low-reflection film are the film very thin relative to the thickness of transparent base, and therefore the concaveconvex structure on surface in fact directly makes carbon copies the surface shape of transparent base.Therefore, for the surface shape of transparent substrate (being formed with the face of anti-soil film side), think it is also identical.
(mist degree mensuration)
In embodiment, comparative example, the sample after formation anti-soil film is carried out to the mensuration of transmittance haze.Mist degree is measured, uses haze meter (ス ガ trier Co., Ltd. system, model: HZ-V3) to carry out.
(friction weather resistance (wear resistance) test)
For the sample after anti-soil film film forming in example 1 ~ example 7, the anti-soil film for this sample carries out friction endurance test with following step.
First, the anti-soil film for example 1 ~ 7 carries out rub(bing)test with following step.
It is the friction head that the surface mounting Steel Wool #0000 of the planar metal pressure head of 10mm × 10mm makes friction sample in bottom surface.
Then, use above-mentioned friction head, connect formula (Daiei science Jing Qi Inc., model: PA-300A) with plane abrasion trier 3 and carry out rub(bing)test.Specifically, the mode first contacted with the antifouling face of sample with the bottom surface of above-mentioned pressure head is arranged on abrasion trier, and adding loads, to make the load of friction head be 1000g, reciprocatingly slides under the condition of one way 40mm at V-bar 6400mm/ minute.Be counted as Rubbing number 1 time by reciprocal 1 time, and test in the mode that Rubbing number is 1000 times.
Then, anti-soil film is carried out to the mensuration of water contact angle with following step.
The mensuration of the water contact angle of anti-soil film is by using automatic contact angle meter (consonance interface science Inc., model: DM-501), and anti-soil film drips pure water 1 μ L measure its contact angle and carry out.During mensuration, for each sample, 10 places on anti-soil film surface measure, and using its mean value as the water contact angle after the endurance test of this sample.
Now, water contact angle is more than 90 ° and is evaluated as qualified, and water contact angle is less than 90 ° and is evaluated as defective.
(2) experimental procedure
[example 1]
By the transparent base of following steps fabricated ribbon anti-soil film.
In this example, as transparent base, adopt the glass substrate (Asahi Glass Co., Ltd's system, trade(brand)name: " Dragontrail " (registered trademark)) using and implement chemical intensification treatment and the frosted process that the first interarea of this glass substrate is specified and the glass substrate (being designated as transparent base A below) that obtains.
Then, first interarea of transparent base A forms anti-soil film with following step.
First, fluorine-containing organic silicon compound (KCC of SHIN-ETSU HANTOTAI system, trade(brand)name: KY-185) is imported in heating container as deposition material.Then, by the solvent removed in solution utilizing degassed more than 10 hours of vacuum pump in heating container, thus fluorine-containing organic silicon compound overlay film formation composition is made.
Next, the heating container that above-mentioned fluorine-containing organic silicon compound film formation composition is housed is heated to 270 DEG C.After reaching 270 DEG C, its state is kept 10 minutes till temperature-stable.
Then, to first interarea (face through frosted process) of the transparent base A be arranged in vacuum chamber, from with the above-mentioned fluorine-containing organic silicon compound film formation nozzle that the heating container of composition is connected be housed supply fluorine-containing organic silicon compound film formation composition, and carry out film forming.
During film forming, while measuring thickness by the quartz oscillator monitor be arranged in vacuum chamber, carry out film forming, until the thickness being formed in the fluorine-containing organic silicon compound film on transparent base A reaches 10nm.
The moment reaching 10nm at fluorine-containing organic silicon compound film stops from nozzle base feed, and takes out the transparent base A being formed with fluorine-containing organic silicon compound film from vacuum chamber.
The transparent base A being formed with fluorine-containing organic silicon compound film taken out is arranged on hot plate in face mode upwards, and at 150 DEG C, carries out thermal treatment in 60 minutes in an atmosphere.
For sample obtained in the above described manner, carry out above-mentioned surface shape measuring, mist degree measures and rub endurance test.Show the result in table 1.
[example 2]
As transparent base, adopt the glass substrate (Asahi Glass Co., Ltd's system, trade(brand)name: " Dragontrail " (registered trademark)) the transparent base B the first interarea of this glass substrate having been carried out to frosted process that use and implement chemical intensification treatment, in addition, on first interarea of transparent base B, anti-soil film is formed in mode same as Example 1.For the transparent base of obtained band anti-soil film, evaluate in mode same as Example 1.Show the result in table 1.
[example 3]
As transparent base, adopt the glass substrate (Asahi Glass Co., Ltd's system, trade(brand)name: " Dragontrail " (registered trademark)) the transparent base C the first interarea of this glass substrate having been carried out to frosted process that use and implement chemical intensification treatment, in addition, on first interarea of transparent base C, anti-soil film is formed in mode same as Example 1.Transparent base for obtained band anti-soil film is evaluated in mode same as Example 1.Show the result in table 1.
[example 4]
Transparent base A forms low-reflection film in the following manner.
First, use niobium oxides target (AGC Ceramic Corporation system, trade(brand)name NBO target) at pressure 0.3Pa, frequency 20kHz, power density 3.8W/cm while being mixed with the mixed gas of the oxygen of 10 volume % in importing argon gas 2, reverse impulse width 5 microsecond condition under carry out pulsed sputter, thus form the high refractive index layer comprising niobium oxides (niobia) of thickness 13nm on first interarea of transparent base A.
Next, use silicon target at pressure 0.3Pa, frequency 20kHz, power density 3.8W/cm while being mixed with the mixed gas of the oxygen of 40 volume % in importing argon gas 2, reverse impulse width 5 microsecond condition under, under the condition of pulse width 5 microsecond, carry out pulsed sputter, thus on above-mentioned high refractive index layer, form the low-index layer comprising silicon oxide (silica) of thickness 30nm.
Next, use niobium oxides target (AGC Ceramic Corporation system, trade(brand)name NBO target) at pressure 0.3Pa, frequency 20kHz, power density 3.8W/cm while being mixed with the mixed gas of the oxygen of 10 volume % in importing argon gas 2, reverse impulse width 5 microsecond condition under carry out pulsed sputter, thus on above-mentioned low-index layer, form the high refractive index layer comprising niobium oxides (niobia) of thickness 110nm.
Next, use silicon target at pressure 0.3Pa, frequency 20kHz, power density 3.8W/cm while being mixed with the mixed gas of the oxygen of 40 volume % in importing argon gas 2, reverse impulse width 5 microsecond condition under, under the condition of pulse width 5 microsecond, carry out pulsed sputter and form the low-index layer comprising silicon oxide (silica) of thickness 90nm.
Define the low-reflection film that total is laminated with 4 layers of niobium oxides (niobia) and silicon oxide (silica) in the above described manner.
Next, on low-reflection film, anti-soil film is formed in mode same as Example 1.
For the transparent base of obtained band anti-soil film, evaluate in mode same as Example 1.Show the result in table 1.
[example 5]
As transparent base, adopt the glass substrate (Asahi Glass Co., Ltd's system, trade(brand)name: " Dragontrail " (registered trademark)) the transparent base D the first interarea of this glass substrate having been carried out to frosted process that use and implement chemical intensification treatment, in addition, on first interarea of transparent base D, anti-soil film is formed in mode same as Example 1.Transparent base for obtained band anti-soil film is evaluated in mode same as Example 1.Show the result in table 1.
[example 6]
As transparent base, adopt the glass substrate (Asahi Glass Co., Ltd's system, trade(brand)name: " Dragontrail " (registered trademark)) the transparent base E the first interarea of this glass substrate having been carried out to frosted process that use and implement chemical intensification treatment, in addition, on first interarea of transparent base E, anti-soil film is formed in mode same as Example 1.Transparent base for obtained band anti-soil film is evaluated in mode same as Example 1.Show the result in table 1.
[example 7]
As transparent base, use transparent base D same as Example 5, in addition, form low-reflection film and anti-soil film in mode same as Example 4, the transparent base for obtained band anti-soil film is evaluated in mode same as Example 1.Show the result in table 1.
[table 1]
According to the result shown in table 1, about the example 1 ~ 4 meeting the present invention and specify, in friction endurance test, water contact angle is more than 90 °, and on the other hand, about example 5 ~ 7, water contact angle is less than 80 °.
Anti-soil film has water repellency, and the situation that water contact angle described above diminishes represents that anti-soil film is peeled off, wearing and tearing.Therefore, about example 5 ~ 7, known anti-soil film is peeled off, wearing and tearing.
Can be confirmed by these results, about the example 1 ~ 4 meeting the present invention and specify, compared with the example 5 ~ 7 of comparative example, the weather resistance of anti-soil film becomes very high.
In addition, about example 1 ~ 4, also can confirm that it has suitable anti-dazzle characteristic according to its haze value.
Above, utilize the transparent base to band anti-soil film such as embodiment and embodiment to be illustrated, but the present invention is not limited to the above-described embodiment and examples etc.Various distortion, change can be carried out in the scope of the main idea of the present invention recorded in detail in the claims.
This application claims the right of priority of No. 2013-015968, the Japanese Patent Application of filing an application to the Japanese Patent Room based on January 30th, 2013, and the full content of No. 2013-015968, Japanese Patent Application is quoted in this international application.
Reference numeral
11 transparent bases
12 anti-soil films
13 low-reflection films

Claims (6)

1. the transparent base with anti-soil film, it has:
Transparent base, described transparent base has the first interarea and second interarea relative with described first interarea, and implements anti-dazzle processing on the surface of described first interarea; With
Fluorine-containing organic silicon compound overlay film, described fluorine-containing organic silicon compound overlay film is the anti-soil film of the described first interarea side being arranged on described transparent base;
The surfaceness RMS of described anti-soil film is more than 0.05 μm and less than 0.25 μm, and the mean length RSm of roughness curve key element is more than 10 μm and less than 40 μm.
2. the transparent base of band anti-soil film as claimed in claim 1, wherein, the mist degree of the transparent base of described band anti-soil film is more than 2% and less than 30%.
3. the transparent base of band anti-soil film as claimed in claim 1 or 2, wherein, described transparent base is glass substrate.
4. the transparent base of the band anti-soil film according to any one of claims 1 to 3, wherein, sequentially laminated with low-reflection film, fluorine-containing organic silicon compound overlay film on the surface of described first interarea of described transparent base.
5. the transparent base of band anti-soil film as claimed in claim 4, wherein, described low-reflection film is the duplexer of niobium oxides layer and silicon oxide layer.
6. the transparent base of the band anti-soil film as described in claim 4 or 5, wherein, described low-reflection film is the duplexer that stacked multiple film obtains, and amounts to and be laminated with more than 2 layers and the film of less than 6 layers in this duplexer.
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DE112014000613T5 (en) 2015-10-29

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