CN100465665C - Optical part and projection type display apparatus using same - Google Patents
Optical part and projection type display apparatus using same Download PDFInfo
- Publication number
- CN100465665C CN100465665C CNB2006101262187A CN200610126218A CN100465665C CN 100465665 C CN100465665 C CN 100465665C CN B2006101262187 A CNB2006101262187 A CN B2006101262187A CN 200610126218 A CN200610126218 A CN 200610126218A CN 100465665 C CN100465665 C CN 100465665C
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- antireflection film
- compound
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- optics
- lens
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 150000002894 organic compounds Chemical class 0.000 claims description 28
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
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- ILVXOBCQQYKLDS-UHFFFAOYSA-N pyridine N-oxide Chemical group [O-][N+]1=CC=CC=C1 ILVXOBCQQYKLDS-UHFFFAOYSA-N 0.000 claims description 12
- 125000003785 benzimidazolyl group Chemical group N1=C(NC2=C1C=CC=C2)* 0.000 claims description 8
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Images
Abstract
The object of the present invention is to provide an optical part having an anti-reflecting membrane (1) which is low in resistance and high in adhesion and is sharply improved in light transmittance by reducing reflectance of light, and a display apparatus using the same. According to the present invention, there are provided an optical part which transmits or partially reflects light, wherein a light receiving face or a light outgoing face has an anti-reflecting membrane (1) which comprises inorganic oxide particles and a binder, has a thickness of 60-190 nm, and has pores of 5-200 nm in size, and a display device using the same.
Description
Technical field
The present invention relates to form the lens of antireflection film, and projection type video display device.
Background technology
Because the lens of use such as camera and telescope with the interface of air on owing to the difference of refractive index produces reflection, thereby loss light, and big under the environment that externally light is strong by reflection mirroring of causing, so on sensitive surface and exiting surface, form antireflection film.
As the extra-high-pressure mercury vapour lamp that utilizes the big light quantity of irradiation etc. as light source, by image-displaying members such as liquid crystal display cells projected image is presented at projection type video display device on the screen, liquid crystal projection apparatus, rear projection type lcd projection tv begin to popularize in enterprise, general family.
Optical system to liquid crystal projection apparatus is carried out simple declaration, and the light that sends from the lamp of light source is by a plurality of lens, polarization, spectroscope, image-displaying member etc., and is synthetic by the look synthetic prisms, is presented on the screen as image by projecting lens.
In addition, in the rear projection type lcd projection tv, the image light that sends from projecting lens is projected on the front panel by the back reflector orientation, thus display image.
Like this, because light advances by various opticses, so in the sensitive surface and the big occasion of the reflection on the exiting surface of each parts, its beam split quantitative change is little, there are problems such as image deepening in the result.Therefore, on the sensitive surface of each parts and exiting surface, antireflection film is set.
But the antireflection film major part of using in the existing optics forms by evaporation coating, so need vacuum technology.And antireflection film exists multi-layered type and single-layer type, because in multi-layered type, the antireflection film manufacturing process that antireflection property is good increases, so if can, hope is single-layer type.
Therefore, the design criteria of the antireflection film of brief description single-layer type below.
As the parts that optical components such as lens use, enumerate glass (refractive index 1.5～1.54), acryl resin (refractive index 1.49), PET resin transparent components such as (refractive indexes 1.56).The refractive index of these parts is designated as n
1, the refractive index of air is designated as n
0The time, reflectivity R represents with following formula.
R＝{(n
1-n
0)/(n
1+n
0)}
2 (1)
In addition, because the refractive index n of air
0Be generally 1.0, so this formula becomes following expression formula.
R＝{(n
1-1)/(n
1+1)}
2 (2)
If the refractive index of substitution glass, acryl resin, PET resin in the formula, then the reflectivity of a side of each transparent component is, glass 3.9～4.0%, acryl resin 3.9%, PET resin 4.8%.In the occasion that on parts surface, designs the antireflection film of single layer structure in order to suppress this reflectivity, if the refractive index of air layer is designated as n with suitable thickness
0, the refractive index of surface substrate is designated as n
1, the refractive index of film is designated as n
2, then reflectivity R ' obtains from following formula:
R′＝{(n
2 2-n
0×n
1)/(n
2 2+n
0×n
1)}
2 (3)
Because the refractive index n of air
0Be generally 1.0, so
R′＝{(n
2 2-n
1)/(n
2 2+n
1)}
2 (4)
At n
2 2=n
1The time, promptly
The time, reflectivity is 0% in theory.
If use above-mentioned equation, the refractive index that then is used for the antireflection film of glass is suitable about 1.22.But in present material, even the lower fluororesin of refractive index also is about about 1.34, the magnesium fluoride of known special low-refraction is about about 1.38 in inorganic material, realizes that with individual layer sufficient antireflection is a difficulty very.
In recent years, proposed further to reduce with monofilm the method for refractive index, a kind of is the エ ア ロ ゲ Le film of record in the following patent documentation 1.エ ア ロ ゲ Le film is to have the inner film that has the particulate (hollow minute particle) in cavity and keep the cementing agent of this hollow minute particle.Because the cavity of this エ ア ロ ゲ Le film inside has identical with air basically refractive index (refractive index 1.0), so even the refractive index of the cementing agent of the material of this hollow minute particle and maintenance hollow minute particle is big, film also can have the refractive index approaching with air.Promptly, can reduce reflectivity by this film is formed on the substrate.
In addition, with エ ア ロ ゲ Le diverse ways in, one of method that further reduces refractive index with monofilm be in the following patent documentation 2 record low refractive index film.It is disclosed to be, on the surface of exposing organic ultrafine dust near a side of air, the surface is gone up produce concavo-convex, thereby superficial density is descended, the result forms the low film of refractive index.
In other method, has the low refractive index film of the pore with honeycomb of following patent documentation 3 records.Because a plurality of pores of cellular formation form in parallel to each other in the mode that connects silicon dioxide microparticle, can not reduce the intensity of silicon dioxide microparticle itself, can access maximum voidage.Thereby can form the good low refractive index film of physical strength.
[patent documentation 1] spy opens the 2003-201443 communique
[patent documentation 2] spy opens flat 7-92305 communique
[patent documentation 3] spy opens the 2004-83307 communique
Summary of the invention
In the multi anti reflection coating of present employing magnesium fluoride etc., be that the adaptation of lens of concave surface or convex surface is low with respect to the surface, the long-term situation about peeling off that exists of using.Be acrylic acid occasion particularly, have tendency significantly in material.
In the エ ア ロ ゲ Le film of above-mentioned patent documentation 1 record, because the void content height, so there is the problem of the physical strength step-down of film.The physical strength of film greatly depends on the physical strength of hollow minute particle.For refractive index is descended, need to increase the emptying aperture of hollow minute particle, therefore, in the thin エ ア ロ ゲ Le film of the shell of hollow minute particle, the physical strength raising has difficulties.And, make the shell thickening of hollow minute particle, increase the occasion of emptying aperture, big because particle size becomes, thus the easy scattering of visible light, because transmissivity descends, so be unpractical.And the singularity that adopts the manufacturing process of overcritical carbonic acid also is difficult point.Particularly for uneven concavo-convex optical components such as lens, also necessity of existence research masking technique of existing.
In addition, in the low refractive index film of the pore that the low refractive index film and the above-mentioned patent documentation 3 of above-mentioned patent documentation 2 records are put down in writing with honeycomb, think and reflect the possibility that uprises but exist by the physical strength height of film because dirt enters concavo-convex the making on film surface owing to crosslinked and polymerization makes.And in these structures, refractive index is about 1.3～1.4, and also there is distance in preferred value (less than 1.3).
The objective of the invention is to solve above-named problem.Optical component, image display device with antireflection film of taking into account high antireflection ability and physical strength promptly are provided.
There is following situation in occasion being arranged under the contour gentle super-humid conditions of hot spring and marine boarding facility, promptly breeds on the optical components such as the lens of mould in image display device, prism, and light transmission is reduced.Therefore the vital issue that illustrates is optics, the image display device with following antireflection film, and this antireflection film possesses mould-proof function.
The inventor studies various material of preparing methods, and the result has found following method, promptly in the film that is formed by inorganic oxide particle and bonding agent, in bonding agent or the space that keeps 5～200nm size between bonding agent and inorganic oxide particle.In the little value of refractive index ratio bonding agent that this film shows, though also learn in this film inside and have the space, but because employing is the inorganic oxide particle that does not have the space, so have excellent physical strength, to the adaptation height of transparent components such as acrylic acid, glass, the surface reflection of opticses such as lens with this film is few, the light transmission height, simultaneously because of adaptation, so the physical strength height to the film surface.
In addition,, compare, be confined to the antireflection film near surface, so, can realize this function to the light of wide wavelength region may simultaneously even thickness exists difference also can bring into play anti-reflective function with substrate surface because the space in the film is not evenly to exist in film.
As membrane material, adopt silicon oxide particle as inorganic oxide particle, the silicon compound (silicon dioxide gel) that utilization has a water-disintegrable residue as the film of bonding agent show with bonding agent be that the refractive index of monox is in a ratio of quite little value (specifically, refractive index is below 1.33) in, though learn that also inside has the space, physical strength is good.
In addition, film is also high to the adaptation of substrate.Particularly compare with the antireflection film that adopts before magnesium fluoride and the fluororesin etc., parts are that the occasion of resin such as acrylic acid obviously wants high.
In addition, because the surface resistance of this film is very little, so, also can bring into play the effect that dust such as dust are difficult to adhere to even under low humidity condition resemble the winter.
But there is following situation in the occasion being arranged under the contour gentle super-humid conditions of hot spring and marine boarding facility, promptly breeds on the optical components such as the lens of mould in image display device, prism, and light transmission is reduced.Therefore, in the present invention, one of purpose is to make the antireflection film that forms on the opticses such as lens, prism possess mould proof property.
Be used to realize that means of above-mentioned purpose are as described below.
(1) be in the optics of feature with transmitted ray or reflecting part light, on the exiting surface of the sensitive surface of light or light, has antireflection film, above-mentioned antireflection film is made of inorganic oxide particle and bonding agent, and the thickness of above-mentioned antireflection film is 60～190nm, and above-mentioned antireflection film has the space of 5～200nm size.
(2) optics of (1) record it is characterized in that above-mentioned inorganic oxide particle is a silicon oxide particle, and above-mentioned bonding agent is made of silicon compound.
(3) optics of (1), (2) record, the major axis footpath that it is characterized in that above-mentioned particulate is below 190nm, and short shaft diameter is littler than thickness.
The optics of (4) (1)～(3) record is characterized in that having the layer that is made of fluorochemicals on the above-mentioned antireflection film surface.
The optics of (5) (1)～(4) record is characterized in that above-mentioned fluorochemicals is following structure, and above-mentioned layer is by chemical bond and substrate combination.
[F{CF(CF
3)-CF
2O}
n-CF(CF
3)]-X-Si(OR)
3
{F(CF
2CF
2CF
2O)
n}-X-Si(OR)
3
{F(CF
2)
n}-Y-Si(OR)
3
X is the bonding position of perfluoro polyether chain and alkoxy silane residue, and Y is the bonding position of perfluoroalkyl chain and alkoxy silane residue, and R is an alkyl.
(6) 1)～(5) Ji Zai optics is characterized in that being added with the organic compound with polyalkylene glycol chain in above-mentioned antireflection film.
The optics of (7) (1)～(5) record is characterized in that being added with the organic compound with salt structure in above-mentioned antireflection film.
The optics of (8) (1)～(5) record is characterized in that being added with the organic compound with pyridiniujm structure or two pyridiniujm structures in above-mentioned antireflection film.
The optics of (9) (1)～(5) record it is characterized in that being added with the organic compound with pyridiniujm structure or two pyridiniujm structures in above-mentioned antireflection film, and the element ratio of this nitrogen in organic compounds is less than 6 weight %.
The optics of (10) (1)～(5) record is characterized in that being added with the organic compound with pyridine-N-oxides structure or two pyridine-N-oxides structures in above-mentioned antireflection film.
The optics of (11) (1)～(5) record is characterized in that being added with the organic compound with benzimidazole structure or thiazole structure in above-mentioned antireflection film.
The optics of (12) (1)～(5) record is characterized in that being added with the organic compound with halogen atom and carbamic acid ester structure in above-mentioned antireflection film.
The optics of (13) (1)～(12) record is characterized in that above-mentioned optics is lens, polarization, spectroscope, image-displaying member, look synthetic prisms, the bulb of lamp, back reflector, front panel.
(14) projection type video display device, make from outgoing after the beam reflection of light source, with the light intensity of display element modulation from the outgoing beam of this light source, amplify to show with projecting lens and it is characterized in that image light after the modulate light intensity: the antireflection film that in the bulb of a plurality of lens that are assembled into above-mentioned projection type video display device inside, polarization, spectroscope, image-displaying member, look synthetic prisms, lamp, back reflector, front panel, is formed with (1)～(12) record at least one sensitive surface of at least one parts.
Description of drawings
Fig. 1 is the example of optics of the present invention.
Fig. 2 is the sketch of the formation method of the antireflection film that adopts of the present invention.
Fig. 3 is the cross-section photograph of the antireflection film that adopts of the present invention.
Fig. 4 be in the antireflection film that adopts of the present invention key element have intensity.(a) the void area place element of the antireflection film that adopts of the present invention exists intensity.(b) outside the void area of the antireflection film that adopts of the present invention element have intensity.
Fig. 5 is the synoptic diagram of the optical system of liquid crystal projection apparatus type image display device of the present invention.
Fig. 6 is the synoptic diagram of rear projection image display device of the present invention.
Fig. 7 is the back reflector of rear projection image display device of the present invention and near synoptic diagram thereof.
Symbol description
1,44 antireflection films 2,41 incident lights, 3 emergent lights 4,39 mirror surfaces 5 are fixed to fixed part 6 substrates 7 coating 8 bubbles 9 of optical system, 10 spaces, 11 lamps, 12 reflecting bodys, 13 concavees lens 14 the 1st lens arra 15 the 2nd lens arra, 16 polarizations 17,18,19 image-displaying members, 20 convergent lenses 21,22,23 collector lenses 24 the 1st relay lens 25 the 2nd relay lens, 26～29 catoptrons 30,31 spectroscopes, 32 look synthetic prisms, 33 projecting lens 34,38 screens, 35 shells, 36 optical units, 37 back reflector, 40 glass plates, 42 image lights, 43 reflected light
Embodiment
Below, utilize accompanying drawing that embodiments of the present invention and embodiment are elaborated, but can utilize various change of the present invention, be not limited to embodiment and embodiment.
Several examples of the optics of present embodiment shown in Figure 1.
The antireflection film that is provided with on the optical component surfaces of present embodiment is formed by inorganic oxide particle and bonding agent.The function of bonding agent is the bonding agent as antireflection film.This film is to be coated on also to heat on the substrate by the coating that will mix inorganic oxide particle and bonding agent and solvent to make basically.At bonding agent is the occasion of Thermocurable materials such as silicon dioxide gel, epoxy monomer, melmac monomer, is used for polymerization promptly promote the to film catalyzer of heat curing and also adds minute quantity to coating.And the antireflection film in the present embodiment can be handled by individual layer and form, and forms but also can handle by multilayer.
Utilize the formation method of the antireflection film that is provided with on the optical component surfaces of Fig. 1 brief description present embodiment.
Fig. 3 is the cross-section photograph about an example of the antireflection film of present embodiment, is to form antireflection film on the acrylic acid substrate.
Inorganic oxide is the particulate of monox, adopts silicon dioxide gel as bonding agent.On the acrylic acid substrate, form low refractive index film, form carbon (carbon) more in the above.Here, carbon only is that do not break and form in the cross section for when make measuring the sample in cross section, can the effect of the antireflection film of present embodiment not exerted an influence.
Among Fig. 3, can confirm to exist several spaces 10 in the inside of low refractive index film.The shape in space is uncertain shape, is about 5～150nm but its size is a major axis.In addition, major axis refers to the axle that connects longest distance in each space here, and the length of major axis is meant its distance.
Here, for the space is confirmed, measure space and non-space part element have intensity.Its result shown in Figure 4.
From the result of Fig. 4 as can be known, compare with the part in non-space, gap carbon, oxygen, silicon etc. exist intensity little.Thereby can confirm the existence in space.
The monox (refractive index about 1.5) of the bonding agent by changing film and the ratio that space (refractive index about 1.0) accounts in film can be controlled refractive index.Particularly, the ratio in space is big more, and refractive index is more little.
In addition, in the filming in the heat curing, the gasification of solvent helps the formation in space, thus also can be according to the boiling point of solvent and the heat curing temperature after being coated on coating on the substrate control the formation in space.
In Fig. 3, found this tendency, promptly the space be formed on mostly film than top (near the surface part).Think that this bubble that is the coating inside on substrate begins to form because heat curing is promptly heated rises to the cause of near surface.This means that beginning refractive index from substrate-side has the slowly tendency of step-down, even and be one deck, refractive index also has gradient in this layer.Consequently, have more refractive index,, have refractive index near air in the face side of non-substrate-side near substrate in substrate-side.Thereby can further reduce each reflection on reflection, air and the antireflection film interface on the interface of substrate and antireflection film.
According to above-mentioned character, the occasion at the different film of the coating formation thickness that utilizes same composition when the heat curing condition is identical, has the low more tendency of the thin more refractive index of film.This is because form a lot of spaces easily near surface.
At near surface, and also form a lot of spaces in inside for not only, consider to adopt double-deckization method.Like this,, also be formed on inside, so the physical strength of film has improved all the more because the space not only is formed near surface.
From the cross-section photograph of Fig. 3 as can be known, the space is present in film inside, because the space on film surface is few, so erasibility might as well.If the lip-deep space of film is many, then the concavo-convex change on film surface is big, thereby is suspended to easily when wiping away using cloth to wipe with, if but concave-convex surface is little, and situation about then being suspended to reduces, so film is difficult to peel off or damage.
Below coating material is described, and to the system film be described in detail.
(1) coating material
Coating material is by bonding agent, inorganic oxide example, solvent composition.Below they are narrated.
(1-1) bonding agent
As class coating material, enumerate the high organic or inorganic macromolecule material of the transparency, material that can producing high-molecular.At transparent base is the occasion of resin, if select the organic coating film material, and the situation that then exists substrate to expand, be out of shape or dissolve owing to the solvent that adopts.In addition, when being inorganic material, has the tendency of high rigidity.Therefore inorganic material is comparatively suitable.When being inorganic material, low-index material is favourable when forming antireflection film.Suitable low-index material is the silicon based material.
As high-molecular organic material, enumerate the thermoplasticity macromolecular material.Specifically, enumerate acryl resin, polystyrene, styrene-propene acid interpolymer, vibrin, Polyvinylchloride, ethylene-vinyl acetate copolymer, pet resin, polyvinylidene chloride resin, polycarbonate resin etc.But, enumerate the macromolecular material of Thermocurable as the material of organic producing high-molecular.Specifically, enumerate the polyamide-based acid derivative etc. of aliphatic structure.
As inorganic macromolecule material, enumerate silicon compound (being commonly referred to as silicon dioxide gel) with water-disintegrable residue, have the titanium compound (being commonly referred to as TiO 2 sol) of water-disintegrable residue etc.They be alkoxy silane or alkoxytitanium to be aggregated to molecular weight be compound after several thousand, be solvable state in alcohols solvent.By they are heated, can form the bonding agent of monox or titanium dioxide.
But, enumerate and have amino and various substituent alkoxy silanes such as chloro base, sulfydryl etc. as the material of inorganic producing high-molecular.Concrete material is shown in the narration of the silicon compound with water-disintegrable residue described later.
As mentioned above, suitable bonding is the silicon based material.Specifically, it is comparatively suitable to have a silicon compound of water-disintegrable residue.Be described in greater detail below.
A kind of as the silicon compound with water-disintegrable residue enumerates silicon dioxide gel.It is the material that becomes monox owing to heating.Because the light transmission height of the monox that forms, so be suitable for the antireflection film that adopts in the image display device.And compare with resins such as acrylic acid and polycarbonate, silicon oxide particle is disperseed.Do not make silicon oxide particle in the inner occasion of disperseing of film, if i.e. cohesion, film muddiness then, the incident light scattering, the optical transmission rate descends, so be not preferred.The general modulator approach of silicon dioxide gel is as described below.Under solutions of weak acidity tetraalkoxysilane is heated, the alkoxy hydrolysis becomes hydroxyl, and itself and near alkoxy silane radical reaction form silicon-oxygen-silicon bound, and macromolecule quantizes simultaneously.In general mean molecular weight is several thousand.If mean molecular weight low excessively (molecular weight is the occasion of hundreds of), then after add when pining for forming silicon oxide film, can produce the problem of part volatilization.If mean molecular weight too high (molecular weight is the occasion more than several ten thousand) is not because dissolve in the solvent that adopts, so can produce the problem of separating out when coating.
The tetraalkoxysilane that adopts during as the making silicon dioxide gel is enumerated tetramethoxy-silicane, tetraethoxysilane, tetrapropoxysilane, tetraisopropoxysilan, tetraisobutoxy-silicane alkane, four butoxy silanes etc.In addition, also enumerate silicon compound, for example silicon tetrachloride etc. with chlorine rather than alkoxysilane group.
As the silicon compound except that silicon dioxide gel, except that tetraalkoxysilane, comprise compound with amino and chloro, sulfydryl etc. with water-disintegrable residue.Specifically, enumerate 3-aminopropyltriethoxywerene werene, 3-TSL 8330, N-(2-amino-ethyl)-3-TSL 8330,3-r-chloropropyl trimethoxyl silane, 3-chloropropylmethyldimethoxysilane, 3-sulfydryl propyl trimethoxy silicane, vinyltrimethoxy silane, vinyltriethoxysilane, 3-glycidoxypropyltrimewasxysilane, 3-glycidoxypropyl methyl dimethoxysilane, 3-isobutylene oxygen base propyl trimethoxy silicane etc.
(1-2) inorganic oxide particle
As inorganic oxide particle, enumerate colourless or white particles such as monox, aluminium oxide, titanium dioxide, cerium oxide.In order to improve the flatness of film, size is preferably the minor axis of particulate below average film thickness.In order to obtain the film of low-refraction easily, in above-mentioned substance, the monox that refractive index is lower (refractive index about 1.5～1.7), aluminium oxide (refractive index about 1.7～1.9) etc. are comparatively suitable.Therefore especially silicon oxide particle is described in detail.
At inorganic oxide particle is spherical occasion, and making the unscattered particle diameter of the light that incides on the film is preferred below 1/2 at wavelength.Because the wavelength of visible light zone is 380nm～780nm, so unscattered particle is preferred below 190nm in this scope.At silicon oxide particle is spherical occasion, and (wavelength is 380～760nm) not scatterings, and preferably mean grain size is below 190nm in order to make the visible light that incides on the film.About visibility region, Na Gujia believes work, and on February 10th, 1984 the 2nd edition, the industry color science towards storehouse bookstore, goes up on the books for the 2nd page.If more than the scope,,, have the occasion that produces inconvenience in the time of in being applied to display so film can be seen muddiness then because of the incident light scattering at this.And be the occasion of chain at silicon oxide particle since with above-mentioned identical reason, also preferred thickness (with respect to the thickness on the vertical cross section of bearing of trend) is below 190nm.The particle diameter of silicon oxide particle is more little, and the transparency is high more.Therefore preferably mean grain size become below the 100nm comparatively suitable.
Inorganic oxide particle can adopt the different or variform particulate of multiple particle diameter.In the occasion that adopts for example bar-shaped or chain particulate, in order not reduce the optical transmission rate, wish minor axis below 100nm, for the minimizing that makes transmissivity becomes below 1%, preferably make as far as possible below the minor axis 40nm.
If but the bonding agent that adopts promptly has the silicon compound of water-disintegrable residue and the dispersiveness in solvent is not enough,, still exist film can see muddy problem then owing to cohesion becomes big offspring.Therefore, preferably adopt the solvent that silicon oxide particle is disperseed well as far as possible, but also will consider to use the occasion of such solvent owing to the kind of substrate.Under such occasion, add spreading agent.Specifically, the nonionic spreading agent is suitable.The ionic spreading agent of a part exists promotion to have the occasion of the silicon compound polymerization of water-disintegrable residue, the viscosity of coating significantly uprises before being applied on the substrate, existing according to occasion becomes gel or full solidification becomes solid, the situation that can not be coated with also exists, so wish to confirm whether to have produced such phenomenon in use.In the occasion that adopts spreading agent,,, also should use on a small quantity in use in addition so wish under passable situation, not use spreading agent because have the tendency that film strength descends.
As silicon oxide particle, suitable is the santocedl that is dispersed in advance in the spreading agent.Particulate in the santocedl has a lot of hydroxyls from the teeth outwards, so the water wettability height.And be that hydrophilic while resistance is also extremely low as the antireflection film that member forms with them.Specifically, be about 1 * 10
10～10 * 10
10About Ω.This numerical value be 1/10000th hundred ten thousand of glass, acryl resin, polycarbonate resin, PET resin etc./, be very little.Therefore, dust such as dust is difficult to adhere to.Therefore be provided with on transparent surface in the greenhouse etc. of film of the present invention, the amount of incident of light increases, and the development time of plant shortens.For image processing system, because on the chamber internal surface of drying, also can not adhere to dust for a long time, so can enjoy distinct image.Be difficult to adhere to dust such as dust because be provided with on the transparency carrier of film of the present invention, so be effective as indoor building materials such as the wall of dirt pocket etc., partition walls.
Because there are a lot of hydroxyls from the teeth outwards, thus compare with commonly used glass plate etc., can be with very big ratio in conjunction with compound with alkoxysilane group.Therefore, compare with substrates such as glass commonly used, what can make that aftermentioned has the perfluoro polytrimethylene ether compound of alkoxysilane group or an all-fluoroalkyl compound hates liquor with very big ratio combination.Therefore and the glass plate of using always etc. compare, be suitable improving on the lyophobicity this point.And, also can have the perfluoro polytrimethylene ether compound of alkoxysilane group or the liquor of hating of all-fluoroalkyl compound is handled to aftermentioned, give lyophobicity.
In the santocedl, as the component parts of antireflection film, suitable silicon oxide particle is atypic particulate.Film have an identical occasion of ratio, compare with real sphere, reduce the refractive index of the film that forms easily.It is silicon dioxide gel that the bonding agent of film promptly keeps body, and monox is extremely low as the function of the maintenance body of film.If therefore do not have silicon dioxide gel, then be difficult to keep the shape of film, become single powder state.Therefore in order to improve the physical strength of film, the exist ratio of monox in film is suitable for a short time.Compare with the occasion that adopts spherical monox, it is not clear to adopt the monox of chain can form the reason of the low film of refractive index, but estimates can not adopt with spherical monox to compare easy interstitial form in film.
Except that monox, about the little and suitable aluminium oxide of refractive index, the alumina sol that also has a lot of hydroxyls from the teeth outwards is suitable on the film this point that forms low-resistivity.
(1-3) solvent
Effectively paint solvent is can dissolved adhesive or make the homodisperse material of bonding agent.
But, be the occasion of resin at substrate, there are the situation that makes substrate expand, be out of shape or dissolve in ketone, ethers or esters solvent, so should be noted that.Have silicon compound and silicon oxide particle at coating, and silicon compound has water-disintegrable residue, be suitable for as aforesaid bonding agent, when silicon oxide particle was suitable for as inorganic oxide particle, alcohols solvent was suitable.Specifically, enumerate ethanol, n-propanol, isopropyl alcohol, normal butyl alcohol, isobutyl alcohol, the tert-butyl alcohol, n-amyl alcohol, isoamylol, tert-pentyl alcohol etc.Alcohols solvent is difficult to make the substrate that is formed by polycarbonate, acrylic acid etc. to expand, be out of shape or dissolving, so be suitable.In addition, for alcohols solvent, the alcohol that carbon number is big has the tendency that boiling point uprises.Also has the low more tendency of the many more boiling points of branch.When system film described later, compare boiling point with heat curing temperature and form the low film of refractive index when low slightly easily.The cause that this volume that is the space that produces because being accompanied by the gasification of film internal solvent accounts in film increases.
(1-4) spreading agent
If inorganic oxide particle cohesion, then the incident light scatter of coming.Therefore exist transmissivity to descend, perhaps problem such as film muddiness.Particularly, obviously find this tendency in the occasion of inorganics particulate more than 60nm.Even this is because with the cohesion of seldom number, the major axis of this condensed matter also can be more than 100nm, thus optical transmission in the overslaugh visibility region.Therefore, can be by adding the cohesion that spreading agent suppresses particulate.
In fact, when on convex lens, forming antireflection film, when adopting the silicon oxide particle of particle diameter 60nm, if form antireflection film with the coating that does not add spreading agent, then the transmissivity of the light of wavelength 550nm is 97%, when the spreading agent with polyalkylene glycol chain that adds in coating was the 1 weight % of solid constituent of antireflection film, the optical transmission rate rose to 99%, and the effect of spreading agent obtains confirming.With end is that the spreading agent of sulfonic acid ammonium salt structure replaces when having the spreading agent of polyalkylene glycol chain, also can confirm same effect.
The addition of spreading agent is about about 0.1～5 weight % of solid constituent of antireflection film, waits according to the adding proportion of particulate and controls suitable addition.
Effectively spreading agent is nonionic, ionic interfacial agent.
(i) interfacial agent of nonionic
As the interfacial agent of nonionic, enumerate compound with polyalkylene glycol chain.The polyalkylene glycol chain possess hydrophilic property is adsorbed on the hydroxyl, oxygen atom etc. on inorganic oxide particle surface, perhaps is confined near them.On the other hand, wish that the part beyond the polyalkylene glycol chain is the structure that has compatibility in solvent, for example alkyl chain, alkene chain etc.
As the macrogol chain, specifically, preferred repetitive structure is that carbon number in the such unit of ethylene oxide unit, propylene oxide unit is in the unit below 3.Carbon number in the unit is in the occasion more than 4, and the tendency that possess hydrophilic property descends is so need to increase the addition of spreading agent.At this moment, the spreading agent filling that the space in the film is added, refractive index can not descend, but has the possibility that influences antireflection property.
(ii) ionic interfacial agent
As ionic interfacial agent, wish that the anionic site is azochlorosulfonate acid ion, carboxylic acid ion.The kation position is alkali metal ion preferably, specifically is sodion, potassium ion, lithium ion, and perhaps alkaline-earth metal ions specifically is magnesium ion, calcium ion, also has ammonium ion etc. in addition.
(1-5) mildewproof agent
As previously mentioned, under hot and humid condition, if produce mould on the optics that in image display device, adopts, then can produce light transmission and descend, the problem that image dimness, vividness are also not enough.Therefore by making the antireflection film that is provided with on the optical component surfaces have antimildew function, under hot and humid condition, also can provide distinct image with the suitable brightness that does not change usually.Need make the mildewproof agent of interpolation not absorb the i.e. light of the wavelength in visible zone of the required wavelength of formation image substantially, and in the coating that forms antireflection film, have intermiscibility.
In aforesaid (1-3), because have the occasion that is suitable for as the coating of the silicon oxide particle of inorganic oxide particle, what suppose employing is alcohols solvent, also is dissolved in alcohols solvent so wish mildewproof agent.And there is the possibility that dissolving is separated out from antireflection film in mildewproof agent soluble in water under high humidity environment.At this moment, if long term exposure under high humidity environment, then mildewproof agent flows out from optical component surfaces, the result worries to make mildew resistance to descend.Therefore, wish that mildewproof agent is the mildewproof agent not high with respect to the dissolubility of water.
Consider above viewpoint, think that the compound group with structure of enumerating below is suitable as mildewproof agent.
(i) has the organic compound group of pyridiniujm structure or two pyridiniujm structures
The chemical constitution of compound group with pyridiniujm structure is as follows.
In this structure, X is a halogen atom, specifically, is any in chlorine, bromine, the iodine.The nitrogen of pyridine ring is level Four salt structure, because this part is hydrophilic, so intramolecular hydrophobic parts is that the part of alkyl chain is big more, water-soluble, hydroscopicity just is suppressed specifically.N is the carbon number of alkyl chain, and it is big more, is insoluble in water more.If consider under high humidity environment and use, wish that carbon number is big, in other words, wish that the ratio of nitrogen element in the molecule is little.Specifically, the ratio of wishing nitrogen element in the compound is lower than 6 weight %.For example wish it is to be the occasion of chlorine at X, n is more than 9, and X is the occasion of bromine, and n is more than 6, and X is the occasion of iodine, and n is the compound more than 2.
There is the absorption of visibility region hardly in these compound groups, also are colourless so comprise their antireflection film when observing with eyes.The part of performance mildew resistance is the level Four salt structure division of the nitrogen of pyridine ring, so in the occasion of adding with identical weight ratio, have the high tendency of the little then mildew resistance of n.
The chemical constitution of the compound group with two pyridiniujm structures is shown below.
In this structure, X also is a halogen atom, specifically, is any in chlorine, bromine, the iodine.The nitrogen of two pyridine rings also is level Four salt structure, because this part is hydrophilic, so intramolecular hydrophobic parts is that the part of alkyl chain is big more, water-soluble, hydroscopicity just is suppressed specifically.Identical with the occasion of compound group with pyridiniujm structure, wish that the ratio of nitrogen element in the molecule is little.Specifically, the ratio of wishing nitrogen element in the compound is lower than 6 weight %.For example wish it is to be the occasion of chlorine at X, n is more than 10, and X is the occasion of bromine, and n is more than 9, and X is the occasion of iodine, and n is the compound more than 7.
There is the absorption of visibility region hardly in these compound groups, also are colourless so comprise their antireflection film when observing with eyes.The part of performance mildew resistance is the level Four salt structure division of the nitrogen of two pyridine rings, so in the occasion of adding with identical weight ratio, have the high tendency of the little then mildew resistance of n.And, compare with compound group with two pyridiniujm structures, have the high tendency of mildew resistance, so even addition seldom also can be brought into play high mildew resistance.
The organic compound group that (ii) has pyridine-N-oxides structure or two pyridine-N-oxides structures
The structure of pyridine-N-oxygen is shown below.
Organic compound group with pyridine-N-oxides structure is to have this structure in molecule.
Said structure does not almost have the absorption of visibility region, is colourless so comprise their antireflection film when observing with eyes yet.The part of performance mildew resistance is the pyridine-N-oxides structure.
The structure of two pyridines-N-oxygen is shown below.
Organic compound group with two pyridine-N-oxides structures is to have this structure in molecule.
Said structure does not almost have the absorption of visibility region, is colourless so comprise their antireflection film when observing with eyes yet.The part of performance mildew resistance is two pyridine-N-oxides structures.
The organic compound group that (iii) has benzimidazole structure or thiazole structure, isothiazole structure
Benzimidazole structure is shown below.
Organic compound group with benzimidazole structure is to have this structure in molecule.
Said structure does not almost have the absorption of visibility region, is colourless so comprise their antireflection film when observing with eyes yet.The part of performance mildew resistance is a benzimidazole structure.
The thiazole structure is shown below.
Organic compound group with thiazole structure is to have this structure in molecule.
Said structure does not almost have the absorption of visibility region, is colourless so comprise their antireflection film when observing with eyes yet.The part of performance mildew resistance is the thiazole structure.
The isothiazole structure is shown below.
Organic compound group with isothiazole structure is to have this structure in molecule.
Said structure does not almost have the absorption of visibility region, is colourless so comprise their antireflection film when observing with eyes yet.The part of performance mildew resistance is the isothiazole structure.
The organic compound group that (iv) has halogen atom and carbamic acid ester structure
The chemical constitution of this compound group is shown below.
The carbamic acid ester structure is-part of NHCOO-.In addition, R
1, R
2Be alkyl chain, perhaps have the alkyl chain of halogen atom.
Said structure does not almost have the absorption of visibility region, is colourless so comprise their antireflection film when observing with eyes yet.The part of inferring the performance mildew resistance is the synergy of carbamic acid ester structure and chlorine or bromine or iodine atom.
And, in these materials, even the organic compound group that has the organic compound group of benzimidazole structure and have a carbamic acid ester structure has big with respect to the interpolation quantitative change of antireflection film, the also little tendency of the variation of antireflection property (specifically, the tendency that the refractive index of film is almost constant), in this, these compound groups are suitable for optics of the present invention, image display device.
(2) film-forming method
Form the low refractive index film of present embodiment by pre-service, coating, heating.Can adopt the individual layer method to form, also can adopt the multilayer method to form.And, also there is the situation of carrying out the aftertreatment after heating in order to improve erasibility.Be described in greater detail.
(2-1) pre-service
In pre-service, evenly adhere to washing substrate, the wettability of raising substrate in order to make coating.
1) washing of substrate
In washing during substrate, the solvent, washing agent of the dirt on the attaching substrates etc. can be dissolved or remove well to employing well.But at substrate is the occasion of resin, and for example the occasion of acrylic acid and polycarbonate is compared thereby produce muddy such solvent (tetrahydrofuran, diox etc.) with the dissolving surface, and hope is alcohols solvents such as methyl alcohol, ethanol, propyl alcohol, butanols.When substrate is glass, make surperficial attenuation by being immersed in the alkaline solution (for example sodium hydrate aqueous solution etc.), carry out etching, also can remove dirt together.
2) wettability of raising substrate
Because by improving the wettability of substrate, coating evenly is coated with, so departing from of thickness is very little, optical characteristics is good.And, because the adaptation between substrate and the film has improved, so film strength strengthens.In order to improve the wettability of substrate, enumerate the surfaction method of equipment execution such as using plasma irradiation unit and utilize acid, aqueous slkali etc. the surface to be carried out the method for chemical modifying.
The surfaction method of employing equipment
As the method for this category, enumerate oxygen plasma irradiation, be placed in the ozone gas, UV irradiation etc.Any all is that active oxygen acts on the substrate surface, generates hydroxyl and carboxyl etc.Because these bases are hydrophilic, so on the surface that has generated these bases, wettability has improved.Therefore, obtain the uniform film of thickness by coating easily.In addition, UV irradiation is to utilize UV that airborne oxygen is become activated state, because it is a modified surface, so can access with the oxygen gas plasma irradiation, be placed on similar effects in the ozone gas.In addition method also has argon plasma.The irradiation argon plasma also can improve wettability.But in the identical occasion of output of the high frequency electric source of plasma producing apparatus, compare, need make irradiation time long with oxygen plasma.
Chemical modification method
If in sodium hydrate aqueous solution, then Biao Mian silicon-oxygen bond rupture generates hydroxyl with glass-impregnated, so wettability improves.Acrylic panel is the same with glass, if be immersed in the alkali, then wettability improves, but its principle is, the hydrolysis of ester group on surface exposes hydroxyl or carboxyl, thereby water wettability improves.
(2-2) coating process
Coating is spin coating, dip-coating, the rod coating that is coated with, adopts applicator roll, spraying, flow coat etc., is not particularly limited.In order to be controlled at suitable thickness, need make the constrained optimization of coating concentration, various coating processes.When spin coating, rotational speed and rotational time can exert an influence to thickness.Particularly the influence of rotational speed is big, has the thin more tendency of the high more then film of rotational speed.When dip-coating, dip time and last pulling rate degree can exert an influence to thickness.The influence of particularly going up the pulling rate degree is big, has the thin more tendency of the more little then film of last pulling rate degree.The suitable number that returns when rod is coated with, the size in gap when adopting the applicator roll coating, the speed of spraying during spraying, the use amount etc. that keeps the coating of the angle of substrate and employing during flow coat are coating conditions separately.
Preferred 60～the 190nm of target film thickness during coating.In the incident light wavelength is λ, when the refractive index of the medium of light incident (transparency carrier and antireflection film of the present invention) is n, and reflectivity minimum during thickness t=λ/4n in theory.
When incident light in the visible region (380～760nm), the refractive index of medium is with the glass substrate (refractive index about 1.7) from air (refractive index about 1.0) to high index during as the usable range of parts, and the minimum thickness of expectation is 380/ (4 * 1.7)=56nm.Less than 56nm the time, the occasion in the light incident of visible region can not cause enough influences to reflectivity.If also consider to make the film thickness distribution when filming, wish that then minimum thickness is the 60nm bigger slightly than 56nm.On the other hand, because maximum film thickness is 760/ (4 * 1.0)=190nm, so preferred 190nm.According to above condition, think that thickness of the present invention is that 60～190nm is suitable.And, people's visibility varies with each individual, but according to Na Gujia letter work, on February 10th, 1984 the 2nd edition, the industry color science, towards storehouse bookstore, 4～8 pages of photopic visions that go up record are than visibility curve, and the maximal value wavelength of relative spectral light sensitivity is that the highest wavelength (λ) of the visibility of the mankind under the bright light environments is near 555nm.Can make reflectivity is the refractive index decision of the refractive index of 0% antireflection film by the substrate that adopts in theory, and the square root of the refractive index of substrate is the refractive index of antireflection film.Substrate about the employing of image display devices such as monitor, enumerate glass, acryl resin, PET resin etc., preferably the glass for refractive index 1.50～1.54 is refractive index 1.22～1.24, acryl resin for refractive index 1.49 is a refractive index 1.22, is the antireflection film of refractive index 1.25 for the PET resin of refractive index 1.56.According to above content, at the wavelength of 555nm, the reflected light that can make the substrate of refractive index 1.5 is that the thickness of 0% antireflection film is 116nm in theory.Because there is not the reflectivity of the substrate side surfaces of antireflection film to be about 4%, thus can make reflectivity at least the thickness of the antireflection film below 4% at 90nm in the scope of 140nm.
(2-3) heating
After the painting process,, perhaps utilize bonding agent to make it overlapping, carry out heating operation in order to make solvent evaporates.By making heating-up temperature more than the boiling point of solvent, in film, produce bubble, finally as voids left in film, the result is the refractive index that has reduced film.
But, need make heating-up temperature below the heat resisting temperature at base material more than the boiling point of solvent.And the occasion adopting the Thermocurable material as bonding agent need make heating-up temperature more than heat curing temperature.Therefore selective solvent, base material and adhesive material under the situation of these requirements need satisfied.If there is difference in the volumetric shrinkage of film and substrate in the cooling after heating, then might cause problems such as film is peeled off, base plate deformation, so the material of preferred substrate of selecting and film is similar, perhaps linear expansivity is close.Consider from this viewpoint, adopt silicon dioxide gel as suitable bonding, adopt the occasion of silicon oxide particle as suitable inorganic oxide particle, because adding the film of thermosetting is monox, so we can say that glass or quartz that linear expansivity is close are suitable as baseplate material.
(2-4) aftertreatment summary
Form antireflection film of the present invention by heat curing, form the layer that forms by fluorochemicals in the above, improve the soil resistance on surface with lyophobicity.But need to make film as thin as a wafer, make the thickness of the layer that forms by fluorochemicals can not make the anti-reflection effect reduction of the antireflection film that forms with lyophobicity.Specifically, by as (2-2) described in less than 56nm, can avoid influence to reflectivity.And at the wavelength of the high 555nm of people's visibility, according to our research, to reflectivity do not affect 1% hate the liquid layer thickness less than 6nm.
Enumerate below 2 kinds by the fluorochemicals with lyophobicity constitute the layer generation type.
By filming that the fluorochemicals with lyophobicity constitutes
The method of filming that formation is made of the fluorochemicals with lyophobicity.By bringing into play lyophobicity with the covering surfaces of filming.Therefore, be low-resistance occasion at antireflection film, because cover the fluorochemicals of lyophobicity, so surface resistance improves, the result is that dust such as dust adheres to easily.
As the material that forms this film, enumerate サ イ ト Star プ (Asahi Glass society system), INT304VC (INT sreen society system) etc.With these materials with solvent dilution after, by the coating, the heating make solvent evaporates, make its heat curing according to occasion, the system film.
In conjunction with perfluoro polyether compound or all-fluoroalkyl compound
Make and have endways and can be attached to method on the antireflection film with the perfluoro polytrimethylene ether compound of the alkoxysilane group of combinations such as hydroxyl or all-fluoroalkyl compound.Specifically, make compound and the antireflection film combination that illustrates below.
[F{CF(CF
3)-CF
2O}
n-CF(CF
3)]-X-Si(OR)
3
{F(CF
2CF
2CF
2O)
n}-X-Si(OR)
3
{F(CF
2)
n}-Y-Si(OR)
3
X is the bonding position of perfluoro polyether chain and alkoxy silane residue, and Y is the bonding position of perfluoroalkyl chain and alkoxy silane residue, and R is an alkyl.
At this moment, do not cover the antireflection film surface fully, on antireflection film, become napier grass and equally produce perfluoro polyether chain or the such situation of perfluoroalkyl chain.Because the surface of antireflection film is not covered fully, so be 10 at film
11Low-resistance occasion that Ω is following is implemented this method caudacoria and also can be kept low resistive.
And by forming perfluoro polyether chain or perfluoroalkyl chain from the teeth outwards, the lubricity on surface has also improved.Therefore can relax the surface physics damage that friction causes, form the high surface of erasibility.
According to foregoing, except that soil resistance, realizing that the surface is low-resistancely kept, on the raising this point of erasibility, forming to adopt when hating liquid layer and have the perfluoro polyether compound of alkoxysilane group endways or the method for all-fluoroalkyl compound is favourable.
That (2-5) adopts in the aftertreatment hates liquor
Described in (2-4), as hating liquor, perfluoro polyether compound or all-fluoroalkyl compound that end has alkoxysilane group are effective.Illustrate below and hate liquor and hate liquid film formation method.
Hate liquor
As the perfluoro polyether compound or the all-fluoroalkyl compound that have alkoxysilane group endways, specifically enumerate following compound 1～12.
F{CF(CF
3)-CF
2O}
n-CF(CF
3)-CONH-(CH
2)
3-Si(OCH
2CH
3)
3
F{CF(CF
3)-CF
2O}
n-CF(CF
3)-CONH-(CH
2)
3-Si(OCH
3)
3
F{CF
2CF
2CF
2O}n-CF
2CF
2-CONH-(CH
2)
3-Si(OCH
2CH
3)
3
F{CF
2CF
2CF
2O}
n-CF
2CF
2-CONH-(CH
2)
3-Si(OCH
3)
3
Compound 4
H(CF
2)
6-CONH-(CH
2)
3-Si(OCH
2CH
3)
3
H(CF
2)
6-CONH-(CH
2)
3-Si(OCH
3)
3
H(CF
2)
8-CONH-(CH
2)
3-Si(OCH
2CH
3)
3
H(CF
2)
8-CONH-(CH
2)
3-Si(OCH
3)
3
F(CF
2)
6-(CH
2)
2-Si(OCH
3)
3
Compound 9
F(CF
2)
8-(CH
2)
2-Si(OOH
3)
3
F(CF
2)
6-(CH
2)
2-Si(OCH
2CH
3)
3
F(CF
2)
8-(CH
2)
2-Si(OCH
2CH
3)
3
Wherein compound 1～8 obtains by the synthetic method that illustrates below carrying out.The compound title of compound 9～12 is respectively 1H, 1H, 2H, 2H-perfluoro octyl group trimethoxy silane, 1H, 1H, 2H, 2H-perfluoro octyltri-ethoxysilane, 1H, 1H, 2H, 2H-perfluoro decyl trimethoxy silane, 1H, 1H, 2H, 2H-perfluoro decyl triethoxysilane, by
The list marketing of De ラ ス chemistry society.In addition, as other material of selling on the market, enumerate the system オ プ of Daikin Industries society Star-Le DSX.The fluorine chain of compound 1～4 is perfluoro polyethers, and beyond dewatering, even long-term (1000 hours) such as the cigarettes of hating liquid film and oil and tobacco that formed by the compound with this fluorine chain contact, water resisting property does not reduce (slippage is below 5 °) substantially yet.The general formula of representing these compounds is as follows.
[F{CF(CF
3)-CF
2O}
n-CF(CF
3)]-X-Si(OR)
3
{F(CF
2CF
2CF
2O)
n}-X-Si(OR)
3
X is the bonding position of perfluoro polyether chain and alkoxy silane residue, and R is an alkyl.
By adopting above-claimed cpd, even worrying also can to form the antireflection film of high soil resistance under the environment that machine oil and gasoline etc. pollute.
If the cigarette of compound 5～12 and oil and tobacco long-term (1000 hours) contacts, then the contact angle with water is reduced to and the essentially identical level of the contact angle of base material from flooding preceding (about 110 °).
(synthesizing of compound 1)
The Network ラ イ ト Star Network ス 157FS-L (mean molecular weight 2500) (25 weight portion) that dissolving DUPONT company makes in the system PF-5080 of 3M society (100 weight portion) adds thionyl chloride (20 weight portion) therein, refluxes 48 hours while stir.Make thionyl chloride and PF-5080 volatilization with evaporator, obtain the chloride thing (25 weight portion) of Network ラ イ ト Star Network ス 157FS-L.Add PF-5080 (100 weight portion), Chisso (strain) system サ イ ラ エ-ス S330 (3 weight portion), triethylamine (3 weight portion) therein, at room temperature stirred 20 hours.Filter with clear and the system ラ ジ オ ラ イ ト of chemical industry society Off ア イ Application Off ロ-A, the PF-5080 in the filtrate is volatilized, obtain compound 1 (20 weight portion) with evaporator.
(synthesizing of compound 2)
Except that replacing Chisso (strain) system サ イ ラ エ-ス S330 (3 weight portion), to obtain compound 2 (20 weight portion) with the synthetic identical mode of compound 1 with Chisso (strain) system サ イ ラ エ-ス S360 (3 weight portion).
(synthesizing of compound 3)
Except that replacing the Network ラ イ ト Star Network ス 157FS-L (mean molecular weight 2500) (25 weight portion) of DUPONT company manufacturing, to obtain compound 3 (30 weight portion) with the synthetic identical mode of compound 1 with the system デ system Na system SH (mean molecular weight 3500) of Daikin Industries society (35 weight portion).
(synthesizing of compound 4)
Remove with Chisso (strain) system サ イ ラ エ-S360 (3 weight portion) and replace Chisso (strain) system サ イ ラ エ-S330 (3 weight portion), replace with the system デ system Na system SH (mean molecular weight 3500) of Daikin Industries society (35 weight portion) outside the Network ラ イ ト Star Network 157FS-L (mean molecular weight 2500) (25 weight portion) of DUPONT company manufacturing, to obtain compound 4 (30 weight portion) with the synthetic identical mode of compound 1.
(synthesizing of compound 5)
Except that replacing the Network ラ イ ト Star Network 157FS-L (mean molecular weight 2500) (25 weight portion) of DUPONT company manufacturing, to obtain compound 5 (3.5 weight portion) with the synthetic identical mode of compound 1 with Daikin Industries society system 7H-12 fluoro enanthic acid (molecular weight 346.06) (3.5 weight portion).
(synthesizing of compound 6)
Remove with Daikin Industries society system 7H-12 fluoro enanthic acid (molecular weight 346.06) (3.5 weight portion) and replace the Network ラ イ ト Star Network 157FS-L (mean molecular weight 2500) (25 weight portion) that DUPONT company makes, replace outside Chisso (strain) system サ イ ラ エ-S310 (2 weight portion), with Chisso (strain) system サ イ ラ エ-S320 (2 weight portion) to obtain compound 6 (3.5 weight portion) with the synthetic identical mode of compound 1.
(synthesizing of compound 7)
Except that replacing the Network ラ イ ト Star Network 157FS-L (mean molecular weight 2500) (25 weight portion) of DUPONT company manufacturing, to obtain compound 7 (4.5 weight portion) with the synthetic identical mode of compound 1 with the system 9H-ten hexafluoro nonane acid (molecular weight 446.07) (4.5 weight portion) of Daikin Industries society.
(synthesizing of compound 8)
Remove with the system 9H-ten hexafluoro nonane acid (molecular weight 446.07) (4.5 weight portion) of Daikin Industries society and replace the Network ラ イ ト Star Network 157FS-L (mean molecular weight 2500) (25 weight portion) that DUPONT company makes, replace outside Chisso (strain) system サ イ ラ エ-S310 (2 weight portion), with Chisso (strain) system サ イ ラ エ-S320 (2 weight portion) to obtain compound 8 (4.5 weight portion) with the synthetic identical mode of compound 1.
Hate liquid film formation method
At first in solvent, be dissolved in end and have the perfluoro polyether compound or the all-fluoroalkyl compound of alkoxysilane group.Concentration is according to coating process two differences, but probably is 0.01～1.0 weight %.Because alkoxysilane group is slowly by moisture in the solvent or the moisture hydrolysis that enters solvent from air, thus the preferred solvent dehydration, perhaps select to resemble be difficult to the fluorine kind solvent to dissolve water material.FC-72, FC-77, PC-5060, PC-5080, HFE-7100, HFE-7200, DUPONT society that concrete fluorine kind solvent is enumerated 3M society make バ-ト レ Le XF etc.The liquid (be designated as later on and hate the liquid treating agent) of perfluoro polyether compound or all-fluoroalkyl compound has been dissolved in such modulation.
The liquid treating agent is hated in coating on the antireflection film surface below.What the method for coating adopted is coating process commonly used such as dip-coating, spin coating.Next heat.Heating be the hydroxyl that forms alkoxy silane residue and surface etc. in conjunction with the time necessity condition, usually 120 ℃ of heating 10 minutes, just be through with in 30 minutes 100 ℃ of heating.To heat 1 hour at 90 ℃.Need a lot of times at normal temperatures.
At last,, remove the remaining liquor of hating, hate the liquid processing to finish with fluorine kind solvent flushing surface.The solvent that uses during flushing can adopt the solvent by the explanation prompting of hating the liquid treating agent.
(3) about being used in lens, projector etc.
The synoptic diagram of the optical system of front projector type image display device shown in Figure 5.
The order of the light formation image light from lamp to output below is shown.
Assemble by catoptron 12 by the white light that lamp 11 produces, by concavees lens 13 to 14 outgoing of the 1st lens arra.The 1st lens arra makes it pass through the mode channeling conduct of the 2nd lens arra 15 and polarization 16 effectively incident beam is divided into a plurality of light beams.The lens unit that constitutes the 2nd lens arra is respectively with the image projection of the lens unit of the 1st lens arra of the correspondence side to the image-displaying member 17,18,19 corresponding with RGB (RGB) three primary colors.The projected image of each lens unit of the 1st lens arra is overlapped onto on each image-display units 17,18,19 by convergent lens 20 and collector lens 21 and 22,23, the 1st relay lens the 24, the 2nd relay lens 25.And, in optical system, also be provided for changing the reflective mirror 26～29 of direction of light.In said process, will be separated into the RGB three primary colors by the white light that light source produces by spectroscope 30,31, shine on each self-corresponding image-displaying member 17,18,19.It is synthetic that image on the image-displaying member 17,18,19 carries out color by look synthetic prisms 32, by projecting lens 33 to screen 34 projections, thereby form big picture image.The 1st relay lens the 24, the 2nd relay lens 25 is to be used for compensation to compare with image-displaying member 17,18, from the elongated parts of light path of the light source of image-displaying member 19.Collector lens the 21,22, the 23rd suppresses the parts that broaden by the light behind the image-display units 17,18,19 for effective projection of carrying out projecting lens.
Because by with various lens, lens arra, polarization, image-displaying member and look synthetic prisms such as bulb by lamp of the light of upper type output, convergent lens, relay lens, collector lenses, so at these light is on this two sides of sensitive surface and exiting surface antireflection film to be set by face, thereby the inhibition surface reflection improves photopermeability.And, antireflection film equally also is set on spectroscopical transparent surface, to suppress surface reflection, improve light transmission.
The synoptic diagram of the optical system of rear projection image display device shown in Figure 6.
In shell 35, have optical unit 36 (removing the outer part of screen of the optical system of Fig. 5) and back reflector 37.The light that comes out from optical unit projects on the screen 38 after being changed direction by back reflector.So image just is displayed on the screen.
Because on the two sides of the transparent surface of screen the reflection antireflection film is set all, so surface reflection is inhibited, light transmission has improved.
The reflecting surface 39 of catoptron is arranged on the occasion on the one side (shell side of Fig. 6) of glass plate 40 overleaf, as shown in Figure 7, the incident light 41 that comes out from optical unit is divided into image light 42 and reflected light 43 by glass surface, project on the screen, so can see dual imaging, there is the problem that precision is reduced in the result.
Therefore, also confirmed by the incident light side at glass antireflection film 44 to be set, can reduce reflected light, the result can suppress the decline of precision.
(4) other purposes
The antireflection film of present embodiment can be formed on glass and the lens substrates such as polycarbonate, acryl resin.
Therefore for hope not reflected sunlight ground effectively the purposes of absorption be effective.As this purposes, at first enumerate the parts of transmitted rays such as lens that various optical devices adopt, light filter.As their purposes, enumerate the image recording structure of employing liquid crystal projection apparatus, microscope, telescope, camera, televisor and DVD etc.In addition, enumerate and be used for realizing the stable of plant etc. and the application of the transparent wall in the greenhouse of rapidly growth etc.Perhaps be set forth in for inhibitory reflex (mirroring), improve visibility and be application in the transparent wall of tank etc. of purpose with the observation appreciation of animals and plants, insect, fish etc. etc.
Equally, also enumerate for inhibitory reflex (mirroring), improve visibility, and the present invention is used in the application in the image display devices such as LCD that the demonstration of TV and mobile phone, navigational system, car speed and rotation number etc. adopts, plasma scope, organic light emission (organic EL) display.Specifically, be suitable for being formed on the surface of display area of these display device.
In addition, also enumerate application in the antireflection film that on the solar cell panel surface, forms for the generating efficiency that improves sunshine.Except that sunshine, because the also effectively incident of light such as laser, so also be effective for the surface of optical recording media.
Except that preventing reflection, thereby because film has the feature that dust such as the low dust of resistance is difficult to adhere to, so even under the many environment of low winter of humidity and dust, light transmission and visibility have also improved.In addition, by giving lyophobicity, soil resistance has also improved, so also cause light transmission and visibility to improve.Because have these features, so the transparency carrier with film of the present invention also is effective as indoor building materials such as the wall of dirt pocket or compartments.
The optics of antireflection film can be accessed,, high performance image display device can be obtained by utilizing this optics with low resistance, high adaptation and low-refraction.
Even also have under hot and humid environment, also be difficult to produce the feature of mould on the antireflection film surface.
Below, according to embodiment the present invention is carried out more specific description, but scope of the present invention is not limited to these embodiment.
[embodiment 1]
At first be illustrated in the method that forms antireflection film on the convex lens.
(1) washing
The acryl resin system lens of diameter 100mm are placed in the tank that has added water, make after the internal vibration, use distilled water flushing, remove the dirt of lens surface with ultrasonic washer.
(2) modulation antireflection coating
As bonding agent, (main solvent is a water to silicon dioxide gel solution, the alkoxysilane polymer that contains 10 weight %) (2 weight portion), inorganic oxide particle is 5 weight % dispersion liquids (35 weight portion) of the monox of the about 60nm of major axis average length, mixed water (80 weight portion) therein, and modulation is used to form the coating (being called antireflection coating later on) of antireflection film.
(3) coating antireflection coating
By spin coating this coating is coated on the washing lens afterwards of having carried out (1).Coating after the coating extends on lens when observing with eyes substantially equably.
(4) heating
After the spin coating, apace lens are put into the calibration cell that is controlled at 90 ℃, heated 10 minutes.Thereby silicon dioxide gel becomes monox, and heat curing finishes.So forming the glass plate of antireflection film has from the teeth outwards just finished.
(5) to the processing at the back side
Upset has formed the glass plate of antireflection film from the teeth outwards, carries out the processing of above-mentioned (1), (3), (4), also forms the antireflection film identical with the surface overleaf.
(6) assessment experiment
With the thickness and the refractive index of the antireflection film that forms on ellipsometer (ellipsometer) the mensuration glass plate, be respectively 120nm and 1.25.
Mensuration forms the reflectivity of the lens behind the antireflection film.During mensuration, the reflectivity when the research wavelength is the highest 550nm of human visibility.Consequently, the reflectivity that is provided with the lens of antireflection film is 0.5%.Do not have the reflectivity of the acryl resin system lens of antireflection film to be about 8%, confirm that film has anti-reflective function.
The transmissivity in research 550nm time.Consequently, the transmissivity that is provided with the lens of antireflection film is 99%.Do not have the transmissivity of the acryl resin system lens of antireflection film to be about 92%, confirm that film has the function that improves light transmission.
When having formed the cross section of antireflection film, as shown in Figure 3, confirm to have the space of size 5～150nm with tem observation.And few in the substrate-side space if observe the cross section of film, along with moving to face side, the ratio in space increases.Thereby can access in the refractive index of substrate-side, at the film of face side near the refractive index of air near membrane material.Thereby the refringence of inferring each interface is little, can prevent the reflection at each interface.In following embodiment, it also is same that the space in the film distributes.
When mensuration has formed the surface resistivity of lens of antireflection film, under the condition of 20 ℃ of temperature, humidity 50%, be 1 * 10
10Ω.Mensuration is carried out according to ASTM D-257.The surface resistivity of lens that does not form antireflection film is 1 * 10
16More than the Ω.Therefore, compare with the lens that do not have antireflection film, the lens of band antireflection film are difficult to charged, and the dust difficulty is adhered to.
Below, in order to study the adaptation of antireflection film, carry out the section line test.Consequently, do not see peeling off that adhesive tape causes fully.
[embodiment 2]
Except that being identically formed lens with antireflection film with the glass lens substitutional crylic acid resin system lens of identical size and (1)～(5) of embodiment 1.
When carrying out the assessment identical with embodiment 1 (6), thickness, refractive index are respectively 120nm and 1.25.Reflectivity during 550nm is 0.5%.There is not the reflectivity of the glass lens of antireflection film to be about 8%.Confirm that film has anti-reflective function.
The transmissivity in research 550nm time.Consequently, the transmissivity that is provided with the lens of antireflection film is 99%.Do not have the transmissivity of the acryl resin system lens of antireflection film to be about 92%, confirm that film has the function that improves light transmission.
Identical with embodiment 1, when mensuration has formed the surface resistivity of lens of antireflection film, under the condition of 20 ℃ of temperature, humidity 50%, be 1 * 10
10Ω.The surface resistivity that does not form the lens of antireflection film is 1 * 10
12Ω.Therefore, compare with the lens that do not have antireflection film, the lens of band antireflection film are difficult to charged, and dust is difficult to adhere to.
Identical with embodiment 1, in order to study the adaptation of antireflection film, carry out the section line test.Consequently, do not see peeling off that adhesive tape causes fully.
[comparative example 1]
Removing the antireflection film parts is magnesium fluorides, and is not coating but makes outside the film and (1)～(5) of embodiment 1 are identically formed the lens of band antireflection film by evaporation coating.
When carrying out the assessment identical with embodiment 1 (6), thickness, refractive index are respectively 120nm and 1.38.Reflectivity during 550nm is 3%.There is not the reflectivity of the acryl resin system lens of antireflection film to be about 8%.Confirm that film has anti-reflective function, but do not reach the such anti-reflective function of lens of embodiment 1.
The transmissivity in research 550nm time.Consequently, the transmissivity that is provided with the lens of antireflection film is 96%.Do not have the transmissivity of the acryl resin system lens of antireflection film to be about 92%, confirm that film has the function that improves light transmission, but the such transmitance of lens that does not reach embodiment 1 improves function.
Identical with embodiment 1, when mensuration has formed the surface resistivity of lens of antireflection film, under the condition of 20 ℃ of temperature, humidity 50%, be 2 * 10
14Ω.Therefore, compare with the lens that form among the embodiment 1, charged easily, dust adheres to easily.
Identical with embodiment 1, in order to study the adaptation of antireflection film, carry out the section line test.Consequently, observe peeling off of antireflection film on the whole zone after taping.
According to above content, compare with the lens of former band magnesium fluoride system antireflection film, confirm that lens of the present invention have the light transmission height, dust is difficult to adhere to, the antireflection film that adaptation is high.
[comparative example 2]
Removing the antireflection film parts is magnesium fluorides, and is not coating but makes outside the film and embodiment 2 is identically formed the lens of band antireflection film by evaporation coating.
When carrying out the assessment identical with embodiment 1 (6), thickness, refractive index are respectively 120nm and 1.38.Reflectivity during 550nm is 3%.There is not the reflectivity of the glass lens of antireflection film to be about 8%.Confirm that film has anti-reflective function, but do not reach the such anti-reflective function of lens of embodiment 2.
The transmissivity in research 550nm time.Consequently, the transmissivity that is provided with the lens of antireflection film is 96%.Do not have the transmissivity of the glass lens of antireflection film to be about 92%, confirm that film has the function that improves light transmission, but the such transmitance of lens that does not reach embodiment 2 improves function.
Identical with embodiment 2, when mensuration has formed the surface resistivity of lens of antireflection film, under the condition of 20 ℃ of temperature, humidity 50%, be 2 * 10
14Ω.Therefore, compare with the lens that form among the embodiment 2, charged easily, dust adheres to easily.
Identical with embodiment 2, in order to study the adaptation of antireflection film, carry out the section line test.Consequently, the part of peeling off of observing antireflection film is whole 50%.
According to above content, compare with the lens of former band magnesium fluoride system antireflection film, confirm that lens of the present invention have the light transmission height, dust is difficult to adhere to, the antireflection film that adaptation is high.
[embodiment 3]
Remove to replace lens, forming outside the antireflection film identical on the sensitive surface of polarization, this two sides of exiting surface and embodiment 1 is identically formed the polarization of band antireflection film with embodiment 1.Consequently, confirm to compare with the polarization that does not have antireflection film, the transmittance of this polarization when 550nm improved about 7%.And confirm to compare with the polarization of the band magnesium fluoride system antireflection film that adopted in the past, transmittance has also improved about 3%.
[embodiment 4]
Remove to replace lens, forming outside the antireflection film identical on the sensitive surface of image-displaying member, this two sides of exiting surface and embodiment 1 is identically formed the image-displaying member of band antireflection film with embodiment 1.Consequently, confirm to compare with the image-displaying member that does not have antireflection film, the transmittance of this image-displaying member when 550nm improved about 7%.And confirm to compare with the image-displaying member of the band magnesium fluoride system antireflection film that adopted in the past, transmittance has also improved about 3%.
[embodiment 5]
Remove to replace lens, amount to 4 at sensitive surface (3 face), the exiting surface of look synthetic prisms and go up and form outside the antireflection film identical and embodiment 1 is identically formed the look synthetic prisms of band antireflection film with embodiment 1.Consequently, confirm to compare with the look synthetic prisms that does not have antireflection film, the transmittance of this look synthetic prisms when 550nm improved about 7%.And confirm to compare with the look synthetic prisms of the band magnesium fluoride system antireflection film that adopted in the past, transmittance has also improved about 3%.
[embodiment 6]
Remove to replace lens, forming outside the antireflection film identical on spectroscopical exiting surface and embodiment 1 is identically formed the spectroscope of being with antireflection film with embodiment 1.But at mirror surface is that antireflection film is not set on the sensitive surface.Consequently, confirm to compare with the spectroscope that does not have antireflection film, the transmittance of this spectroscope when 550nm improved about 7%.And confirm to compare with the spectroscope of the band magnesium fluoride system antireflection film that adopted in the past, transmittance has also improved about 3%.
[embodiment 7]
Carrying out on the optics with antireflection film that embodiment 1～6 makes hates liquid to handle.
(1) the liquid treating fluid is hated in modulation
At first modulate the 0.5 weight % solution (solvent is the system Off ロ リ of 3M society Na-ト PF-5080) of compound 1～12.With it as hating the liquid treating fluid.And 0.1 weight %PF-5080 solution of compound 1 is designated as hates liquid treating fluid [1], 0.1 weight %PF-5080 solution of compound 2 is designated as hates liquid treating fluid [2] ... 0.1 weight %PF-5080 solution of compound 12 is designated as hates liquid treating fluid [12].
Next for relatively, adopt the 0.1 weight % solution conduct of the system サ イ ト of Asahi Glass society Star プ CTL-107M to hate liquid treating fluid [13].
(2) hate liquid processing method
Hate the occasion of liquid treating fluid [1]～[12] in employing
Each optics was flooded 3 minutes in hating the liquid treating fluid.Take out optics, in inside is heated to 95 ℃ calibration cell, placed 30 minutes.Take out optics, with PF-5080 flushing surface, remove the remaining liquid treating fluid of hating, processing finishes.
Hate the occasion of liquid treating fluid [13] in employing
Each optics was flooded 3 minutes in hating the liquid treating fluid.Take out optics, in inside is heated to 95 ℃ calibration cell, placed 90 minutes.Take out optics, processing finishes.
(3) lyophobicity assessment
The lyophobicity of the optical component surfaces after the liquid processing finishes is hated in the contact angle assessment of utilization and water.In table 1～6, export the result.
Table 1
Optics of the present invention is hating liquid to handle contact angle, refractive index, transmittance, the surface resistance of front and back to water
(on the lens of making by embodiment 1, carrying out the result who hates after liquid is handled)
*: antireflection film forms the refractive index of face.
**: compare the raising rate of the optical transmission rate of 550nm with the occasion that does not have antireflection film.
Table 2
Optics of the present invention is hating liquid to handle contact angle, refractive index, transmittance, the surface resistance of front and back to water
(on the lens of making by embodiment 2, carrying out the result who hates after liquid is handled)
*: antireflection film forms the refractive index of face.
*: compare the raising rate of the optical transmission rate of 550nm with the occasion that does not have antireflection film.
Table 3
Optics of the present invention is hating liquid to handle contact angle, refractive index, transmittance, the surface resistance of front and back to water
(on the lens of making by embodiment 3, carrying out the result who hates after liquid is handled)
*: antireflection film forms the refractive index of face.
*: compare the raising rate of the optical transmission rate of 550nm with the occasion that does not have antireflection film.
Table 4
Optics of the present invention is hating liquid to handle contact angle, refractive index, transmittance, the surface resistance of front and back to water
(on the lens of making by embodiment 4, carrying out the result who hates after liquid is handled)
*: antireflection film forms the refractive index of face.
*: compare the raising rate of the optical transmission rate of 550nm with the occasion that does not have antireflection film.
Table 5
Optics of the present invention is hating liquid to handle contact angle, refractive index, transmittance, the surface resistance of front and back to water
(on the lens of making by embodiment 5, carrying out the result who hates after liquid is handled)
*: antireflection film forms the refractive index of face.
*: compare the raising rate of the optical transmission rate of 550nm with the occasion that does not have antireflection film.
Table 6
Optics of the present invention is hating liquid to handle contact angle, refractive index, transmittance, the surface resistance of front and back to water
(on the lens of making by embodiment 6, carrying out the result who hates after liquid is handled)
*: antireflection film forms the refractive index of face.
*: compare the raising rate of the optical transmission rate of 550nm with the occasion that does not have antireflection film.
And put down in writing in the lump with the contact angle of water and refractive index and reflectivity, the surface electrical blocking solution of hating liquid to handle front and back before hating liquid to handle.
Before hating liquid to handle, arbitrary antireflection film touches less than 10 ο water.But, hate liquid to handle by execution, the contact angle of any film has all become greatly.Refractive index, reflectivity are hating liquid to handle not variation of front and back, so show that hating liquid to handle can not make the performance relevant with optical characteristics reduce.
But, only uprised with resistance after the 0.1 weight % solution-treated of サ イ ト Star プ CTL-107M.Think this be because, with サ イ ト Star プ CTL-107M cover substantially fully antireflection film surface relative be, for compound 1～12, everywhere lip-deep at antireflection film, the fluorine class chain of lyophobicity is by the alkoxysilane group combination, the result can not cover antireflection film fully, so resistance does not change substantially.If film resistance rises, then become charged film easily, the problem that dust and dust adhere to easily appears, to be difficult to be attached on the state this point on the film be suitable so the compound 1～12 that does not improve film resistance is keeping dust and dust.
According to above content, show that even also do not improve the film resistance this point from giving lyophobicity, the fluoride compound that has alkoxysilane group endways is suitable when hating liquid to handle.
Try to compare, adopt the occasion of compound 1～4, have the high tendency of contact angle according to the compound of hating liquid handle to adopt, minimum is after handling with compound 1 or 2 on the film of embodiment 2 106 °.Particularly adopting the occasion of compound 3,4, the contact angle height, any film all shows 110 ° contact angle.Soil resistance is good in other words because say the contact angle height, so wish that it is high as far as possible.Compound 1～4th has the compound of perfluoro polyether chain, other be compound with perfluoroalkyl chain or fluoro-alkyl chain.This expression can form the good film of lyophobicity when hating liquid to handle by the compound with perfluoro polyether chain.
[embodiment 8]
In coating during antireflection coating, except that be not spin coating but the dip-coating and embodiment 1 be identically formed lens with antireflection film.When studying these lens in the same manner, obtain identical result with embodiment 1 (6).Thereby show that coating process is not to be necessary for spin coating, employing dip-coating etc. also can form.
[embodiment 9]
Remove the replacement lens, lamp is carried out outside the dip-coating, carry out and embodiment 8 identical operations, form the lamp that has antireflection film from the teeth outwards.Compare with the lamp that does not have antireflection film, confirm that the light intensity of this lamp when 550nm improved about 3%.
[embodiment 10]
The optics that utilization is formed by embodiment 1～6,9, making has the image display device of optical system shown in Figure 5, when display image, compare with the image display device of the optics of former employing band magnesium fluoride system antireflection film, can form briliancy and improve about 1.5 times image.Think that this is because antireflection film has been brought into play the effect that improves light transmission.
In the occasion that magnesium fluoride system antireflection film is not set, drop to 73% of former briliancy.
[embodiment 11]
As mildewproof agent, study following 17 kinds of compounds.
Modulate the 2wt% ethanolic solution of these mildewproof agents.
Adopt following method modulation antireflection film coating below.
As bonding agent, (main solvent is the 2-propyl alcohol to silicon dioxide gel solution, contain 10 weight % alkoxysilane polymers) (2 weight portion), inorganic oxide particle is 5 weight % dispersion liquids (35 weight portion) of the monox of the about 60nm of major axis average length, mix 2-propyl alcohol (100 weight portion) therein, the 2wt%2-propanol solution of mildewproof agent (2 weight portion), the antireflection coating of mildewproof agent has been added in modulation.Here, adopt the 2-propyl alcohol to be because the cause of most of mildewproof agent only dissolving part in water as solvent.
Next, identical with embodiment 1, wash an optics of the present invention, promptly with embodiment 1 in the identical acryl resin system lens of optics that adopt, be coated with the antireflection film that the antireflection film that has added mildewproof agent replaces embodiment 1 afterwards, heat.At this moment, identical with embodiment 1, also to back side system film.Such making has the lens of the antireflection film that has added mildewproof agent.
Mensuration has the reflectivity of the lens of the antireflection film that has added mildewproof agent.The mensuration wavelength is 550nm.Consequently the reflectivity of these lens is 0.5～0.6%.Do not have the reflectivity of the acryl resin system lens of antireflection film to be about 8%, even confirm to add mildewproof agent of the present invention, film also has anti-reflective function.Study the optical transmission rate of these lens to 550nm.Consequently, the transmissivity of these lens is 99%.Do not have the transmissivity of the acryl resin system lens of antireflection film to be about 92%, confirm that film has the function that improves optical transmission.Then, carry out the section line test in order to study the adaptation of the antireflection film that has added mildewproof agent.Consequently, do not see peeling off that adhesive tape causes fully.
Then in order to confirm whether these lens have mildew resistance, these lens were placed for 1 week in 40 ℃, the high humidity calibration cell of 95%RH.And in order to compare, the lens of making among the embodiment 1 with the antireflection film that does not add mildewproof agent are also placed together.After 1 week, with the naked eye and with 5 times magnifier confirm whether to produce mould.In result shown in the table 7.
Table 7
Optics of the present invention is placed on whether produce mould in the high humidity calibration cell
| The mildewproof agent that adopts | Whether |
| Compound | |
| 13 | ○ |
| |
○ |
| |
○ |
| |
○ |
| |
○ |
| |
○ |
| |
○ |
| |
○ |
| |
○ |
| |
○ |
| |
○ |
| |
○ |
| |
○ |
| |
○ |
| |
○ |
| |
○ |
| |
○ |
| Do not add mildewproof agent | ×× |
Zero: with the naked eye and with 5 times magnifier all confirm not produce mould.
*: with the naked eye confirm not produce.But confirm to have produced mould with 5 times magnifieres.
* *: with the naked eye and with 5 times magnifier all confirms to have produced mould.
The lens that do not add mildewproof agent are placed the material that is attached with the white fiber shape after 1 week from the teeth outwards.It is analyzed, be confirmed to be mould.Do not see on the lens of the antireflection film that has added mildewproof agent that mould produces but have.
After then the lens with the antireflection film that has added mildewproof agent floods 1 hour in 40 ℃ water, 1 week of placement in 40 ℃, the high humidity calibration cell of 95%RH.After 1 week, with the naked eye and with 5 times magnifier confirm whether to produce mould.In result shown in the table 8.
Table 8
Behind the used for optical part water retting of the present invention, be placed on whether cause the mould generation in the high humidity calibration cell
| The mildewproof agent that adopts | Have or not mould to produce | The ratio of nitrogen element (weight %) in the compound | The architectural feature of |
| Compound | |||
| 13 | × | 6.15 | The |
| Compound | |||
| 14 | ○ | 5.48 | The |
| Compound | |||
| 15 | ○ | 4.12 | The |
| Compound | |||
| 16 | × | 6.48 | The |
| Compound | |||
| 17 | ○ | 5.74 | The |
| Compound | |||
| 18 | × | 6.34 | The |
| Compound | |||
| 19 | ○ | 5.96 | The |
| Compound | |||
| 20 | × | 6.71 | Two |
| Compound | |||
| 21 | ○ | 5.91 | Two pyridiniujm structures |
Zero: with the naked eye and with 5 times magnifier all confirm not produce mould.
*: with the naked eye confirm not produce.But confirm to have produced mould with 5 times magnifieres.
* *: with the naked eye and with 5 times magnifier all confirms to have produced mould.
Adopt compound 13,16,18,20 few, but see and produced mould as the lens of mildewproof agent.Compound 13～19 has the pyridiniujm structure, and compound 20,21 has two pyridiniujm structures.Nitrogen element ratio in the compound 13,16,18,20 is more than 6 weight %.If the ratio of nitrogen element is big, then the ratio of 4 grades of salt structure divisions of the nitrogen of hydrophilic pyridine ring or two pyridine rings becomes big in the compound, thereby soluble in water.Therefore, think that a part of mildewproof agent in the antireflection film is dissolved in the water owing to be immersed in 40 ℃ the water of the accelerated test that also can be described as high wet test, so the mildewproof agent in the film reduces, the result is that anti-mold effect reduces, and produces mould.
This result shows to have the occasion of the mildewproof agent of pyridiniujm structure or two pyridiniujm structures in employing, and the ratio of nitrogen is suitable less than 6 weight % in the compound.
Claims (12)
1. optics, it is the optics of transmitted ray or reflecting part light, it is characterized in that: on the exiting surface of the sensitive surface of light or light, have antireflection film, above-mentioned antireflection film is made of inorganic oxide particle and bonding agent, and the thickness of above-mentioned antireflection film is 60～190nm, and above-mentioned antireflection film has the space of 5～200nm size
Above-mentioned inorganic oxide particle is a silicon oxide particle, and above-mentioned bonding agent is made of silicon compound.
2. the optics of claim 1 record, the major axis footpath that it is characterized in that above-mentioned particulate is below 190nm, and short shaft diameter is littler than thickness.
3. the optics of claim 1 record is characterized in that having the layer that is made of fluorochemicals on the above-mentioned antireflection film surface.
4. the optics of claim 1 record is characterized in that being added with the organic compound with polyalkylene glycol chain in above-mentioned antireflection film.
5. the optics of claim 1 record is characterized in that being added with the organic compound with salt structure in above-mentioned antireflection film.
6. the optics of claim 1 record is characterized in that being added with the organic compound with pyridiniujm structure or two pyridiniujm structures in above-mentioned antireflection film.
7. the optics of claim 1 record it is characterized in that being added with the organic compound with pyridiniujm structure or two pyridiniujm structures in above-mentioned antireflection film, and the element ratio of this nitrogen in organic compounds is less than 6 weight %.
8. the optics of claim 1 record is characterized in that being added with the organic compound with pyridine-N-oxides structure or two pyridine-N-oxides structures in above-mentioned antireflection film.
9. the optics of claim 1 record is characterized in that being added with the organic compound with benzimidazole structure or thiazole structure in above-mentioned antireflection film.
10. the optics of claim 1 record is characterized in that being added with the organic compound with halogen atom and carbamic acid ester structure in above-mentioned antireflection film.
11. the optics of claim 1 record is characterized in that above-mentioned optics is lens, polarization, spectroscope, look synthetic prisms, the bulb of lamp, back reflector, front panel.
12. projection type video display device, make from outgoing after the beam reflection of light source, with the light intensity of display element modulation from the outgoing beam of this light source, amplify demonstration modulate light intensity image light afterwards with projecting lens, it is characterized in that: at a plurality of lens that are assembled into above-mentioned projection type video display device inside, polarization, spectroscope, the look synthetic prisms, the bulb of lamp, back reflector, be formed with antireflection film at least one sensitive surface of at least one parts in the front panel
Above-mentioned antireflection film is made of inorganic oxide particle and bonding agent, and the thickness of above-mentioned antireflection film is 60～190nm, and above-mentioned antireflection film has the space of 5～200nm size, and above-mentioned inorganic oxide particle is a silicon oxide particle, and above-mentioned bonding agent is made of silicon compound.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2005254303A JP4760237B2 (en) | 2005-09-02 | 2005-09-02 | Optical component and projection-type image display device using the same |
| JP2005254303 | 2005-09-02 | ||
| JP2006089836 | 2006-03-29 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1924617A CN1924617A (en) | 2007-03-07 |
| CN100465665C true CN100465665C (en) | 2009-03-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101262187A Active CN100465665C (en) | 2005-09-02 | 2006-08-28 | Optical part and projection type display apparatus using same |
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| JP (1) | JP4760237B2 (en) |
| CN (1) | CN100465665C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102253585A (en) * | 2010-05-20 | 2011-11-23 | 鸿富锦精密工业（深圳）有限公司 | Projection screen and system and manufacture method of projection screen |
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| US8550552B2 (en) | 2009-01-26 | 2013-10-08 | Ts Tech Co., Ltd. | Vehicle seat |
| FR2969313B1 (en) * | 2010-12-16 | 2012-12-21 | Essilor Int | OPTICAL ELEMENT COMPRISING A NON-CRACKING AEROGEL |
| WO2012157719A1 (en) | 2011-05-17 | 2012-11-22 | キヤノン電子株式会社 | Optical filter and optical device |
| WO2015159829A1 (en) * | 2014-04-14 | 2015-10-22 | 国立大学法人東京工業大学 | Film for transparent screen, method for manufacture thereof, and transparent screen comprising same |
| CN106646698A (en) * | 2017-01-23 | 2017-05-10 | 中山市光大光学仪器有限公司 | Gluing prism set |
| US10459123B2 (en) | 2017-03-10 | 2019-10-29 | Canon Kabushiki Kaisha | Optical member, image pickup apparatus, and method for manufacturing optical member |
| JP6932524B2 (en) | 2017-03-10 | 2021-09-08 | キヤノン株式会社 | Optical member and manufacturing method of optical member |
| JP7118614B2 (en) | 2017-03-10 | 2022-08-16 | キヤノン株式会社 | OPTICAL MEMBER, IMAGING DEVICE, AND OPTICAL MEMBER MANUFACTURING METHOD |
| JP6580101B2 (en) | 2017-09-29 | 2019-09-25 | 日東電工株式会社 | Void layer, laminate, method for producing gap layer, optical member and optical device |
| CN114966935A (en) * | 2018-11-12 | 2022-08-30 | 日东电工株式会社 | Polarizing film, laminated polarizing film, image display panel, and image display device |
| JPWO2021006126A1 (en) * | 2019-07-10 | 2021-01-14 |
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Also Published As
| Publication number | Publication date |
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| JP2007065522A (en) | 2007-03-15 |
| CN1924617A (en) | 2007-03-07 |
| JP4760237B2 (en) | 2011-08-31 |
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