CN101042438B - Method for producing layered material comprising layer with inorganic particles - Google Patents
Method for producing layered material comprising layer with inorganic particles Download PDFInfo
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- CN101042438B CN101042438B CN2007100878393A CN200710087839A CN101042438B CN 101042438 B CN101042438 B CN 101042438B CN 2007100878393 A CN2007100878393 A CN 2007100878393A CN 200710087839 A CN200710087839 A CN 200710087839A CN 101042438 B CN101042438 B CN 101042438B
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- 239000010954 inorganic particle Substances 0.000 title claims abstract description 123
- 239000000463 material Substances 0.000 title claims abstract description 37
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 133
- 239000006185 dispersion Substances 0.000 claims abstract description 58
- 230000015271 coagulation Effects 0.000 claims abstract description 51
- 238000005345 coagulation Methods 0.000 claims abstract description 51
- 238000000034 method Methods 0.000 claims abstract description 35
- 238000000576 coating method Methods 0.000 claims abstract description 22
- 239000011248 coating agent Substances 0.000 claims abstract description 21
- 239000000758 substrate Substances 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims description 41
- 238000009826 distribution Methods 0.000 claims description 14
- 238000007561 laser diffraction method Methods 0.000 claims description 13
- 238000000790 scattering method Methods 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000741 silica gel Substances 0.000 claims description 12
- 229910002027 silica gel Inorganic materials 0.000 claims description 12
- 239000000084 colloidal system Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 230000001186 cumulative effect Effects 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 3
- 238000009825 accumulation Methods 0.000 claims description 2
- 125000003158 alcohol group Chemical group 0.000 claims 1
- 239000000701 coagulant Substances 0.000 abstract description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 27
- 239000002585 base Substances 0.000 description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 239000007787 solid Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 229920002284 Cellulose triacetate Polymers 0.000 description 7
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- -1 acryl Chemical group 0.000 description 4
- 239000000470 constituent Substances 0.000 description 4
- 238000002296 dynamic light scattering Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 238000002310 reflectometry Methods 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- 238000004438 BET method Methods 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- SMEGJBVQLJJKKX-HOTMZDKISA-N [(2R,3S,4S,5R,6R)-5-acetyloxy-3,4,6-trihydroxyoxan-2-yl]methyl acetate Chemical compound CC(=O)OC[C@@H]1[C@H]([C@@H]([C@H]([C@@H](O1)O)OC(=O)C)O)O SMEGJBVQLJJKKX-HOTMZDKISA-N 0.000 description 1
- 229940081735 acetylcellulose Drugs 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- HGAZMNJKRQFZKS-UHFFFAOYSA-N chloroethene;ethenyl acetate Chemical compound ClC=C.CC(=O)OC=C HGAZMNJKRQFZKS-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000003851 corona treatment Methods 0.000 description 1
- 229920005994 diacetyl cellulose Polymers 0.000 description 1
- OBNCKNCVKJNDBV-UHFFFAOYSA-N ethyl butyrate Chemical compound CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000007763 reverse roll coating Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical compound [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/113—Anti-reflection coatings using inorganic layer materials only
- G02B1/115—Multilayers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D11/00—Producing optical elements, e.g. lenses or prisms
- B29D11/00865—Applying coatings; tinting; colouring
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/133502—Antiglare, refractive index matching layers
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/86—Arrangements for improving contrast, e.g. preventing reflection of ambient light
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J2211/00—Plasma display panels with alternate current induction of the discharge, e.g. AC-PDPs
- H01J2211/20—Constructional details
- H01J2211/34—Vessels, containers or parts thereof, e.g. substrates
- H01J2211/44—Optical arrangements or shielding arrangements, e.g. filters or lenses
- H01J2211/442—Light reflecting means; Anti-reflection means
Landscapes
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Physics & Mathematics (AREA)
- Nonlinear Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mathematical Physics (AREA)
- Health & Medical Sciences (AREA)
- Mechanical Engineering (AREA)
- Ophthalmology & Optometry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Surface Treatment Of Optical Elements (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Laminated Bodies (AREA)
Abstract
The invention provides a method for producing layered material comprising layer with inorganic particles on a substrate, which comprises the following processes (1)-(3) of process (1): adding coagulant to a dispersion liquid (A) comprising a liquid medium and inorganic particles dispersed therein to obtain a coagulation liquid (B) with at least partial of the inorganic particles coagulated; process (2): coating above-mentioned coagulation liquid (B) on the substrate; and process (3): removing liquid medium from the coated coagulation liquid (B) and forming a film made up of inorganic particles on the substrate.
Description
Technical field
The present invention relates to a kind of manufacture method with duplexer of layer with inorganic particles, particularly a kind of manufacture method that comprises the duplexer of layer with inorganic particles relates to the method for making the method for the outstanding antireflection film duplexer of antireflection property and can being suitable for effectively as low-cost.
Background technology
In the various displays of LCD, PDP, CRT, organic EL, inorganic EL, FED and so on, because the exterior light of sunshine or fluorescent light reflects on the surface, so generation is mirrored or dazzling generation, the problem of visual identity reduction.
The reason of the problems referred to above is in the refractive index of display surface violent variation to have taken place, in order to relax these problems, known have at display surface form the technology that is lower than the antireflection film that the material of the material that constitutes display surface constitutes by refractive index.Known in theory: the material that constitutes display surface is that the refractive index of base material is n2, when the refractive index of the antireflection film that forms on this base material is n1, if satisfy n1=(n2)
0.5Relation, then reflectivity is 0.Base material is under the situation of acryl resin, about n2=1.5, so the best antireflection film that is made of the material about n1=1.2.But, as the known magnesium fluoride of the material of low refractive index film, because refractive index is about 1.38, so, can not obtain sufficient anti-reflection effect even use such material to form antireflection film.
As the outstanding antireflection film of anti-reflection effect, there is the antireflection film of the hollow minute particle in cavity known use inside.By making the granule interior cavityization, as the refractive index reduction of particle, the result can form low refractive index film, obtains high anti-reflection effect (with reference to patent documentation 1).
Patent documentation 1: the spy opens the 2003-201443 communique
But if use aforesaid hollow minute particle, then cost uprises.
Summary of the invention
The invention provides a kind of can be used as cheap make the method for the outstanding antireflection film duplexer of antireflection property and can be suitable for effectively, have a manufacture method of the duplexer of base material and layer with inorganic particles.
The present invention is a kind of manufacture method of duplexer, and it is the manufacture method of the duplexer that forms at the folded film that is made of inorganic particles of layers on substrates, wherein, comprises following operation (1)～(3).
Operation (1): in the dispersion liquid (A) of the inorganic particles that contains liquid medium and in this liquid medium, disperse, add polycoagulant, thereby the operation of the coagulation liquid (B) of cohesion takes place at least a portion that obtains the inorganic particles that contains in the described dispersion liquid (A),
Operation (2): on base material the coating described coagulation liquid (B) operation and
Operation (3):, on described base material, form the operation of the film that constitutes by described inorganic particles by from the coagulation liquid (B) of coating, removing liquid medium.
Utilize method of the present invention, can make the outstanding antireflection film duplexer of antireflection property with low cost.
Embodiment
Antireflection film among the present invention is meant with as described below to be the film of purpose, that is: be configured in LCD, PDP, CRT, organic EL, inorganic EL, FED and so on various displays the surface or inner, prevent in mirroring that display surface generation exterior light causes; Or prevent that the luminophor of display interior or the light that luminescent layer produces from reflecting in display interior, and the result causes light penetration to reduce, and the brightness of display reduces.
One of the present invention is the manufacture method of the duplexer that forms at the folded film that is made of inorganic particles of layers on substrates.In the present invention,, preferably use transparent base,, can from the transparent plastic film of mechanical rigid with appropriateness or thin slice and clear glass, suitably select to use according to the purposes of goods as base material.As the object lesson of plastic sheeting or thin slice, can enumerate film or thin slices such as polyethylene terephthalate, tygon, polypropylene, viscose paper, triacetyl cellulose, diacetyl cellulose, acetylcellulose butyric ester, polymethylmethacrylate.Because the transparency is outstanding and do not have optical anisotropy, so preferred film or the thin slice that is made of triacetyl cellulose or polyethylene terephthalate.
Method of the present invention is manufactured on the duplexer that the folded film that is made of inorganic particles of layers on substrates forms, and in order to form the film that is made of inorganic particles, uses the dispersion liquid (A) of the inorganic particles that contains liquid medium and disperse in this liquid medium.As inorganic particles, can enumerate particulates such as monox, titanium dioxide, aluminium oxide, zinc paste, tin oxide, lime carbonate, barium sulphate, talcum, porcelain earth.
Method of the present invention is added polycoagulant in this dispersion liquid (A), coating makes the coagulation liquid (B) that at least a portion cohesion of the inorganic particles that contains in this dispersion liquid (A) obtains on substrate surface, and the colloid that in order to ensure the stability of the condensed system of this coagulation liquid of coating when (B) on base material, that the dispersion liquid of use (A) is preferably is charged, inorganic particles stably disperses in liquid medium because of electric charge.This colloid can be hydrophilic colloid or hydrophobic colloid.Liquid medium is under the situation of water, and dispersion liquid (A) is preferably hydrophilic colloid, the preferred especially silica gel because size distribution is little.
The liquid medium of dispersion liquid (A) can make water or volatile organic solvent.Inorganic particles is separated under the situation of colloidal, can carries out the pH adjustment or add electrolyte, spreading agent.In addition, disperse equably, also can be suitable for and utilize stirrer stirring, ultrasonic dispersing, UHV (ultra-high voltage) to disperse gimmicks such as (super-high-pressure homogenization devices) in order to make inorganic particles.Concentration to the inorganic particles in the dispersion liquid (A) is not particularly limited, and from the viewpoint of the screening characteristics of dispersion liquid (A) base material, is preferably 1～20 weight %.
Dispersion liquid (A) is preferably in the size distribution figure of the transverse axis particle diameter that utilizes the laser diffraction and scattering method to measure this dispersion liquid to obtain, longitudinal axis frequency, the particle diameter that top Ra represents is in the scope of 0.01～1 μ m, and, has D utilizing the laser diffraction and scattering method to measure among the cumulative particle size distribution figure that this dispersion liquid obtains
90Following size particles accumulation number is 90% o'clock of whole granule numbers, particle diameter D
90Be below the 1 μ m.Top Ra is meant the highest peak in above-mentioned size distribution figure.From the viewpoint of the homogeneity of filming that forms, the particle diameter that the top Ra of preferred dispersion liquid (A) represents is in the scope of 0.05～0.5 μ m.
Operation of the present invention (1) is to add polycoagulant in above-mentioned dispersion liquid (A), thereby the operation of the coagulation liquid (B) of cohesion takes place at least a portion that obtains the inorganic particles in the described dispersion liquid (A).
Described polycoagulant is meant to have and makes the inorganic particles that disperses in the liquid medium that the material of the effect of cohesion take place.Dispersion liquid (A) is under the situation of colloidal state, and inorganic particles condenses by electrolytical interpolation.As electrolyte, can enumerate citrate, tartrate, sulfate, acetate, nitrate, chloride, bromide, iodide, thiocyanate, sodium carboxymethyl cellulose, mosanom etc.In addition, also can use by having the polymer coagulant that polymer of monomers such as nonionic macromolecules such as the polyvinyl alcohol (PVA) that makes the inorganic particles cohesion, methylcellulose or acrylic acid, acrylamide, PAA, dimethyl amino ethyl methacrylate constitute.In addition, can make under the situation of the inorganic particles cohesion in the dispersion liquid by adding acid or alkali adjustment pH, such acid or alkali also are equivalent to polycoagulant.
At dispersion liquid (A) is under the situation of hydrophilic colloid, by use dewatering agent or dewatering agent with electrolytical and with making up as polycoagulant, inorganic particles is condensed.At this, dewatering agent is meant that the surface with the inorganic particles from hydrophilic colloid removes the material of the effect of hydrate water, alcohols such as particular methanol, ethanol, propyl alcohol, isopropyl alcohol.
The coagulation liquid (B) that obtains in operation of the present invention (1) is to add the material that polycoagulant obtains in by dispersion liquid (A), this coagulation liquid (B) in the size distribution figure of the transverse axis particle diameter that utilizes the laser diffraction and scattering method to measure this coagulation liquid to obtain, longitudinal axis frequency, the preferred peak Rb that has the particle diameter more than 20 times of the particle diameter shown in the above-mentioned top Ra of expression.By using such coagulation liquid (B), can utilize antireflection property to form outstanding antireflection film.Coagulation liquid (B) be preferably in this size distribution figure exist the expression particle diameter be the particle diameter shown in the Ra of top more than 50 times so that the coagulation liquid of preferred peak Rb more than 100 times.
Operation of the present invention (2) is the operation of the above-mentioned coagulation liquid of coating (B) on base material, and operation (3) is for by removing the operation of the film that liquid medium is made of above-mentioned inorganic particles in above-mentioned base material formation from the coagulation liquid (B) that applies.Coagulation liquid (B) can be in the one or both sides coating of base material.The coating of coagulation liquid (B) on base material can be used applying devices such as roll coater, reverse roll coating machine, photogravure coating machine, scraper coating machine, scraper coating machine.Preferably on the face of the coagulation liquid (B) of coated substrate, implement pre-treatments such as corona treatment, ozone treatment, plasma treatment, flame treatment, electron ray processing, tackifier coating processing, cleaning treatment in advance.In addition,, can use to have, on such superficial layer, apply coagulation liquid (B) containing the base material of such as the antistatic backing of the hard conating that constitutes by uv curing resin etc. or electrically conductive microparticle etc. as superficial layer as base material.Operation (3) is removed liquid medium from the coagulation liquid (B) that applies at base material, usually by making its volatilization remove this liquid medium.The temperature (baking temperature) of this moment is generally room temperature～200 ℃.On the base material two sides, apply coagulation liquid (B), after forming under the situation of the film that constitutes by inorganic particles on the two sides of base material, can on the one side of base material, forming film, further form film, also can on the two sides, form simultaneously at another side.
Suppositions such as inventor utilize the film of the inorganic particles that such method forms on base material, by contacting between the inorganic particles, form the space.This space shows and the substantially the same refractive index of refractive index (refractive index 1.0) of air that so have the film in such space, its refractive index is lower.
The thickness of the inorganic particles that forms on the method preferred substrates of the present invention is in 50～150nm scope, more preferably in the scope of 80～130nm.Particularly under the situation of the duplexer that will make as the anti-reflection member use of display apparatus, the top layer that constitutes display with the film of this inorganic particles prevents under the situation of outside reflection of light, if consider catoptrical interference effect, the thickness of inorganic particles is preferably in above-mentioned scope.The thickness of inorganic particles can be by concentration or the coating method control of selecting particle aggregation liquid (B).In addition, the thickness of the film of inorganic particles is the mean value in 10 above Determination of thickness values of point of thickness direction cross-section determination of this film.
As a mode of the present invention, the inorganic particles that contains in the dispersion liquid (A) is preferably the inorganic particles that mean grain size Da is 1～300nm (C).Dispersion liquid by using such inorganic particles (C) to disperse can form the outstanding inorganic particles film of homogeneity.In addition, the mean grain size of inorganic particles (C) is meant the value of utilizing BET method or laser diffraction and scattering method to measure.
As another mode of the present invention, the inorganic particles that contains in the dispersion liquid (A) is preferably the inorganic particles (C) of mean grain size in 30～300nm scope of 55～90 weight % and the potpourri of the inorganic particles (D) of mean grain size in 1～20nm scope of 10～45 weight % (wherein, inorganic particles (C) is 100 weight % with the total amount of inorganic particles (D)).By using such dispersion liquid (A), can make it form the outstanding film of intensity.In addition, the mean grain size of inorganic particles (D) is meant the value of utilizing Sears (Sears) method or dynamic light scattering determination.
As dispersion liquid (A), use under the situation of dispersion liquid of potpourri of above-mentioned inorganic particles (C) or inorganic particles (C) and inorganic particles (D), in this dispersion liquid (A), add the coagulation liquid (B) that polycoagulant obtains, in the size distribution figure of the transverse axis particle diameter that utilizes the laser diffraction and scattering method to measure this coagulation liquid to obtain, longitudinal axis frequency, preferable particle size is more than 1% of cumulative volume that the volume of the flocculated particle more than 20 times of the particle diameter shown in the described top Ra adds up to the inorganic particles in this coagulation liquid (B).By using such coagulation liquid, can form the outstanding antireflection film of antireflection property.
As further other modes of the present invention, the inorganic particles that contains in the dispersion liquid (A) is preferably chain inorganic particles (E).The chain inorganic particles is meant that common 3 above spherical particles are linked to be the inorganic particles of chain.By using such chain inorganic particles (E) to disperse the dispersion liquid (A) that forms, form the outstanding antireflection film of antireflection property and become possibility.
As other modes of the present invention, the inorganic particles that contains in the dispersion liquid (A) is preferably the chain inorganic particles (E) of 55～90 weight % and the potpourri of the inorganic particles (F) of mean grain size in 1～20nm scope of 10～45 weight % (wherein, inorganic particles (E) is 100 weight % with the total amount of inorganic particles (F)).(wherein, inorganic particles (E) is 100 weight % with the total amount of inorganic particles (F)) by using such dispersion liquid (A), can make it form the outstanding film of intensity.Use in the antireflection film of such dispersion liquid (A) formation, inorganic particles (F) is present in the surface and the gap of chain inorganic particles (E), plays the effect that links inorganic particles (E), so can become the outstanding film of intensity.In addition, the mean grain size of inorganic particles (F) is meant the value of utilizing Sears method or dynamic light scattering determination.
As dispersion liquid (A), use contains under the situation of dispersion liquid of potpourri of above-mentioned chain inorganic particles (E) or chain inorganic particles (E) and inorganic particles (F), in this dispersion liquid (A), add the coagulation liquid (B) that polycoagulant obtains, in the size distribution figure of the transverse axis particle diameter that utilizes laser diffraction and scattering method mensuration to obtain, longitudinal axis frequency, preferable particle size is more than 5% of cumulative volume that the volume of the flocculated particle more than 20 times of the particle diameter shown in the described top Ra adds up to the inorganic particles in this coagulation liquid (B).By using such coagulation liquid, can form the outstanding antireflection film of antireflection property.
In the dispersion liquid that contains chain inorganic particles (E) (A), add the flocculated particle that polycoagulant forms, owing to connect by chain between the spherical particle of this chain inorganic particles (E) of formation, so be difficult to closely fill, form antireflection film easily with appropriate space.
On the degree of not damaging anti-reflection effect, the dispersion liquid that uses among the present invention (A) also can add resin binder.In addition, can form on base material after the inorganic particles film, stacked resin binder on this film perhaps also can make in the resin binder infiltration film.In addition, utilize method of the present invention on the inorganic particles film that forms on the base material, also can further form the stain-proofing layer that constitutes by the fluorine based compound.
The duplexer that utilizes the present invention to obtain can use with member as optics such as polaroid, diffuser plate, light guide plate, brightness improving film, reflecting polarizers by suitably selecting base material.In addition, also can fit on the surface of member and formed plastic sheeting or the thin slice or the glass of antireflection film at above-mentioned various optics.
[embodiment]
The present invention will be described in more detail below to utilize embodiment, but the present invention is not limited by it.Base material uses the description Off イ of Fuji Le system system triacetylcellulose film.The reflectivity of this film surface is 4.0%, transmitance is 93.0%.In addition, utilize following method to carry out the evaluation of embodiment.
(1) size-grade distribution:
Size-grade distribution uses hole Games to make made laser diffraction/diffuse transmission type particle size distribution device LA-910, utilizes the flow cell mode to measure.During mensuration, the isopropyl alcohol concentration in the liquid medium is equated with the isopropyl alcohol concentration of dispersion liquid (B).
(2) reflectivity:
Use the system spectrophotometer UV-3150 of Shimadzu Seisakusho Ltd., measure the relative normal reflection intensity of 5 ° of incident angles.During mensuration, paste black belt at the film inner face.
(3) transmitance:
Use the system spectrophotometer UV-3150 of Shimadzu Seisakusho Ltd., measure whole light penetrations.
[embodiment 1]
Mix the system silica gel ST-XL of 25.00g daily output chemical company (the mean grain size 40～60nm that utilizes the BET method to measure, solid component concentration: 40 weight %; Liquid medium: water) as inorganic particles (C), the system silica gel ST-XS of 12.50g daily output chemical company (mean grain size 4～6nm, solid component concentration: 20 weight %; Liquid medium:, obtain dispersion liquid (A) water) as inorganic particles (D), 100.00g pure water.In this dispersion liquid (A), add the 112.50g isopropyl alcohol as polycoagulant, mix, obtain coagulation liquid (B).This coagulation liquid (B) consist of inorganic particles 12.5g, water 125g, isopropyl alcohol 112.5g, the relative inorganic particles of weight (C) of inorganic particles (C) is 80% with the ratio of the general assembly (TW) of inorganic particles (D), the weight rate of inorganic particles (D) is 20%.In addition, to by dilute the formulated sample of dispersion liquid (A) (A ') with pure water, utilize the laser diffraction and scattering method to measure mean grain size, top Ra is 0.08 μ m as a result, D
90Be 0.10 μ m.To passing through water: the formulated sample of the mixed solvent of isopropyl alcohol=125: 112.5 (weight ratio) dilution coagulation liquid (B) (B '), utilize the laser diffraction and scattering method to measure mean grain size, as seen the result shows the peak Rb of summit near 86 μ m.In this sample (B '), the flocculated particle volume of the particle diameter more than 100 times of expression Ra is 85.2%.
Use the scraper coating machine, coating this coagulation liquid (B) on triacetylcellulose film, dry under 60 ℃, form antireflection film.The minimum reflectance of the antireflection film that obtains in the visible region is 0.5%, and maximum transmission is 96.0%, and antireflection property is outstanding.In addition, the thickness from the antireflection film of measuring reflectance results presumption is 110nm.
[embodiment 2]
Mix the system chain silica gel PS-M of 62.50g daily output chemical company and (utilize the mean grain size 111nm of dynamic light scattering determination, solid component concentration: 20 weight %; Liquid medium: water) and the system chain silica gel PS-S of 6.25g daily output chemical company (utilize the mean grain size 106nm of dynamic light scattering determination, solid component concentration: 20 weight %; Liquid medium: water) as chain inorganic particles (E), the system silica gel ST-XS of 25.00g daily output chemical company (mean grain size 4～6nm, solid component concentration: 20 weight %; Liquid medium:, obtain dispersion liquid (A) water) as inorganic particles (F), 81.25g pure water.In this dispersion liquid (A), add the 75.00g isopropyl alcohol as polycoagulant, mix, obtain coagulation liquid (B).This coagulation liquid (B) consist of inorganic particles 18.75g, water 156.25g, isopropyl alcohol 75g, the relative chain inorganic particles of the weight of chain inorganic particles (E) (E) is 73% with the ratio of the general assembly (TW) of inorganic particles (F), and the weight rate of inorganic particles (F) is 27%.In addition, to by dilute the formulated sample of dispersion liquid (A) (A ') with pure water, utilize the laser diffraction and scattering method to measure mean grain size, top Ra is 0.12 μ m as a result, D
90Be 0.15 μ m.To passing through water: the formulated sample of the mixed solvent of isopropyl alcohol=156: 25.75 (weight ratio) dilution coagulation liquid (B) (B '), utilize the laser diffraction and scattering method to measure mean grain size, as seen the result shows the peak Rb of summit near 77 μ m.In this sample (B '), the flocculated particle volume of the particle diameter more than 100 times of expression Ra is 90.1%.
Use the scraper coating machine, coating this coagulation liquid (B) on triacetylcellulose film, dry under 60 ℃, form antireflection film.The minimum reflectance of the antireflection film that obtains in the visible region is 0.1%, and maximum transmission is 95.8%, and antireflection property is outstanding.In addition, the thickness from the antireflection film of measuring reflectance results presumption is 120nm.
[comparative example 1]
Mixing 25.00g silica gel ST-XL as inorganic particles (D), 212.50g pure water, obtains the solid constituent containing ratio dispersion liquid (A) identical with the solid constituent containing ratio of the coagulation liquid (B) of embodiment 1 as inorganic particles (C), 12.50g silica gel ST-XS.The relative inorganic particles of weight (C) of inorganic particles (C) is 80% with the ratio of the general assembly (TW) of inorganic particles (D), and the weight rate of inorganic particles (D) is 20%.Use the scraper coating machine, coating this coagulation liquid (A) on triacetylcellulose film, dry under 60 ℃, form antireflection film.The minimum reflectance of the antireflection film that obtains in the visible region is 1.6%, and maximum transmission is 93.7%, and antireflection property is poor.In addition, the thickness from the antireflection film of measuring reflectance results presumption is 110nm.
[comparative example 2]
Mixing 62.50g chain silica gel PS-M and 6.25g and 12.50g chain silica gel PS-S as inorganic particles (F), 156.25g pure water, obtain the solid constituent containing ratio dispersion liquid (A) identical with the solid constituent containing ratio of the coagulation liquid (B) of embodiment 2 as chain inorganic particles (E), 25.00g silica gel ST-XS.The relative chain inorganic particles of the weight of chain inorganic particles (E) (E) is 73% with the ratio of the general assembly (TW) of inorganic particles (F), and the weight rate of inorganic particles (F) is 27%.Use the scraper coating machine, coating this coagulation liquid (A) on triacetylcellulose film, dry under 60 ℃, form antireflection film.The minimum reflectance of the antireflection film that obtains in the visible region is 0.8%, and maximum transmission is 94.6%, and antireflection property is poor.In addition, the thickness from the antireflection film of measuring reflectance results presumption is 70nm.
Claims (11)
1. the manufacture method of a duplexer, it is in the folded manufacture method that the duplexer that the film that is made of inorganic particles forms is arranged of layers on substrates, wherein, comprises following operation (1)～(3):
Operation (1) is added polycoagulant in its dispersion liquid to the inorganic particles that contains liquid medium and disperse (A) in this liquid medium, thereby obtain the coagulation liquid (B) of at least a portion cohesion of the inorganic particles that contains in the described dispersion liquid (A);
Operation (2), it applies described coagulation liquid (B) on base material; With
Operation (3), it forms the film that is made of described inorganic particles by remove liquid medium from the coagulation liquid (B) of coating on described base material;
Described dispersion liquid (A) satisfies following necessary condition (A1), and coagulation liquid (B) satisfies following necessary condition (B1),
Necessary condition (A1): in the size distribution figure that utilizes laser diffraction and scattering method mensuration dispersion liquid (A) to obtain, the particle diameter that top Ra represents is in the scope of 0.01～1 μ m, and, has D utilizing the laser diffraction and scattering method to measure among the cumulative particle size distribution figure that this dispersion liquid obtains
90Following size particles accumulation number is 90% particle diameter D of whole granule numbers
90Be below the 1 μ m,
Necessary condition (B1): in the size distribution figure that utilizes laser diffraction and scattering method mensuration coagulation liquid (B) to obtain, have the peak Rb of the particle diameter more than 20 times of the particle diameter shown in the described top Ra of expression.
2. method according to claim 1, wherein,
The mean grain size Da of the inorganic particles that contains in the described dispersion liquid (A) is in the scope of 1～300nm.
3. method according to claim 1, wherein,
The inorganic particles that contains in the described dispersion liquid (A) is a potpourri as described below: the potpourri of the inorganic particles (D) of mean grain size in 1～20nm scope of the inorganic particles (C) of the mean grain size of 55～90 weight % in 30～300nm scope and 10～45 weight %, wherein, inorganic particles (C) is 100 weight % with the total amount of inorganic particles (D).
4. according to claim 2 or 3 described methods, wherein,
In described coagulation liquid (B), particle diameter is more than 1% of cumulative volume that the volume of the flocculated particle more than 20 times of the particle diameter shown in the described top Ra adds up to the inorganic particles in this coagulation liquid (B).
5. method according to claim 1, wherein,
The inorganic particles that contains in the described dispersion liquid (A) is chain inorganic particles (E).
6. method according to claim 1, wherein,
The inorganic particles that contains in the described dispersion liquid (A) is a potpourri as described below: the potpourri of the chain inorganic particles (E) of 55～90 weight % and the inorganic particles (F) of the mean grain size of 10～45 weight % in 1～20nm scope, wherein, inorganic particles (E) is 100 weight % with the total amount of inorganic particles (F).
7. according to claim 5 or 6 described methods, wherein,
In described coagulation liquid (B), particle diameter is more than 5% of cumulative volume that the volume of the flocculated particle more than 20 times of the particle diameter shown in the described top Ra adds up to the inorganic particles in this coagulation liquid (B).
8. method according to claim 1, wherein,
Described dispersion liquid (A) is a hydrophilic colloid.
9. method according to claim 1, wherein,
Described dispersion liquid (A) is a silica gel.
10. according to Claim 8 or 9 described methods, wherein,
Described polycoagulant is a dewatering agent.
11. method according to claim 10, wherein,
Described dewatering agent is an alcohol.
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| JP6758809B2 (en) * | 2015-09-29 | 2020-09-23 | 日東電工株式会社 | A method for producing a porous gel-containing liquid, a method for producing a porous gel-containing liquid, a method for producing a high void layer, a method for producing a high porosity porous body, and a method for producing a laminated film roll. |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4792490A (en) * | 1986-04-08 | 1988-12-20 | Kanegafuchi Kagaku Kogyo Kabushiki Kaisha | Compacted agglomerates of polymer latex particles |
| CN1550537A (en) * | 2003-05-09 | 2004-12-01 | ��Ħ��ѧ��ҵ��ʽ���� | Abrasive slurry having high dispersion stability and manufacturing method for a substrate |
| CN1648692A (en) * | 2004-01-19 | 2005-08-03 | 力特光电科技股份有限公司 | Method for producing surface optical layer |
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| JP3948049B2 (en) * | 1997-03-31 | 2007-07-25 | 王子製紙株式会社 | Method for producing ink jet recording material |
| JP2000157914A (en) | 1998-11-30 | 2000-06-13 | Toppan Printing Co Ltd | Coating method and device therefor |
| JP2003096211A (en) | 2001-09-25 | 2003-04-03 | Konica Corp | Sheet-like material and its manufacturing method |
| TW200535517A (en) * | 2003-12-26 | 2005-11-01 | Zeon Corp | Polarizing plate protective film, polarizing plate with reflection preventing function and optical product |
| KR101114932B1 (en) * | 2004-06-10 | 2012-03-06 | 코오롱인더스트리 주식회사 | Hardcoating film |
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|---|---|---|---|---|
| US4792490A (en) * | 1986-04-08 | 1988-12-20 | Kanegafuchi Kagaku Kogyo Kabushiki Kaisha | Compacted agglomerates of polymer latex particles |
| CN1550537A (en) * | 2003-05-09 | 2004-12-01 | ��Ħ��ѧ��ҵ��ʽ���� | Abrasive slurry having high dispersion stability and manufacturing method for a substrate |
| CN1648692A (en) * | 2004-01-19 | 2005-08-03 | 力特光电科技股份有限公司 | Method for producing surface optical layer |
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| CN101042438A (en) | 2007-09-26 |
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| KR101291455B1 (en) | 2013-07-30 |
| KR20070096828A (en) | 2007-10-02 |
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