KR101656461B1 - Reflection film based on silver nano layer produced by wet coating and production method thereby - Google Patents
Reflection film based on silver nano layer produced by wet coating and production method thereby Download PDFInfo
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- KR101656461B1 KR101656461B1 KR1020150094688A KR20150094688A KR101656461B1 KR 101656461 B1 KR101656461 B1 KR 101656461B1 KR 1020150094688 A KR1020150094688 A KR 1020150094688A KR 20150094688 A KR20150094688 A KR 20150094688A KR 101656461 B1 KR101656461 B1 KR 101656461B1
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/08—Mirrors
- G02B5/0816—Multilayer mirrors, i.e. having two or more reflecting layers
- G02B5/085—Multilayer mirrors, i.e. having two or more reflecting layers at least one of the reflecting layers comprising metal
- G02B5/0858—Multilayer mirrors, i.e. having two or more reflecting layers at least one of the reflecting layers comprising metal the reflecting layers comprising a single metallic layer with one or more dielectric layers
- G02B5/0866—Multilayer mirrors, i.e. having two or more reflecting layers at least one of the reflecting layers comprising metal the reflecting layers comprising a single metallic layer with one or more dielectric layers incorporating one or more organic, e.g. polymeric layers
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- G02B1/105—
Abstract
Description
BACKGROUND OF THE
Silver has a higher light reflectance in the entire visible light region than any known material. The high reflection properties of silver have long been applied to the manufacture of mirrors through silver halide reactions. In recent years, there has been a growing demand for high reflectivity and electrical and electronic products, Are being developed.
As a method of applying a silver thin film on the surface of any substrate, there are a plating method other than a silver halide reaction, which is a chemical reduction method, and a sputtering deposition method. The double plating method is widely used for exterior use such as surface treatment of ornaments, but it is gradually getting out of the market due to the fundamental environmental problem of plating method, limitation of kinds of plating base materials, productivity problems, and the deposition method is curved and various appearance It is difficult to uniformly coat a silver thin film on the substrate surface and the equipment cost is very high. Especially, in case of a large product, the operation is impossible due to the limit of the size of the evaporator chamber.
Reflective film is a necessary component in the backlight unit of the liquid crystal display device, and so-called white PET is mainly used for a display of a size over a notebook. However, white PET should be manufactured to a certain thickness or more in order to exhibit an appropriate reflectance. Therefore, white PET can not be used for mobile devices that require light and thin characteristics, especially smart phones. Most of the smartphones currently manufactured use 3M's retroreflective film (ESR). Retroreflective films exhibit reflectivities of up to 99% in reflection characteristics, but are sold at a high price due to difficulties in manufacture and monopoly, and there is reliability problem under high temperature and high humidity. Therefore, The silver reflective film using the high reflection characteristic of silver recently began to be partially used as a reflective film for BLU.
The currently commercialized silver reflective film is manufactured by depositing silver on the surface of PET, which is a substrate, and sputtering deposition is mainly used as a physical vapor deposition method. However, silver deposition requires expensive equipments and the productivity is not high. Therefore, the price of manufactured reflective film can not be lowered significantly compared with the conventional 3M retroreflective method. Recently, there have been some attempts to fabricate silver deposited films by wet coating rather than by vapor deposition. In Korean Patent No. 0861146, one of polyurethane, epoxy or modified acrylic paint is selected on the surface of PET film, and a pre-treatment film is coated on the surface of the PET film, and a fine uneven surface is formed thereon by corona discharge, , And a technique of coating one of the same resins as the pretreatment film to prevent discoloration of silver is proposed. This patent does not mention the catalyst in the silver halide reaction and does not mention the rate of silver film formation or the rate of silver reflective film production. The silver halide reaction is difficult to achieve the productivity of silver film formation sufficient for the roll-to-roll process without the catalyst, and the progress of the reaction is not easy to occur at room temperature. In addition, the silver film thickness of 20 to 60 nm suggested in the above patent is insufficient to reflect all the visible light as the thickness of light transmission. That is, there is a high possibility that a part of light, particularly light of a short wavelength, is transmitted to lower the final reflectance. In the above patent, there is no specific expression as patent technology for silver halide reaction. Also, the organic resin used as a protective coating film is a great factor for lowering the reflectance.
One of the fundamental problems with silver reflective films is the difference in the reflectance of silver by wavelength. Silver is the metal with the highest average reflectance in the entire region of visible light, but reflectance differs by wavelength. Silver has a high reflectance in a high wavelength region in a visible light and a low reflectance in a relatively short wavelength region. The reason why a silver wire made by a silver halide reaction gives a soft and warm feeling is due to a difference in reflectance of silver do. In order to use the silver reflection film as a reflection film of a liquid crystal display device backlight unit, the reflectance must be corrected for each wavelength band. Otherwise, the color coordinate of the light source may be distorted.
It is an object of the present invention to provide a silver reflective film manufactured by a wet coating method which can replace the conventional 3M retroreflective film or silver evaporated reflection film and a method of manufacturing the same.
More specifically, in the production of a silver reflection film by a wet method or a roll-to-roll method, correction of a short wavelength region and transmission of light are eliminated, and the interfacial adhesion with the silver layer of the film substrate is maximized , A protective coating layer for preventing discoloration of silver after silver layer formation by maximizing silver layer formation speed and silver layer thickness and introducing a protective coating layer having a final average reflectance of 97% or more and having a uniform reflectance in the visible light propagation region, Film production technology and a silver reflection film manufactured using the same.
In order to accomplish the above object, the present invention provides a method for manufacturing a silver reflection film by a wet process or a roll-to-roll process, comprising the steps of: preparing a polyethylene terephthalate (PET) film, , A polycarbonate (PC), a polyacrylate, or a white PET is used. The primer layer to be treated on the surface of the film substrate is composed of a resin layer containing silica nanoparticles, A protective coating layer for preventing discoloration of silver after silver layer formation is coated with an inorganic material of silica system to maximize the adhesion and maximize the silver layer formation speed and the silver layer thickness by using a metal salt as a catalyst layer, Wet materials with a uniform reflectance of more than 97% and visible light transmission range, To provide a silver reflective film.
More specifically, the present invention relates to a film substrate selected from the group consisting of polyethylene terephthalate (PET), polycarbonate (PC), polyacrylate or white PET on which aluminum is deposited on the backside; A primer layer composed of a resin containing nanoparticles formed on the film substrate; A catalyst layer formed on the primer layer; A silver layer formed on the catalyst layer; And a protective coating layer formed on the silver layer.
The nanoparticles may be silica nanoparticles, and the primer layer may be composed of a thermosetting resin, a UV curable resin, or a mixed resin thereof.
The catalyst layer may include a metal salt containing tin, aluminum, or an iron ion, or a mixed metal salt thereof, and the protective coating layer may be a silica-based inorganic layer.
The method for manufacturing a silver reflection film according to the present invention is a method for manufacturing a silver reflection film comprising a film for preparing a film substrate selected from the group consisting of polyethylene terephthalate (PET), polycarbonate (PC), polyacrylate, A substrate preparation step; A primer layer forming step of forming a primer layer with a resin containing nanoparticles on the film substrate; A catalyst layer forming step of forming a catalyst layer on the primer layer; A silver layer forming step of forming a silver layer on the catalyst layer by a wet coating method; And a protective coating layer forming step of forming a protective coating layer on the silver layer.
The nanoparticles may be silica nanoparticles and the primer layer forming step may be to apply thermosetting, UV curable resins containing nanoparticles, or mixed resins thereof.
The catalyst layer forming step may be an application of an aqueous solution containing a metal salt containing tin, aluminum, or an iron ion, or a mixed metal salt thereof, and the silver layer forming step may be performed by a spinning solution containing silver nitrate and ammonia water; And a reducing liquid may be wet-coated. The wet coating may be a spray coating or a dual slit coating.
The protective coating layer may be formed by wet coating a protective coating solution containing silica sol.
The present invention relates to a silver reflection film which can be used in a backlight unit for a liquid crystal display, and which can be applied by spraying or roll-to-roll wet coating Which is superior in cost, productivity and environment friendliness compared to the plating method, has the advantages of high productivity as compared with vapor deposition, and low defectiveness.
In addition, the present invention solves the problem of non-uniformity in reflectance between the silver reflection film constituting layers required for optical films for electronic products, durability, resistance to discoloration inherent to silver, and non-uniformity of reflectance by visible light wavelength, The reflective film manufactured according to the present invention exhibits a high reflectance enough to be used for an LCD backlight unit (BLU), and has a constant reflectance for each wavelength Reflectance.
Further, the silver reflection film according to the present invention has a reflectance of 97% or more in the visible light propagation region and has no discoloration, so that it can be used as a reflective film for a liquid crystal display device having excellent durability.
1 is a cross-sectional view of a silver reflection film according to an embodiment of the present invention.
2 is a process diagram showing a manufacturing process of a silver reflection film according to an embodiment of the present invention.
Hereinafter, the present invention will be described in detail.
The present invention relates to a process for producing a silica nanoparticle having a structure in which silica nanoparticles are formed on the surface of polyethylene terephthalate (PET), polycarbonate (PC), polyacrylate film (30 to 75 μm thick) or white PET (thickness 50 μm or less) A primer layer formed by coating with an added urethane thermosetting resin; A catalyst layer treated with a metal salt on a primer layer; A silver layer (50-100 nm) formed on the catalyst layer; And a protective coating layer mainly composed of silica sol on the silver layer. Fig. 1 shows the structure of such a silver reflection film.
The silver layer formed by the general silver reaction does not exceed the thickness of 50 to 60 nm. This means that the silver layer can not reflect all the light but some part is transmitted. Therefore, it is preferable that the thickness of the silver layer is made 70 nm or more in the production of the silver reflection film so that only the minimum light is transmitted. Also, due to the inherent characteristics of silver, the reflectance of a short wavelength is higher than that of a long wavelength. Aluminum, on the other hand, reflects light of shorter wavelengths rather than longer wavelengths in the visible light region. This reflection characteristic of aluminum can be usefully applied to a product having a uniform reflectance in the entire visible region by correcting the relatively low reflectance of short wavelength of silver. Also, since the thickness of the film formed instantaneously by the chemical reduction as in the present invention is insufficient to completely block transmission of light, the aluminum layer also helps prevent some light transmission. For the above reasons, it is preferable to use a film in which the back surface is deposited with aluminum. In this case, the thickness of the film is preferably 30 to 100 nm, more preferably 30 to 70 nm, and the thickness of the aluminum film is 1 To 100 nm, more preferably 20 to 50 nm.
On the other hand, white PET may be used instead of an aluminum-deposited PET film used as a film substrate. White PET is a reflective film used in products with a relatively large surface area. Since fine bubble particles are dispersed in the internal matrix of the film, the light is scattered and reflected, and the average reflectance is insufficient for a retroreflective film or a silver reflective film. , The reflectance is 94% or more at the entire wavelength range of visible light. Therefore, it shows better characteristics than transparent PET in shielding the transmittance of a part of light which is insufficient only by the silver layer or improving the reflectance at a short wavelength.
The surface of the PET or white PET film as the film substrate is coated with a polar primer to enhance the adhesion between the silver layer and the film interface. The primer is preferably urethane or acrylic, and in the present invention, silica nanoparticles are added to the primer layer in order to maximize adhesion. In general, the polar group enhances the interfacial adhesion, and the silica nanoparticles contain a large amount of OH groups, thereby enhancing the adhesion between the primer layer and the silver layer. The content of the silica particles is preferably 10 to 70 wt%, more preferably 20 to 40 wt%, of the total weight of the primer. The primer is either UV-curable or thermosetting, whichever is relevant, but a UV-curable type is more preferable for improving the reflectance and a thermosetting type is more preferable for improving the adhesion. In order to take advantage of two advantages, UV curing type and thermosetting type resin can be mixed and used. When the thickness of the primer layer is 0.1 to 10 μm, there is no problem in showing the characteristics, and preferably 1 to 5 μm is preferable.
The silver acceptance reaction is a kind of plating reaction by a precipitation mechanism by oxidation and reduction. In the original silver acceptance reaction, it is necessary to heat to start and proceed the reaction. However, in the present invention, The catalyst is used. The surface of the primer treated film was sprayed with a catalyst aqueous solution composed of a metal salt or a mixture of two or more kinds of metal salts to catalyze the surface of the primer, thereby increasing the rate of silver halide reaction and enabling reaction at low temperature. The metal salts used as catalysts in this reaction were Fe-based, Al-based. Zn system. The metal salt is dissolved in water and applied to the surface of the substrate. If the wettability is poor according to the base, it is preferable to add a small amount of surfactant.
A silver film is formed by spraying a silver liquor and a reducing solution simultaneously on the surface of the film constituted of the catalyst layer. Silver juice contains a silver ion containing salt such as silver nitrate and a certain amount of ammonia water. The reducing solution may be variously used as the main component of formaldehyde, acetaldehyde, sodium (Na + ) or potassium (K + ) organic salts, and amine compounds as long as they can reduce silver. For example, NaOH, KOH, reducing sugar, etc. can be used. Depending on the concentration and kind, the rate of precipitation and the purity of silver are different.
Silver has the advantage of showing high gloss and high reflection characteristics and good appearance, but it has the biggest weak point that it is easily discolored by contact with various active gases in oxidation or air. To prevent discoloration after plating, some large-scale plating solution manufacturers sell so-called anti-discoloring liquids. However, most such products require that the silver product be immersed for more than a few minutes, and that does not guarantee sufficient discoloration.
The prevention of the discoloration of the silver surface can be achieved by applying a transparent thermosetting or UV curable resin to seal the surface, as in Korean Patent No. 0861146, which is a patent cited above. However, sealing the surface with an organic resin should be treated to a certain thickness or more, generally 5 to 10 μm or more. In this case, the protective coating layer can lower the reflectance of the reflective film, and further, the protective coating layer itself promotes the discoloration of silver . In addition, the sealing of the silver surface with the organic resin usually causes curling of the film, and if it is applied too thinly to prevent curling, the substances that cause discoloration of the silver, such as oxygen or sulfur dioxide, And eventually discoloration occurs. In the present invention, the surface is treated with an inorganic coating liquid having a sufficient seal even at a thin coating thickness, so that silver does not discolor even when subjected to external exposure for a long time.
Hereinafter, the present invention will be described in more detail by way of examples. However, the present invention is not limited by the following examples and comparative examples.
Example 1: Preparation of silver reflection film and physical property analysis (based on aluminum-deposited PET film)
A 75 μm thick PET film with aluminum backing was sprayed with a 1% solution of dodecyl benzene sulfonic acid (sodium salt) to remove surface contaminants and then sprayed with distilled water to remove residual surfactant. Most of the surface water was removed with a high-pressure air gun. After passing through the drying furnace, moisture of the surface was completely removed. Then, an acrylic thermosetting / UV curing type mixed binder solution containing 30% of silica sol was sprayed. The PET film coated with the resin was dried to remove the solvent, passed through a heating chamber at 80 ° C, and heated at 700 mJ / sec. It was completely cured by passing through a UV chamber of light quantity. The thickness of the formed primer layer was 3.0 占 퐉. The surface of the PET film coated with the primer was immersed in a solution containing 1% surfactant and alum [KAl (SO 4 ) 2 .12H 2 O] at a concentration of 10% The mixture was sprayed with distilled water to wash away excess salts. On the surface of the washed film, a silver stock solution containing silver nitrate and ammonia water as main components and a reducing solution containing acetaldehyde (CH 3 CHO) and sodium hydroxide (NaOH) as main components were simultaneously sprayed on the surface. The working temperature at the formation of the silver film was 28 ° C and the spraying time of the silver liquid and the reducing liquid was 10 seconds. After the silver film formation was completed, the reaction byproducts remaining on the silver film and the excess reaction solution were sprayed with purified water, washed thoroughly, dried by hot air at 70 ° C, spray-coated with a protective coating solution mainly composed of silica sol, and dried and cured at 80 ° C.
The reflectance of the obtained silver reflective film was almost uniformly 96% on the visible light range of 350 to 900 nm. The thickness of the silver layer observed by the electron microscope was 70 nm and the thickness of the top coat for sealing was Was about 200 nm. A cross-cut test was performed by drawing a line of 10 lines each at 2 mm intervals. In order to evaluate the surface sealability to prevent discoloration of silver, it was sprayed every hour with a 10% aqueous saline solution for 24 hours in a salt water spray test, and there was no discoloration.
Example 2: Preparation of silver reflection film and physical property analysis (white PET film base)
The procedure of Example 1 was the same as that of Example 1 except that white PET (50 μm in thickness) was used instead of an aluminum evaporated film, and the surface was treated with a plasma to improve adhesion during primer coating. The adhesiveness, reflectance and sealability of the obtained silver reflection film were similar to those of Example 1, with no significant difference.
Comparative Example 1: Preparation of silver reflection film and physical property analysis (transparent PET film base)
Example 1 and the entire process are the same, but transparent PET (50 μm) for optical use is used as a base film instead of an aluminum evaporated film. The reflectance was 98%, 97%, 95% and 92% at the wavelengths of 750 nm, 650 nm, 550 nm and 450 nm, respectively, and the reflectance in the short wavelength region was remarkably low. On the other hand, the transmittance was relatively high in the short wavelength region of 1%, 1%, 2% and 5% at the wavelengths of 750 nm, 650 nm, 550 nm and 450 nm, respectively.
Comparative Example 2: Preparation of silver reflection film and physical property analysis (using silica particle-free primer)
The procedure of Example 1 was the same as that of Example 1, except that no silica sol was added to the primer. The obtained silver reflection film showed similar results to those of Example 1 in reflectance and sealability, but was remarkably decreased in adhesion. That is, in the cross-cut test, 29 grids of about 30% were detached.
Comparative Example 3: Preparation of silver reflection film and physical property analysis (silver reflection film without catalyst layer formation)
Example 1 and the entire process were performed in the same manner. However, the catalyst layer formation spraying and cleaning process before the silver film formation spray process were omitted, and the silver film formation rate was relatively slow as compared with Example 1, Respectively. The reflectance of the obtained silver reflective film was 95% on average, and 10 pieces of 100 2 mm x 2 mm pieces fell in the cross-cut test. In the salt spray test, results similar to those of Example 1 were obtained.
Comparative Example 4: Preparation of silver reflection film and physical property analysis (Silver surface sealing with UV curing type urethane resin)
Until the formation of the silver layer, the same as in Example 1, but a UV curing type urethane resin was used for sealing coating for preventing discoloration. The thickness of the topcoat was 2.5 탆. As a result of the saline spray test under the same conditions as in Example 1, it was discolored to yellow as a result of yellow spraying, and was unsatisfactory compared with the sealing performance of silica sol.
INDUSTRIAL APPLICABILITY As can be seen from the above Examples and Comparative Examples, the present invention is excellent in the interlayer adhesion of the silver reflection film, the uniformity of reflectance by wavelength band, the sealing performance of silver top coat for preventing discoloration, Reflecting film to meet the requirements of the film.
That is, in the present invention, aluminum-deposited PET or white PET is used as a film substrate for light transmission and for improving the reflectance of a short wavelength band; Silica nanoparticles added to the primer layer for ease of adhesion and silver film formation; Formation of a metal salt catalyst layer on the surface of the layer for improving the silver film formation rate and increasing the adhesion between silver-primer interfaces; Introduction of a protective coating layer which is a top coat of an inorganic silica sol solution for securing the sealing property.
If any one of these elements is excluded, the final properties of the silver reflective film are degraded. In Examples 1 and 2 and Comparative Example 1, it is preferable to use aluminum-deposited PET or white PET as a substrate for improving the reflectance in a short wavelength region. In Comparative Example 2, a silver reflection film was prepared by using a primer not containing silica particles, but the interfacial adhesion between the silver layer and the primer layer was remarkably decreased. It is interpreted that the hydroxyl group (OH) group contained in the silica nanoparticles not only increases the chemical bonding force with silver but also improves the roughness of the surface, thereby improving the adhesion of the silver-PET interface. In Comparative Example 3, a silver film was formed without forming a catalyst layer with a metal salt. At this time, a decrease in silver film formation rate was remarkably observed. It can be interpreted that the metal ions in the catalyst layer contribute to the formation of silver seed particles at the initial stage of silver film formation, thereby improving the silver film formation rate. Finally, in Comparative Example 4, it is confirmed that the silica-based coating, which is an inorganic material, is superior in sealing property and reflectance than that coated with an organic resin as a sealing top coating material for preventing silver discoloration. From this, it can be said that the coating of the inorganic material applied in the present invention forms a dense coating film with fewer pinholes, less variation in thickness, and the like compared with the organic coating layer generally used.
1: Film substrate
2: Primer layer
3: catalyst layer
4: silver layer
5: Protective coating layer
Claims (12)
A primer layer composed of a resin containing nanoparticles formed on the film substrate;
A catalyst layer formed on the primer layer;
A silver layer formed on the catalyst layer; And
And a protective coating layer formed on the silver layer.
Wherein the nanoparticles are silica nanoparticles.
Wherein the primer layer is composed of a thermosetting resin, a UV curable resin, or a mixed resin thereof.
Wherein the catalyst layer comprises a metal salt containing tin, aluminum, or an iron ion, or a mixed metal salt thereof.
Wherein the protective coating layer is a silica-based inorganic layer.
A primer layer forming step of forming a primer layer with a resin containing nanoparticles on the film substrate;
A catalyst layer forming step of forming a catalyst layer on the primer layer;
A silver layer forming step of forming a silver layer on the catalyst layer by a wet coating method; And
And forming a protective coating layer on the silver layer. ≪ RTI ID = 0.0 > 21. < / RTI >
Wherein the nanoparticles are silica nanoparticles.
Wherein the primer layer forming step comprises applying a thermosetting, UV curable resin containing nanoparticles, or a mixed resin thereof.
Wherein the catalyst layer forming step comprises applying an aqueous solution containing tin, aluminum, or a metal salt containing iron ions or a mixed metal salt thereof.
Wherein the silver layer forming step is a wet coating method in which a reducing solution is wet-coated on a surface of a silver nitrate solution and ammonia water.
Wherein the wet coating is a spray coating or a dual slit coating.
Wherein the protective coating layer forming step is a wet coating method of a protective coating solution containing silica sol.
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Cited By (2)
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| US20180164486A1 (en) * | 2016-12-12 | 2018-06-14 | Kolon Glotech, Inc. | Surface lighting apparatus and method for manufacturing the same |
| CN114214600A (en) * | 2021-12-17 | 2022-03-22 | 东莞市光志光电有限公司 | Preparation method of antioxidant PET silver film |
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| JP2005338625A (en) * | 2004-05-28 | 2005-12-08 | Kitagawa Ind Co Ltd | Visible ray reflection film |
| KR20080051311A (en) * | 2006-12-05 | 2008-06-11 | (주)한누리 | Silver reflection film and method for making the same |
| JP2008304795A (en) * | 2007-06-08 | 2008-12-18 | Toyo Kohan Co Ltd | Light reflection plate, its manufacturing method, and light reflection device |
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| JP2004085874A (en) * | 2002-08-27 | 2004-03-18 | Nitto Denko Corp | Reflecting plate and reflective polarizing plate |
| JP2005338625A (en) * | 2004-05-28 | 2005-12-08 | Kitagawa Ind Co Ltd | Visible ray reflection film |
| KR20080051311A (en) * | 2006-12-05 | 2008-06-11 | (주)한누리 | Silver reflection film and method for making the same |
| KR100861146B1 (en) | 2006-12-05 | 2008-09-30 | (주)한누리 | Silver reflection film and method for making the same |
| JP2008304795A (en) * | 2007-06-08 | 2008-12-18 | Toyo Kohan Co Ltd | Light reflection plate, its manufacturing method, and light reflection device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20180164486A1 (en) * | 2016-12-12 | 2018-06-14 | Kolon Glotech, Inc. | Surface lighting apparatus and method for manufacturing the same |
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| US10557981B2 (en) | 2016-12-12 | 2020-02-11 | Kolon Glotech, Inc. | Surface lighting apparatus and method for manufacturing the same |
| CN114214600A (en) * | 2021-12-17 | 2022-03-22 | 东莞市光志光电有限公司 | Preparation method of antioxidant PET silver film |
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