CN108152871B - Silver-plated reflecting film - Google Patents
Silver-plated reflecting film Download PDFInfo
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- CN108152871B CN108152871B CN201711298181.0A CN201711298181A CN108152871B CN 108152871 B CN108152871 B CN 108152871B CN 201711298181 A CN201711298181 A CN 201711298181A CN 108152871 B CN108152871 B CN 108152871B
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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
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- G—PHYSICS
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- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
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Abstract
The invention relates to a silver-plated reflecting film, which structurally comprises a high-refractive-index resin layer, a barrier layer, a base film layer, a silver reflecting film layer, a corrosion-resistant glue layer and a reinforced reflecting layer which are sequentially arranged. The silver-plated reflecting film takes the base film surface as a reflecting surface, and the reflecting surface is added with the high-refractive-index resin layer and the barrier layer to further improve the reflectivity and the corrosion resistance of the reflecting film. Meanwhile, the enhanced reflecting layer is compounded on the surface of the silver reflecting film layer, and a corrosion inhibitor which is easy to complex with silver is added into the adhesive to form a corrosion-resistant adhesive layer, so that the corrosion resistance of the surface of the silver layer to water, oxygen, halide and sulfur-containing gas can be effectively protected, and the service life and the overall performance of the silver-plated reflecting film are obviously improved. The silver-plated reflecting film disclosed by the invention is excellent in weather resistance, long in service life, high in reflectivity, excellent in scratch resistance and strong in silver layer adhesion.
Description
The technical field is as follows:
the invention relates to the technical field of thin films, in particular to a silver-plated reflecting film.
Background art:
LCDs are non-emissive display devices, and display functions must be achieved by using a backlight, and high-performance backlight technology must be used in conjunction with the demand for slimness, miniaturization, and low power consumption of LCDs for mobile phones, notebook computers, and the like. The reflecting film in the backlight component is mainly used for improving the reflectivity of the optical surface and reflecting the light leaked out of the bottom of the light guide plate with high efficiency and no loss, thereby reducing the light loss, reducing the power consumption and improving the light saturation of the liquid crystal display surface. The silver-plated reflective film has the advantages of high reflectivity, thin thickness and the like, and is widely used for portable equipment such as mobile phones and tablet computers at present. However, the silver metal is unstable and reacts with water, oxygen, halide, sulfide and the like in the environment, so that the reflectivity is obviously reduced, and the whole display effect is influenced.
JP09-111442A proposes coating a high polymer film as an anti-corrosion layer on top of a silver film, and then laminating a high polymer film as a protective layer. However, the barrier capability of the base film serving as a support is limited, so that water and oxygen permeation from the surface of the base film layer also causes corrosion of the silver layer, which affects the service life of the reflective film.
JP2000-241612 proposes to deposit an inorganic protective layer such as an aluminum oxide layer, a titanium oxide layer, and a silicon oxide layer on a silver film in sequence, and this silver-plated reflective film with a multilayer structure has a certain weather resistance, but the manufacturing process is complicated, the cost is high, and when the matching between the inorganic materials is not good, the interlayer peeling phenomenon is likely to occur, and the element migration between the deposited layers is likely to occur, so that the surface fogging is likely to affect the reflectivity of the reflective film.
In US4645714A, it is proposed that a corrosion inhibitor is added to a transparent acrylic resin and then coated on the surface of a silver layer, which has a certain effect on improving the weather resistance of the silver layer, but a dense hydrophobic layer formed by the corrosion inhibitor and the silver layer has a certain effect on reducing the reflectivity of the silver layer, and particularly, the reflectivity is significantly reduced in a high-temperature and humid environment.
In conclusion, silver-plated reflective films with high reflectivity, long service life and excellent corrosion resistance are still the goal pursued in the industry.
The invention content is as follows:
aiming at the problems, the invention provides a silver-plated reflecting film with a novel structure, and the reflectivity of the silver-plated reflecting film is more than or equal to 99% by introducing a high-refractive-index resin layer and a reinforced reflecting layer; the silver-plated reflecting film has more excellent corrosion effects of resisting water vapor, oxygen, halide and sulfur-containing gas on the silver-plated layer by introducing the barrier layer and the corrosion-resistant glue layer, so that the service life of the silver-plated reflecting film is prolonged.
In order to achieve the purpose, the invention adopts the following technical scheme:
a silver-plated reflective film is sequentially provided with a high-refractive-index resin layer, a barrier layer, a base film layer, a silver reflective film layer, a corrosion-resistant glue layer and a reinforced reflective layer; the corrosion-resistant adhesive layer is a corrosion inhibitor which is easily complexed with silver and is added into the main adhesive; the enhanced reflecting layer is an aluminized film or a white film which can cover light.
The silver-plated reflecting film comprises a high-refractive-index resin layer and inorganic nanoparticles, wherein the weight ratio of the high-refractive-index resin layer to the acrylic resin layer is 99.5/0.5-40/60, and the refractive index of the high-refractive-index resin layer is 1.6-2.0.
The refractive index of the inorganic nanoparticles of the silver-plated reflective film is 1.65-2.70, the silver-plated reflective film specifically comprises one or more of titanium oxide, zirconium oxide, hafnium oxide, zinc oxide, tantalum oxide, cerium oxide and zinc sulfide, and the particle size is 5-80 nm.
In the silver-plated reflecting film, the barrier layer is formed by depositing one or more layers of silicon oxide and/or aluminum oxide layers on the reflecting surface of the base film layer.
In the silver-plated reflecting film, the visible light transmittance of the plastic film used for the base film layer is more than or equal to 88 percent, and the surface energy is more than 36 dyn/cm.
The corrosion-resistant adhesive layer of the silver-plated reflecting film comprises a main adhesive and a corrosion inhibitor, and the weight ratio of the main adhesive to the slow release agent is 100:0.01-100: 10.
The corrosion inhibitor of the silver-plated reflecting film comprises one or more of 1-Octadecanethiol (ODT), ethylene Glycol Dimercaptoacetate (GDA), trimethylolpropane tris (3-mercaptopropionate) (TMP), 5-methyl-1H-benzotriazole (MBT), pentaerythritol tetrakis (3-mercaptopropionate) (PTT) and 1-phenyl-5-mercaptotetrazole (PMTA).
According to the silvered reflecting film, the reflectivity of an aluminized film or a white film used for enhancing the reflecting layer at the wavelength of 550nm is more than or equal to 90%.
According to the silver-plated reflecting film, the thickness of the high-refractive-index resin layer is 0.1-3 mu m, the thickness of the barrier layer is 10-30 nm, the thickness of the base film layer is 12-100 mu m, the thickness of the silver reflecting film layer is 20-200nm, the thickness of the corrosion-resistant glue layer is 2-10 mu m, and the thickness of the enhanced reflecting layer is 10-75 mu m.
Has the advantages that:
1. the silver-plated reflecting film further improves the reflectivity of the silver-plated reflecting film through the synergistic effect of the high-refractive-index resin layer and the enhanced reflecting layer, and the reflectivity of the reflecting film at the wavelength of 550nm is more than or equal to 99%.
2. The silver-plated reflecting film provided by the invention forms sandwich protection for the silver reflecting film layer through the barrier layer and the corrosion-resistant adhesive layer, so that the silver reflecting film layer has more excellent corrosion resistance to water vapor, oxygen, halide and sulfur-containing gas, and the service life of the silver-plated reflecting film is prolonged.
3. The high-refractive-index resin layer is an acrylate resin layer added with inorganic nanoparticles, so that the reflectivity of the silver-plated reflecting film is improved, and the high-refractive-index resin layer also has excellent scratch resistance.
Drawings
FIG. 1 is a schematic structural view of a silver-plated reflective film according to the present invention.
In the drawings, the reference numerals denote: 1. the high-refractive-index resin layer comprises a high-refractive-index resin layer 2, a blocking layer 3, a base film layer 4, a silver reflecting film layer 5, a corrosion-resistant glue layer 6 and an enhanced reflecting layer.
The specific implementation mode is as follows:
the invention is described in further detail below with reference to specific embodiments, as shown in fig. 1:
the base film selected by the invention is a plastic film with excellent light transmission performance, and comprises one of a polyethylene terephthalate film, a polyethylene naphthalate film, a polymethyl methacrylate film and a triacetate film, and the polyethylene terephthalate film and the polyethylene naphthalate film are more preferable. Before the base film is used, the surface of the plastic film base material needs to be subjected to activation treatment by corona and/or plasma treatment technology. The surface of the plastic film can be cleaned through treatment, and the polymer structure on the surface of the plastic film can be modified through treatment, for example, the closed bonding state of the original material is changed, so that non-closed bonds such as broken bonds, surface dangling bonds, grafted active groups and the like appear, the surface activity is improved, the mechanical occlusion and physical adsorption between the coating and the base film are facilitated, and the adhesion between the coating and the base film is improved. The invention can achieve beneficial effects by carrying out corona treatment and plasma treatment on the surface of the base material or simultaneously adopting two technologies.
The visible light transmittance of the base film is more than or equal to 88 percent, and the overall reflectivity of the reflecting film is influenced if the visible light transmittance is too low; the surface energy of the base film is more than or equal to 36dyn/cm, and if the surface energy is too low, the activation treatment on the surface of the base film is insufficient, so that the adhesive force between the plating layer and the base film is influenced; the thickness of the base film is preferably 12-100 micrometers, more preferably 25-80 micrometers, the quality of the plated silver reflecting film layer is affected if the base film is too thin, and the overall thickness of the plated silver reflecting film is too thick and does not meet the requirement of the backlight module on thinning of the plated silver reflecting film.
The silver reflecting film selected by the invention is obtained by vacuum coating in common modes of vacuum thermal evaporation, electron beam Evaporation (EBPVD), magnetron sputtering and the like.
The purity of the silver used in the silver reflecting film layer is 99.99% or more, and the thickness of the silver layer is preferably 40-200 nm, and more preferably 50-120 nm. The silver reflecting film layer is formed through four stages of formation of critical nucleus, particle growth (island-shaped film), labyrinth structure (net-shaped film) and continuous film, and the silver is low in purity or thin in silver layer, so that the continuity of the silver reflecting film layer is poor, the island-shaped or net-shaped structure is presented, and the reflectivity of the silver-plated reflecting film is reduced; if the silver reflecting film layer is too thick, a silver mound is easily formed, so that the surface of the silver film is rough, the specular reflectivity is reduced, the reflectivity of the silver-plated reflecting film is reduced, and the method is not economical.
The high-refractive-index resin layer selected by the invention is a resin layer formed by adding inorganic nanoparticles with high refractive index into an acrylic resin layer, and the refractive index of the resin layer can be effectively controlled by controlling the adding amount of the inorganic nanoparticles with high refractive index. The reflectivity of the silvered reflective film can be effectively improved only when the difference between the refractive indexes of the high-refractive-index resin layer and the barrier layer with the medium refractive index is larger than 0.1. Meanwhile, inorganic nano particles in the resin layer with high refractive index are uniformly embedded to form a compact coating, so that the reduction of the brightness of the reflecting surface caused by element migration between the inorganic nano particles and the high-barrier deposition layer can be avoided, and the scratch resistance of the reflecting surface is improved.
The weight ratio of the acrylic resin layer to the inorganic nanoparticles in the high-refractive-index resin layer is 99.5/0.5-40/60, and the refractive index is 1.6-2.0. When the addition amount of the inorganic nanoparticles is too small, the refractive index of the high-refractive-index resin layer is less than 1.6, and the effect of improving the reflectivity of the silver-plated reflecting film cannot be achieved; when the amount of the inorganic nanoparticles added is too large, compatibility with the acrylic resin layer is deteriorated and it is not economical.
The refractive index of the inorganic nanoparticles is 1.65-2.70, preferably one or more of titanium oxide, zirconium oxide, hafnium oxide, zinc oxide, tantalum oxide, cerium oxide and zinc sulfide, and more preferably titanium oxide, zirconium oxide and zinc sulfide; the size of the inorganic nanoparticles is preferably 5-80nm, and more preferably 10-50 nm.
The thickness of the high refractive index resin layer is preferably 0.1 to 3 μm, and more preferably 0.3 to 1.5 μm. If the coating is too thin, the effects of improving the reflection reflectivity and scratch resistance of the silver coating cannot be achieved, and if the coating is too thick, the brightness of the reflecting surface is reduced, and the reflectivity of the silver coating reflecting film is also influenced. The high refractive index resin layer may be realized by a conventional coating means such as gravure coating, slide coating, screen roll coating, blade coating, slot coating, and the like.
The selected barrier layer has two functions, on one hand, the barrier layer can effectively prevent water vapor, oxygen and other corrosive gases from corroding the silver reflecting film layer through the permeation of the base film layer, so that the service life of the silver-plated reflecting film is prolonged; on the other hand, the reflectivity of the silvered reflecting film is further improved by utilizing the difference between the refractive index of the barrier layer and the high-refractive-index resin layer.
The barrier layer is formed by depositing one or more layers of silicon oxide and/or aluminum oxide layers on the reflecting surface of the base film layer, and the thickness of the barrier layer is preferably 10-30 nm, and more preferably 15-25 nm. Too thin a barrier layer results in poor barrier properties, while too thick a barrier layer results in reduced reflectivity of the silvered reflective film, and is also uneconomical. The barrier layer can be formed by a conventional coating method, such as vacuum thermal evaporation, electron beam Evaporation (EBPVD), magnetron sputtering, Plasma Enhanced Chemical Vapor Deposition (PECVD), and the like.
The anti-corrosion glue layer selected by the invention can effectively protect the silver reflecting film layer on one hand, and further improve the reflectivity of the silver-plated reflecting film by compounding with the enhanced reflecting layer on the other hand.
The anti-corrosion adhesive layer is a corrosion inhibitor which is added into the main adhesive and is easy to complex with silver, and the thickness of the adhesive layer is preferably 2-10 micrometers, and more preferably 5-8 micrometers. The corrosion inhibitor is introduced into the adhesive, so that the corrosion inhibitor forms an anti-corrosion layer at the interface of the adhesive and a silver film, thereby achieving the purpose of protecting the silver reflecting film layer. Therefore, the silver reflecting film layer cannot be protected when the adhesive layer is too thin, and the composite bonding performance of the adhesive layer and the enhanced reflecting layer is also poor; if the adhesive layer is too thick, the adhesive layer is compounded with the reinforced reflecting layer, so that adhesive overflow is easy to occur, and the method is not economical.
The corrosion inhibitor is preferably one or more of 1-Octadecanethiol (ODT), ethylene Glycol Dimercaptoacetate (GDA), trimethylolpropane tris (3-mercaptopropionate) (TMP), 5-methyl-1H-benzotriazole (MBT), pentaerythritol tetrakis (3-mercaptopropionate) (PTT) and 1-phenyl-5-mercaptotetrazole (PMTA), and more preferably one or more of 1-Octadecanethiol (ODT), ethylene Glycol Dimercaptoacetate (GDA), trimethylolpropane tris (3-mercaptopropionate) (TMP) and 5-methyl-1H-benzotriazole (MBT).
The adhesive used for the anti-corrosion adhesive layer is required to be capable of being mutually soluble with the corrosion inhibitor and simultaneously incapable of reacting with the corrosion inhibitor. One of acrylic, polyurethane and epoxy adhesives is preferable. The weight ratio of the adhesive to the corrosion inhibitor is 100:0.01-100:10, and when the ratio of the corrosion inhibitor is too low, a compact protective layer is difficult to form, so that the corrosion prevention effect is not achieved; when the height is too high, not only waste is caused, but also the reflectivity of the silvered reflecting film is reduced.
The enhanced reflection layer can be an aluminized film or a white film doped with an opacifier. The introduction of the enhanced reflecting layer ensures that the visible light leaked from the silver reflecting film layer can be reflected back again after entering the aluminized film or the white film, so that the reflectivity of the silvered reflecting film is improved to the maximum extent, the thickness of the silver layer is reduced, and the cost is reduced. Wherein, the side of the aluminum surface of the aluminizer is compounded with the silver film, and the service surfaces of the white film and the aluminizer require the reflectivity at the wavelength of 550nm to be more than 90 percent, and the reflectivity is more preferably more than 92 percent; the thickness of the enhanced reflection layer is 10 to 75 μm, and more preferably 12 to 50 μm.
The present invention is further illustrated by the following specific examples.
Example 1
1. Preparation of high refractive index resin layer coating material
9.6 parts by weight of aliphatic polyurethane acrylate prepolymer 6196-100 (Changxing chemical; functionality 10) is dissolved in 27.87 parts by weight of butanone solvent, 0.05 part by weight of leveling agent BYK-377 (Bike chemical), 0.40 part by weight of photoinitiator 184 (Tianjin Tianjiao chemical Co., Ltd.) is added, and finally 12.0 parts by weight of 20% titanium dioxide dispersion (Xuancheng crystal-Rexin; 20nm) is added to obtain a high-refractive-index resin layer material for later use.
2. Preparation of anti-corrosion adhesive for adhesive layer
LB 355100 parts by weight
Ethyl acetate 100 parts by weight
GDA 0.005 part by weight
100 parts by weight of a one-component polyacrylate adhesive LB355 (Lanbao chemical industry; solid content 50%) is dissolved in 100 parts by weight of an ethyl acetate solvent, and then 0.005 part by weight of ethylene glycol dimercaptoacetate GDA (Allantin; purity 99%) is added to obtain the anticorrosive adhesive layer adhesive for later use.
3. Preparation of silver-plated reflective film
Carrying out plasma technology treatment on both sides of a base film layer with the light transmittance of 89 percent and 50 mu mPE, and plating a silicon oxide barrier layer (the refractive index is 1.49 and the thickness is 20nm) on one side of a PET base film by PECVD; then coating the high-refractive-index resin coating on the surface of the barrier layer, firstly performing heat curing at 85 ℃,then 150mJ/cm2Carrying out secondary curing under ultraviolet light to obtain a resin layer with high refractive index (the refractive index is 1.60; the thickness is 0.3 mu m); after the process is finished, a silver reflecting film layer (the purity of metal silver is 99.99 percent, the thickness is 80nm) is deposited on the other surface of the PET basal film by vacuum thermal evaporation; and (3) coating the corrosion-resistant adhesive on the aluminum surface of a 12-micron aluminized film (with the reflectivity of 92%), performing thermosetting at 85 ℃ to obtain a corrosion-resistant adhesive layer (with the thickness of 5 microns), and compounding the corrosion-resistant adhesive layer with the silver reflecting film layer to obtain the silver-plated reflecting film. The silvered reflective film was cured at 50 ℃ for 72 h. The relevant data were measured and are shown in table 1.
Example 2
1. Preparation of high refractive index resin layer coating material
10.8 parts by weight of aliphatic polyurethane acrylate prepolymer 6196-100 (Changxing chemical; functionality 10) is dissolved in 31.35 parts by weight of butanone solvent, 0.05 part by weight of leveling agent BYK-377 (Bike chemical), 0.45 part by weight of photoinitiator 184 (Tianjin Tianjiao chemical Co., Ltd.) is added, and finally 3.0 parts by weight of 20% titanium dioxide dispersion (Xuancheng crystal-Rexin; 50nm) is added to obtain a high-refractive-index resin layer material for later use.
2. Preparation of anti-corrosion adhesive for adhesive layer
LB 355100 parts by weight
Ethyl acetate 100 parts by weight
0.05 part by weight of GDA;
100 parts by weight of a single-component polyacrylate adhesive LB355 (Lanbao chemical industry; solid content 50%) is dissolved in 100 parts by weight of an ethyl acetate solvent, and then 0.05 part by weight of ethylene glycol dimercaptoacetate GDA (Allantin; purity 99%) is added to obtain the anticorrosive adhesive layer adhesive for later use.
3. Preparation of silver-plated reflective film
Carrying out plasma technical treatment on two sides of a 25-micron PET (light transmittance of 90%) base film layer, and plating one side of the PET base film layer by PECVDA barrier layer of the upper silicon oxide layer (refractive index 1.40; thickness 15 nm); then coating the high refractive index resin coating on the surface of the barrier layer, thermally curing at 85 deg.C, and then 150mJ/cm2Obtaining a resin layer with high refractive index (refractive index 1.55; thickness 1.5 μm) by secondary curing under ultraviolet light; after the deposition, a silver reflecting film layer (with the thickness of 70nm) is deposited on the other surface of the PET base film through magnetron sputtering; and (3) coating the corrosion-resistant adhesive on the aluminum surface of a 50-micron aluminized film (with the reflectivity of 94%), carrying out thermosetting at 85 ℃ to obtain a corrosion-resistant adhesive layer (with the thickness of 10 microns), and compounding the corrosion-resistant adhesive layer with the silver reflecting film layer to obtain the silver-plated reflecting film. The silvered reflective film was cured at 50 ℃ for 72 h. The relevant data were measured and are shown in table 1.
Example 3
1. Preparation of high refractive index resin layer coating material
12.0 weight parts of ethoxylated pentaerythritol tetraacrylate monomer EM-2411 (Changxing chemical; functionality 4) is dissolved into 33.0 weight parts of butanone solvent, 0.05 weight parts of flatting agent BYK-377 (Pico chemical) is added, 0.50 weight parts of photoinitiator 184 (Tianjin Tianjiao chemical Co., Ltd.) is added, and finally 18.0 weight parts of 20% titanium dioxide dispersion liquid (Xuancheng crystal material; 50nm) is added to obtain the high-refractive-index resin layer material for later use.
2. Preparation of anti-corrosion adhesive for adhesive layer
LB 355100 parts by weight
Ethyl acetate 100 parts by weight
MBT 5 parts by weight;
100 parts by weight of a single-component polyacrylate adhesive LB355 (Lanbao chemical industry; solid content 50%) is dissolved in 100 parts by weight of an ethyl acetate solvent, and then 5 parts by weight of 5-methyl-1H-benzotriazole MBT (Annaiji; purity 98%) is added to obtain the anticorrosion adhesive for later use.
3. Preparation of silver-plated reflective film
Carrying out plasma technology treatment on both sides of a 38 mu mPEN (light transmittance of 92%) base film layer, and depositing an alumina barrier layer (refractive index of 1.55; thickness of 25nm) on one side of a PET base film by vacuum thermal evaporation; then coating the high refractive index resin coating on the surface of the barrier layer, thermally curing at 85 deg.C, and then 150mJ/cm2Carrying out secondary curing under ultraviolet light to obtain a resin layer with high refractive index (the refractive index is 1.68; the thickness is 0.5 mu m); after the process is finished, a silver reflecting film layer (the purity of metal silver is 99.99 percent, the thickness is 60nm) is deposited on the other surface of the PET basal film by vacuum thermal evaporation; and (3) coating the corrosion-resistant adhesive on the aluminum surface of a 50-micron aluminized film (with the reflectivity of 94%), carrying out thermosetting at 85 ℃ to obtain a corrosion-resistant adhesive layer (with the thickness of 7 microns), and compounding the corrosion-resistant adhesive layer with the silver reflecting film layer to obtain the silver-plated reflecting film. The silvered reflective film was cured at 50 ℃ for 72 h. The relevant data were measured and are shown in table 1.
Example 4
1. Preparation of high refractive index resin layer coating material
8.4 parts by weight of ethoxylated pentaerythritol tetraacrylate monomer EM-2411 (Changxing chemical; functionality 4) is dissolved in 23.13 parts by weight of butanone solvent, 0.05 part by weight of leveling agent BYK-377 (Bike chemical) is added, 0.50 part by weight of photoinitiator 184 (Tianjin Tianjiao chemical Co., Ltd.) is added, and finally 18.0 parts by weight of 20% zinc sulfide dispersion (Xuancheng crystal Rexin; 20nm) is added to obtain a high-refractive-index resin layer material for later use.
2. Preparation of anti-corrosion adhesive for adhesive layer
LB 355100 parts by weight
Ethyl acetate 100 parts by weight
0.2 part by weight of TMP;
100 parts by weight of a single-component polyacrylate adhesive LB355 (Lanbao chemical industry; solid content 50%) is dissolved in 100 parts by weight of an ethyl acetate solvent, and then 0.2 part by weight of trimethylolpropane tris (3-mercaptopropionate) TMP (Annaiji; purity 85%) is added to obtain the anticorrosive adhesive for later use.
3. Preparation of silver-plated reflective film
Carrying out plasma technology treatment on both sides of a 12 mu mPEN (light transmittance of 90%) base film layer, and depositing a silicon oxide barrier layer (with the refractive index of 1.49 and the thickness of 20nm) on one side of a PET base film by PECVD; then coating the high refractive index resin coating on the surface of the barrier layer, thermally curing at 85 deg.C, and then 150mJ/cm2Carrying out secondary curing under ultraviolet light to obtain a resin layer with high refractive index (the refractive index is 1.66; the thickness is 1.5 mu m); after the deposition, a silver reflecting film layer (the purity of the metal silver is 99.99 percent, the thickness is 20nm) is deposited on the other surface of the PET basal film through magnetron sputtering; and (3) coating the corrosion-resistant adhesive on a white film with the thickness of 75 micrometers (the reflectivity is 90%), performing thermosetting at the temperature of 85 ℃ to obtain a corrosion-resistant adhesive layer (the thickness is 3 micrometers), and compounding the corrosion-resistant adhesive layer with the silver reflective film layer to obtain the silver-plated reflective film. The silvered reflective film was cured at 50 ℃ for 72 h. The relevant data were measured and are shown in table 1.
Example 5
1. Preparation of high refractive index resin layer coating material
7.2 parts by weight of aliphatic polyurethane acrylate prepolymer 6196-100 (Changxing chemical; functionality 10) is dissolved in 18.39 parts by weight of butanone solvent, 0.05 part by weight of leveling agent BYK-377 (Bike chemical), 0.40 part by weight of photoinitiator 184 (Tianjin Tianjiao chemical Co., Ltd.) is added, and finally 24.0 part by weight of 20% chromium dioxide dispersion (Xuancheng crystal Rexin; 10nm) is added to obtain a high-refractive-index resin layer material for later use.
2. Preparation of anti-corrosion adhesive for adhesive layer
LB 355100 parts by weight
Ethyl acetate 100 parts by weight
0.005 part by weight of GDA;
100 parts by weight of a one-component polyacrylate adhesive LB355 (Lanbao chemical industry; solid content 50%) is dissolved in 100 parts by weight of an ethyl acetate solvent, and then 0.005 part by weight of ethylene glycol dimercaptoacetate GDA (Allantin; purity 99%) is added to obtain the anticorrosive adhesive layer adhesive for later use.
3. Preparation of silver-plated reflective film
Carrying out plasma technical treatment on two surfaces of a 50-micron PET (light transmittance is 89%) base film layer, and plating a silicon oxide barrier layer (with the refractive index of 1.40 and the thickness of 10nm) on one surface of a PET base film by PECVD; then coating the high refractive index resin coating on the surface of the barrier layer, thermally curing at 85 deg.C, and then 150mJ/cm2Carrying out secondary curing under ultraviolet light to obtain a resin layer with high refractive index (the refractive index is 1.71; the thickness is 0.5 mu m); after the process is finished, a silver reflecting film layer (the purity of the metal silver is 99.99 percent, the thickness is 80nm) is deposited on the other surface of the PET basal film through magnetron sputtering; and (3) coating the corrosion-resistant adhesive on the aluminum surface of a 12-micron aluminized film (with the reflectivity of 92%), performing thermosetting at 85 ℃ to obtain a corrosion-resistant adhesive layer (with the thickness of 7 microns), and compounding the corrosion-resistant adhesive layer with the silver reflecting film layer to obtain the silver-plated reflecting film. The silvered reflective film was cured at 50 ℃ for 72 h. The relevant data were measured and are shown in table 1.
Example 6
1. Preparation of high refractive index resin layer coating material
9.0 weight part of aliphatic polyurethane acrylate prepolymer UXE1000 (chemical industry; functionality 4) is dissolved in 25.5 weight parts of butanone solvent, 0.05 weight part of leveling agent BYK-377 (Pico chemical industry), 0.40 weight part of photoinitiator 184 (Tianjin Tianjiao chemical industry Co., Ltd.) is added, and finally 2415.0 weight part of 20% chromium dioxide dispersion liquid (Xuancheng crystal-Rexin; 20nm) is added to obtain the high-refractive-index resin layer material for later use.
2. Preparation of anti-corrosion adhesive for adhesive layer
LB 355100 parts by weight
Ethyl acetate 100 parts by weight
ODT 0.05 weight portion;
100 parts by weight of a single-component polyacrylate adhesive LB355 (Lamebao chemical industry; solid content 50%) is dissolved in 100 parts by weight of an ethyl acetate solvent, and then 0.05 part by weight of 1-octadecanethiol ODT (Western Asia reagent; purity 99%) is added to obtain the anticorrosion adhesive layer for later use.
3. Preparation of silver-plated reflective film
Carrying out plasma technical treatment on both sides of a 50-micron PET (light transmittance is 89%) base film layer, and plating a silicon oxide barrier layer (with the refractive index of 1.42 and the thickness of 20nm) on one side of the PET base film layer by PECVD; then coating the high refractive index resin coating on the surface of the barrier layer, thermally curing at 85 deg.C, and then 150mJ/cm2Carrying out secondary curing under ultraviolet light to obtain a high-refractive-index resin layer (the refractive index is 1.64; the thickness is 0.5 mu m); after the process is finished, a silver reflecting film layer (the purity of the metal silver is 99.99 percent, the thickness is 80nm) is deposited on the other surface of the PET basal film through magnetron sputtering; and (3) coating the corrosion-resistant adhesive on the aluminum surface of a 12-micron aluminized film (with the reflectivity of 92%), performing thermosetting at 85 ℃ to obtain a corrosion-resistant adhesive layer (with the thickness of 7 microns), and compounding the corrosion-resistant adhesive layer with the silver reflecting film layer to obtain the silver-plated reflecting film. The silvered reflective film was cured at 50 ℃ for 72 h. The relevant data were measured and are shown in table 1.
Example 7
1. Preparation of high refractive index resin layer coating material
7.8 parts by weight of aliphatic polyurethane hexaacrylate prepolymer EB5129 (CyanoTechnology, Inc.; functionality 6) was dissolved in 20.76 parts by weight of butanone solvent, 0.05 parts by weight of leveling agent BYK-377 (Bike chemical Co., Ltd.), 0.40 parts by weight of photoinitiator 184 (Tianjin Tianjiao chemical Co., Ltd.) was added, and finally 21.0 parts by weight of 20% titanium dioxide dispersion (Xuancheng crystal Rexin; 20nm) was added to obtain a high refractive index resin layer material for use.
2. Preparation of anti-corrosion adhesive for adhesive layer
LB 355100 parts by weight
Ethyl acetate 100 parts by weight
0.005 part by weight of GDA;
100 parts by weight of a one-component polyacrylate adhesive LB355 (Lanbao chemical industry; solid content 50%) is dissolved in 100 parts by weight of an ethyl acetate solvent, and then 0.005 part by weight of ethylene glycol dimercaptoacetate GDA (Allantin; purity 99%) is added to obtain the anticorrosive adhesive layer adhesive for later use.
3. Preparation of silver-plated reflective film
Carrying out plasma technology treatment on both sides of a 75 mu mPE (light transmittance of 88%) base film layer, and depositing a layer of aluminum oxide barrier layer (with the refractive index of 1.60 and the thickness of 10nm) on one side of a PET base film by vacuum thermal evaporation; then coating the high refractive index resin coating on the surface of the barrier layer, thermally curing at 85 deg.C, and then 150mJ/cm2Carrying out secondary curing under ultraviolet light to obtain a resin layer with high refractive index (the refractive index is 1.71; the thickness is 1.5 mu m); after the process is finished, a silver reflecting film layer (the purity of metal silver is 99.99 percent, and the thickness is 120nm) is deposited on the other surface of the PET base film through vacuum thermal evaporation; and (3) coating the corrosion-resistant adhesive on the aluminum surface of a 12-micron aluminized film (with the reflectivity of 92%), performing thermosetting at 85 ℃ to obtain a corrosion-resistant adhesive layer (with the thickness of 5 microns), and compounding the corrosion-resistant adhesive layer with the silver reflecting film layer to obtain the silver-plated reflecting film. The silvered reflective film was cured at 50 ℃ for 72 h. The relevant data were measured and are shown in table 1.
Comparative example 1
1. Preparation of high refractive index resin layer coating material
9.6 parts by weight of aliphatic polyurethane acrylate prepolymer 6196-100 (Changxing chemical; functionality 10) is dissolved in 27.87 parts by weight of butanone solvent, 0.05 part by weight of leveling agent BYK-377 (Bike chemical), 0.40 part by weight of photoinitiator 184 (Tianjin Tianjiao chemical Co., Ltd.) is added, and finally 12.0 parts by weight of 20% titanium dioxide dispersion (Xuancheng crystal-Rexin; 50nm) is added to obtain the high-refractive-index resin layer material for later use.
2. Preparation of anti-corrosion adhesive for adhesive layer
LB 355100 parts by weight
Ethyl acetate 100 parts by weight
100 parts by weight of a one-component polyacrylate adhesive LB355 (Lanbao chemical; solid content 50%) is dissolved in 100 parts by weight of an ethyl acetate solvent to obtain a polyacrylate adhesive for later use.
3. Preparation of silver-plated reflective film
Carrying out plasma technology treatment on both sides of a base film layer with the light transmittance of 89 percent and 50 mu mPE, and plating a silicon oxide barrier layer (the refractive index is 1.49 and the thickness is 20nm) on one side of a PET base film by PECVD; then coating the high refractive index resin coating on the surface of the barrier layer, thermally curing at 85 deg.C, and then 150mJ/cm2Carrying out secondary curing under ultraviolet light to obtain a resin layer with high refractive index (the refractive index is 1.60; the thickness is 0.3 mu m); after the process is finished, a silver reflecting film layer (the purity of metal silver is 99.99 percent, the thickness is 80nm) is deposited on the other surface of the PET basal film by vacuum thermal evaporation; the polyacrylic acid adhesive is coated on an aluminum surface of a 12-micron aluminized film (with the reflectivity of 92%), the adhesive is obtained through thermosetting at 85 ℃ to obtain the adhesive (with the thickness of 5 microns), and then the adhesive is compounded with a silver reflecting film layer to obtain the silver-plated reflecting film. The silvered reflective film was cured at 50 ℃ for 72 h. The relevant data were measured and are shown in table 1.
Comparative example 2
1. Preparation of anti-corrosion adhesive for adhesive layer
LB 355100 parts by weight
Ethyl acetate 100 parts by weight
0.005 part by weight of GDA;
100 parts by weight of a one-component polyacrylate adhesive LB355 (Lanbao chemical industry; solid content 50%) is dissolved in 100 parts by weight of an ethyl acetate solvent, and then 0.005 part by weight of ethylene glycol dimercaptoacetate GDA (Allantin; purity 99%) is added to obtain the anticorrosive adhesive layer adhesive for later use.
2. Preparation of silver-plated reflective film
Carrying out plasma technology treatment on both sides of a 50 mu mPE (light transmittance: 89%) base film layer, and depositing a silver reflecting film layer (the purity of metal silver is 99.99 percent, and the thickness is 80nm) on one side of a PET base film layer by vacuum thermal evaporation; the polyacrylic acid adhesive is coated on an aluminum surface of a 12-micron aluminized film (with the reflectivity of 92%), the adhesive is obtained through thermosetting at 85 ℃ to obtain the adhesive (with the thickness of 5 microns), and then the adhesive is compounded with a silver reflecting film layer to obtain the silver-plated reflecting film. The silvered reflective film was cured at 50 ℃ for 72 h. The relevant data were measured and are shown in table 1.
Comparative example 3
1. Preparation of high refractive index resin layer coating material
9.6 parts by weight of aliphatic polyurethane acrylate prepolymer 6196-100 (Changxing chemical; functionality 10) is dissolved in 27.87 parts by weight of butanone solvent, 0.05 part by weight of leveling agent BYK-377 (Bike chemical), 0.40 part by weight of photoinitiator 184 (Tianjin Tianjiao chemical Co., Ltd.) is added, and finally 12.0 parts by weight of 20% titanium dioxide dispersion (Xuancheng crystal-Rexin; 50nm) is added to obtain the high-refractive-index resin layer material for later use.
2. Preparation of silver-plated reflective film
Carrying out plasma technology treatment on both sides of a base film layer with the light transmittance of 89 percent and 50 mu mPE, and plating a silicon oxide barrier layer (the refractive index is 1.49 and the thickness is 20nm) on one side of a PET base film by PECVD; then coating the high refractive index resin coating on the surface of the barrier layer, thermally curing at 85 deg.C, and then 150mJ/cm2Carrying out secondary curing under ultraviolet light to obtain a resin layer with high refractive index (the refractive index is 1.60; the thickness is 0.3 mu m); after the process is finished, a silver reflecting film layer (the purity of metal silver is 99.99 percent, the thickness is 80nm) is deposited on the other surface of the PET basal film by vacuum thermal evaporation; in silver reflectionAnd coating a layer of GDA ethyl acetate solution with the solid content of 5% on the film layer to obtain the silver-plated reflecting film. The relevant data were tested and are shown in table 1.
Comparative example 4
Directly thermally evaporating a 50-micron PET (polyethylene terephthalate) base film (with the light transmittance of 89%) on the inner surface to form a silver reflecting film layer (with the purity of metal silver of 99.99 percent and the thickness of 80 nm); and coating a layer of polyacrylate adhesive with the thickness of 3 micrometers and the solid content of 25% on the aluminum surface of the 12-micrometer aluminum-plated film (the reflectivity is 92%), and compounding the polyacrylate adhesive with the silver reflecting film layer to obtain the silver-plated reflecting film. The silvered reflective film was cured at 50 ℃ for 72 h. The relevant data were measured and are shown in table 1.
TABLE 1
The combined action of the high-refractive-index resin layer and the enhanced reflecting layer in the embodiments 1-6 can ensure that the reflectivity of the silvered reflecting film at the visible light wavelength of 550nm is 99% or more; the corrosion resistance of the silver-plated reflective film is obviously improved under the combined action of the barrier layer and the corrosion-resistant glue layer; in comparative example 1, the edge of the reflective film was corroded after the high temperature and high humidity aging test due to no corrosion inhibitor added to the adhesive layer, and the reflectance was reduced more at the same time; in comparative example 2, no barrier layer and high refractive index resin layer were provided, the reflectance was low before and after aging, and the edge of the reflective film was corroded after the high temperature and high humidity corrosion aging test; in the comparative example 3, no enhanced reflection layer is arranged, and a layer of corrosion inhibitor solution is directly coated, so that the silver layer is not protected; in the comparative example 4, the substrate is directly plated with silver without treatment, the corrosion inhibitor is not added in the adhesive, and the overall performance of the silver-plated reflecting film is obviously reduced after the reflecting film is subjected to a high-temperature high-humidity aging test.
The above description is only a preferred embodiment of the present invention, and does not limit the present invention, and those skilled in the art can make various modifications and variations; any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
The method for detecting the performance of the silver-plated reflecting film prepared in the implementation and comparative examples comprises the following steps:
1. and (3) reflectivity testing:
according to GB/T3979-2008 'measuring method for object color'. The test was carried out using a Konika minolta spectrophotometer CM-2600d, taking the reflectance at 550 nm.
2. High temperature and high humidity aging test:
and (3) placing the sample in a constant temperature and humidity box with 65 ℃ and 90% RH for aging test, after 200h, performing reflectivity test, observing edge corrosion condition and performing silver layer stripping test.
3. Silver layer stripping test:
and (4) scratching the sample wafer aged at high temperature and high humidity to the adhesive layer on one side by using a blade, stripping the antireflection protection layer and the substrate, and observing whether the silver layer falls off on the substrate.
Claims (7)
1. A silver-plated reflective film characterized in that: the silver-plated reflecting film is sequentially provided with a high-refractive-index resin layer (1), a barrier layer (2), a base film layer (3), a silver reflecting film layer (4), a corrosion-resistant adhesive layer (5) and a reinforced reflecting layer (6), wherein the corrosion-resistant adhesive layer is formed by adding a corrosion inhibitor which is easily complexed with silver into a main adhesive; the enhanced reflecting layer is an aluminized film or a white film which can cover light;
the high-refractive-index resin layer comprises acrylic resin and inorganic nanoparticles, the weight ratio of the acrylic resin to the inorganic nanoparticles is 99.5/0.5-40/60, and the refractive index is 1.6-2.0;
the refractive index of the inorganic nanoparticles is 1.65-2.70, the inorganic nanoparticles specifically comprise one or more of titanium oxide, zirconium oxide, hafnium oxide, zinc oxide, tantalum oxide, cerium oxide and zinc sulfide, and the particle size is 5-80 nm;
before use, the base film layer is subjected to activation treatment by corona and/or plasma treatment technology on the surface of the plastic film base material, and a modification effect is generated on a high molecular structure on the surface of the plastic film, so that the original material closed bonding state is changed, a non-closed bond is generated, and the surface activity is improved.
2. The silvered reflective film of claim 1, wherein the barrier layer is formed by depositing one or more layers of silicon oxide and/or aluminum oxide on the reflective surface of the base film layer.
3. The silver-plated reflecting film according to claim 2, wherein the plastic film used for the base film layer has a visible light transmittance of 88% or more and a surface energy of 36dyn/cm or more.
4. The silver-plated reflecting film according to claim 3, wherein the corrosion-resistant adhesive layer comprises a main adhesive and a corrosion inhibitor, and the weight ratio of the main adhesive to the slow-release agent is 100:0.01-100: 10.
5. The silver-coated reflective film according to claim 4, wherein said corrosion inhibitor comprises one or more of 1-Octadecanethiol (ODT), ethylene Glycol Dimercaptoacetate (GDA), trimethylolpropane tris (3-mercaptopropionate) (TMP), 5-methyl-1H-benzotriazole (MBT), pentaerythritol tetrakis (3-mercaptopropionate) (PTT), and 1-phenyl-5-mercaptotetrazole (PMTA).
6. The silver-plated reflective film according to claim 5, wherein the reflectance of the aluminum-plated film or white film used for the reflection enhancing layer at a wavelength of 550nm is not less than 90%.
7. The silver-plated reflective film according to claim 6, wherein the thickness of the high refractive index resin layer is 0.1 to 3 μm, the thickness of the barrier layer is 10 to 30nm, the thickness of the base film layer is 12 to 100 μm, the thickness of the silver reflective film layer is 20 to 200nm, the thickness of the corrosion-resistant adhesive layer is 2 to 10 μm, and the thickness of the enhanced reflective layer is 10 to 75 μm.
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| CN109655950A (en) * | 2018-12-17 | 2019-04-19 | 宁波激智科技股份有限公司 | A kind of dirty high silver lustre reflectance coating of slim anti-finger of high reliability |
| CN109870753A (en) * | 2018-12-21 | 2019-06-11 | 宁波激智科技股份有限公司 | A kind of dirty silver-colored reflectance coating of the anti-finger of super bright high reliability |
| CN110328466B (en) * | 2019-07-06 | 2021-09-21 | 苏州龙腾万里化工科技有限公司 | Halogen-free cleaning-free soldering flux |
| CN113400757A (en) * | 2021-07-16 | 2021-09-17 | 马鞍山东毅新材料科技有限公司 | Silver reflective display screen composite film and production process thereof |
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| CN114045124A (en) * | 2021-12-01 | 2022-02-15 | 上海尚傲新材料科技有限公司 | Magnetron sputtering Low-E film |
| CN115016168A (en) * | 2021-12-31 | 2022-09-06 | 东莞市托普莱斯光电技术有限公司 | High-brightness silver-plated reflective film for backlight module |
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