Untitled record

FIELD OF THE INVENTION The present invention relates to an optical device in which a plastic base member is arranged.

Optical devices with an anti-reflection film on a plastic backing are well known in the art. It is also known to apply a thin layer of metal film to the surface of a plastic substrate in order to improve adhesion between the substrate and the anti-reflection film. For example, JP-A-186202/1987 discloses an optical device having a thin metal layer applied to a surface of a plastic backing layer, wherein the metal layer material is selected from the group consisting of Cu, Al, Ni, Au, Cr, Pd and Sn. .

However, these optical devices are inadequate in terms of heat resistance and impact resistance. As a result, it was necessary to further develop or improve these physical properties.

In order to improve the strength and impact resistance of film coatings, usually plastic lenses SiO₂ we provide a base coat. However, SiO₂ The disadvantage of this layer is that it reduces the heat resistance of the plastic lens.

It is an object of the present invention to solve these problems, for example, it is an object of the present invention to provide an optical device having a plastic base layer and an anti-reflection film layer, and

95184-13034 / FT-Ko

-2, which has excellent adhesion properties between the base coat and the anti-reflection film, which has excellent heat resistance and impact resistance.

The present inventors have carefully studied the solutions to the problems described above and, as a result, have found that by forming a niobium (Nb) layer between the plastic backing and the anti-reflection film, which together forms an optical device, between the backing and the anti-reflection film adhesion, as well as heat resistance and impact resistance or impact resistance of the optical device are enhanced.

Thus, the present invention is essentially directed to the production of an optical device in which a plastic substrate and a niobium substrate (Nb) and an anti-reflection film layer are arranged in that order.

It is an object of our invention to provide an optical device in which a plastic base member is arranged and the following layers are formed on the plastic base member in sequence:

- a base layer of niobium, containing 0% to 50% by weight of one or more alloys selected from the group consisting of aluminum, tantalum, chromium and mixtures thereof, and

- anti-reflection film.

The base layer is preferably formed of niobium.

The base layer is preferably 1 to 5 nm thick.

The backing layer is preferably formed by an ion-beam deposition process.

The anti-reflection film layer is preferably formed of two or more sub-layers.

Preferably, the at least one sublayer of the anti-reflection film layer is formed by ion-beam deposition.

The antireflection film layer is preferably formed of a low refractive silica sublayer and a high refractive titanium dioxide sublayer.

The antireflection film layer preferably comprises a niobium sublayer.

Preferably, the antireflection film layer is one to seven sequentially mounted on the base layer. The sub-layers and the sub-layers 1, 3, 5 and 7 are formed of silica, the sub-layers 2, 4 and 6 are made of titanium dioxide.

Advantageously, the anti-reflection film layer is formed by the first to seventh sequentially applied layers on the base layer. and sub-layers 1, 3, 5 and 7 of silicon dioxide, sub-layer 2 of niobium, sub-layers 4 and 6 of titanium dioxide.

Preferably, a hardened film layer is disposed between the plastic base member and the base layer.

Thus, it can be seen that the optical device of the present invention has a base layer of niobium (Nb) and thereby provides not only excellent adhesion between the plastic substrate and the anti-reflection film, but also excellent resistance to abrasion and impact. properties such as the low value of the metal absorption index.

In a very favorable case, the niobium base layer contains 100% by weight niobium. However, mixtures of niobium and other elements, such as aluminum, chromium, tantalum, and mixtures of two or more of these elements may be used. The amount of these additional elements may be up to 50% by weight over the whole layer, preferably up to 25% by weight.

Preferably, the anti-reflection film layer comprises two or more sub-layers. It is very advantageous if the sub-layers in the anti-reflection film layer are arranged so that the low refractive index layers and the high refractive index layers alternate. Two embodiments corresponding to such a layered structure will now be described.

However, it is also advantageous if the niobium backing layer is formed by an ion-beam deposition process, which further increases the impact resistance and abrasion resistance. Furthermore, it is very advantageous if at least one or some of the layers of the anti-reflection film layer is formed by this method.

In the ion beam deposition process, a certain material is deposited from a vapor phase on a substrate, such as a lens, by using ion plasma in a gas atmosphere such as argon and / or oxygen. The apparatus for carrying out the process generally operates in such a way that, among the key parameters of vapor phase separation, the preferred accelerating voltage is 100 to 250 V and the accelerating current is between 50 and 150 mA. A detailed description of the process can be found in U.S. Patent No. 5,268,781. Further details are described in Fliedner et al., Society of Vacuum Coaters, Albuquerque, NM, USA, 237-241. 1995, p., and from sources cited herein.

In the ion-beam separation process, argon is the preferred ionizing gas because it protects the film to be formed from oxidation. This stabilizes the resulting film quality and allows easy control of film thickness through the use of an optical film thickness gauge.

In the ion beam separation process, in order to achieve proper adhesion between the plastic substrate and the substrate, and to obtain sufficient homogeneity of the resulting film structure, the plastic substrate must be subjected to ion-beam pre-treatment prior to forming the substrate. During ion gun pretreatment, the ionizing gas may be argon or oxygen. In the power range, the accelerating voltage is most preferably 50 to 200 V, and the accelerating current is preferably 50 to 150 mA.

If either the accelerating voltage or the accelerating current is lower than the corresponding lower limit mentioned above, the adhesion enhancement effect between the plastic substrate and the underlying substrate will not be sufficient in some cases. On the other hand, if either the accelerating voltage or the accelerating current exceed said upper limit, the plastic core and the hardened film layer, as well as the hard coating layer thereon, may become yellowed or the wear resistance of the optical device may be reduced.

According to the present invention, the anti-reflection film layer is formed after applying a niobium base layer to the base member. Several possible methods may be considered in developing an anti-reflection film layer. For example, it may be formed from a vapor phase such as chemical vapor deposition (CVD), reactive physical vapor deposition (PVD), or other methods such as ion plating from a vapor phase.

The low refractive index sub-layer of the anti-reflection film layer is the silica sub-layer and the high refractive index layer is the titanium dioxide sub-layer. If necessary

6, the antireflection film layer may also contain a niobium sublayer.

By forming a low-refractive silica layer by employing an ion-beam deposition process to settle the silica in the presence of argon gas as the ionizing gas, the residual stress within these sub-layers can be eliminated and wear resistance increased. In order to achieve this extremely favorable result, the conditions of the ion-beam separation process should preferably be adjusted so that the ionic current density in the dome of the digestion apparatus is between 15 and 35 μΑ and the accelerating voltage is between 400 and 700 V.

If the ion current density is less than 15 μΑ or the accelerating voltage is less than 400 V, the effect of reducing the internal voltage and increasing the abrasion resistance is difficult to achieve. On the other hand, if the ion current density is greater than 35 μΑ or the accelerating voltage is above 700 V, the plastic core may become yellow or the optical properties may be slightly impaired.

A high refractive index sub-layer, such as a titanium dioxide layer, ion-beam deposition! method. Since the ionizing gas is preferably O₂ or Ar, more preferably O₂ and a mixture of Ar, as this helps to increase the refractive index of the resulting high refractive index and also promotes the increase of abrasion resistance. O₂ The mixing ratio of Ar to Ar is preferably from 1: 0.5 to 2.

The materials used to form the high refractive index include titanium dioxide, dinibium pentoxide, ditantal pentoxide, zinc oxide, diittrium trioxide, and

-7 • · ·· / '* · * a mixture of these. Preferably, titanium dioxide, dinibium pentoxide, ditantal pentoxide and mixtures thereof.

If TiO₂, Nb₂Os or mixtures of these two compounds are used, ion beam separation! The process parameters should preferably be set so that the ionic current density in the separation device dome is between 8 and 15 μΑ and the accelerating voltage between 300 and 700 V. O₂ and the ratio of Ar in the ionizing gas mixture may conveniently be from 1: 0.7 to 1: 1.0.

If the Ta₂05 or a mixture thereof, TiO₂and / or Nb₂With Os - apply, ion beam separation! The process parameters are preferably set so that the ionic current density in the separation device dome is between 12 and 20 μΑ and the accelerating voltage is between 400 and 700 V. O₂ and the ratio of Ar to the ionizing gas mixture is preferably from 1: 0.5 to 1: 2.0.

If the ion current density, accelerating voltage, and ionizing gas ratios are outside the specified ranges, the target refractive index will not be achieved and, in addition, the absorbance index may be increased and / or the abrasion resistance reduced.

The thickness of the backing layer of the optical device according to the invention is preferably between 1 and 5 nm. If this thickness exceeds the specified range, the base layer may exhibit an absorbency problem within the layer.

Advantageous embodiments A and B of the antireflection film layer formed on the plastic substrate and of the BL substrate layer are described below with reference to the thickness and material of the layer. In these embodiments, the multilayer structure formed from sublayers 1 to 7 serves as an anti-reflection film layer.

-8.... * ···· ♦·, :

• ·! .···* ···. : · ·-···/· ... ··♦ · ··

<td colspan="2">BL:</td><td>(THE) nb</td><td>1-5 nm</td><td>BL:</td><td>(B) nb</td><td>1-5 nm</td>

<td> 1.</td><td>layer:</td><td>SiO₂</td><td>5 to 50 nm</td><td>Layer 1:</td><td>SiO₂</td><td>20-100 nm</td>

<td> 2.</td><td>layer:</td><td>TiO₂</td><td>1-15 nm</td><td>Layer 2:</td><td>nb</td><td>1-5 nm</td>

<td> 3.</td><td>layer:</td><td>SiO₂</td><td>20-360 nm</td><td>Layer 3:</td><td>SiO₂</td><td>20-100 nm</td>

<td> 4.</td><td>layer:</td><td>TiO₂</td><td>5 to 55 nm</td><td>Layer 4:</td><td>TiO₂</td><td>5-55 nm</td>

<td> 5.</td><td>layer:</td><td>SiO₂</td><td>5 to 50 nm</td><td>Layer 5:</td><td>SiO₂</td><td>5 to 50 nm</td>

<td> 6.</td><td>layer:</td><td>TiO₂</td><td>5-130 nm</td><td>Layer 6:</td><td>TiO₂</td><td>Δ -130 nm</td>

<td> 7.</td><td>layer:</td><td>SiO₂</td><td>70-100 nm</td><td>Layer 7:</td><td>SiO₂</td><td>70-100 nm</td>

<td></td><td>THE</td><td>layer thickness</td><td colspan="2">ranges above</td><td colspan="2">the most favorable are the</td>

adhesion between the plastic substrate and the anti-reflection film, as well as the thermal and impact resistance of the optical device.

The material of the plastic base element used in the present invention is not specified. Preferred are methyl methacrylate homopolymers, methyl methacrylate copolymers, and one or more other monomers, diethylene glycol bisallyl carbonate homopolymers, diethylene glycol bisallyl carbonate copolymers, and one or more other monomers, sulfur-containing copolymers, such as polystyrenes, polyvinylchlorides, unsaturated polyesters, polyethylene terephthalates, polyurethanes and polyurethanes.

If necessary, the optical device of the invention may also comprise a hardened film layer between the plastic substrate and the substrate.

As the material of the hardened film layer, it is desirable to use a compound containing metal oxide colloidal particles and an organosilicon compound represented by the following general formula (1):

- 9 - (R¹ )price²) BSi (OR³) -4- (a_{+ B)}, (1) wherein R¹ and R² each independently selected from the group consisting of C 1 -C 8 alkyl, C 2 -C 8 alkenyl, aryl (phenyl or 5- or 6-membered heteroaryl) with at least one sulfur or nitrogen heteroatom optionally substituted by one or more 1 to 6 carbon atoms; C 3 -C 8 alkyl group or groups), C 1 -C 8 acyl, halogen, glycidoxy, epoxy, amino, phenyl, mercapto, methacryloxy, and cyano; R³ and a group selected from C 1-8 alkyl, C 1-8 acyl, and phenyl; and a and b are independently 1 or 0.

Specific examples of organic silicon compounds of formula (1) include methyl silicate, ethyl silicate, n-propyl silicate, isopropyl silicate, n-butyl silicate, sec-butyl silicate, tert-butyl silicate, tetraacetoxy, and the like. silane, methyl trimethoxysilane, methyl triethoxysilane, methyl tripropoxysilane, methyl triacetoxysilane, methyl tributoxysilane, methyl tripropoxysilane, methyl triamyloxysilane, methyl triphenoxysilane , methyltribenzyloxysilane, methyltriphenethyloxysilane, glycidoxymethyltrimethoxysilane, glycidoxymethyltriethoxysilane, α-glycidoxyethyltriethoxysilane, β-glycidoxyethyltrimethoxysilane, β-glycidoxyethyltriethoxysilane, α-glycidoxy- propyltrimethoxysilane,? -glycidoxypropyltriethoxysilane,? -glycidoxypropyltrimethoxysilane,? -glycidoxypropyltriethoxysilane,? -glycidoxypropyltrimethoxysilane,? -glycidoxy-? propyl triethoxysilane, γ-glycidoxypropyltripropoxysilane, γ-glycidoxypropyl tributoxysilane, γ-glycidoxypropyltriphenoxysilane, α-glycidoxy-butyl-trimethoxysilane, α-glycidoxy-butyl-triethoxysilane, β-glycidoxy-butyl-trimethoxysilane, β-glycidoxy-butyl-triethoxysilane, γ-glycidoxy-butyl-trimethoxysilane, γ-glycidoxy-butyl-triethoxysilane, δ-glycidoxy-butyl-trime · «· · ···· ·

- 10-Toxosilane, δ-glycidoxybutyl triethoxysilane, (3,4-epoxycyclohexyl) methyltrimethoxysilane, (3,4-epoxycyclohexyl) methyl triethoxysilane, B- (3,4-epoxycyclohexyl) ethyl tri methoxysilane, B- (3,4-epoxycyclohexyl) ethyl triethoxysilane, S- (3,4-epoxycyclohexyl) ethyl tripropoxysilane, B- (3,4-epoxycyclohexyl) ethyl tributoxy- silane, B- (3,4-epoxycyclohexyl) ethyl-triphenoxysilane, γ- (3,4-epoxycyclohexyl) propyl trimethoxysilane, γ- (3,4-epoxycyclohexyl) propyl methoxysilane, 5- (3,4-epoxycyclohexyl) butyl trimethoxysilane, O- (3,4-epoxycyclohexyl) butyl triethoxysilane, glycidoxymethylmethyldimethoxysilane, glycidoxymethylmethyl diethoxysilane, α-glycidoxyethylmethyldimethoxysilane, α-glycidoxyethylmethyl diethoxysilane, β-glycidoxyethylmethyldimethoxysilane, β-glycidoxyethylmethyl diethoxysilane, α- glycidoxypropylmethyldimethoxysilane,? -glycidoxypropylmethyldimethoxysilane,? -glycidoxypropylmethyldimethoxysilane,? -glycidoxypropylmethyldimethoxysilane, γ-glycidoxypropylmethyldimethoxysilane, γ-glycidoxypropylmethyl diethoxysilane, γ-glycidoxypropylmethyldipropoxysilane, γ-glycidoxypropylmethyldibutoxysilane, γ- glycidoxypropylmethyldiphenoxysilane, γ-glycidoxypropylethyldimethoxysilane, γ-glycidoxypropylethyl diethoxysilane, γ-glycidoxypropyl vinyldimethoxysilane, γ-glycidoxy- propyl vinyl diethoxysilane, γ-glycidoxypropyl-phenyl-dimethoxysilane, γ-glycidoxy-propyl-phenyl-diethoxysilane, ethyl-trimethoxysilane, ethyl triethoxysilane, vinyl trimethoxysilane, vinyl triacetoxysilane, vinyl trimethoxyethoxysilane, phenyl trimethoxysilane, phenyl triethoxysilane, phenyl triacetoxysilane, γ-chloropropyltrimethoxy- silane, γ-chloropropyltriethoxysilane, γ-chloropropyltriacetoxysilane, 3,3,3-trifluoropropyltrimethoxysilane, γ-methacryloxypropyltrimethoxysilane, γ-mercaptopropyltrimethoxysilane, γ- mercaptopropyl triethoxysilane, β-cyanoethyl triethoxysilane, chloromethyltrimethoxysilane, chloromethyltriethoxysilane, N- (N-aminoethyl) -? - aminopropyltrimethoxy-?

Ί *

-silane, N- (B-aminoethyl) γ-aminopropylmethyldimethoxysilane, γ-aminopropylmethyldimethoxysilane, N- (B-aminoethyl) γ-aminopropyltriethoxysilane, N- ( B-aminoethyl) -Y-aminopropylmethyl diethoxysilane, dimethyldimethoxysilane, phenylmethyldimethoxysilane, dimethyldiethoxysilane, phenylmethyldiethoxysilane, γ-chloropropylmethyl- dimethoxysilane, γ-chloropropylmethyl diethoxysilane, dimethyldiacetoxysilane, γ-methacryloxypropylmethyldimethoxysilane, γ-methacryloxypropylmethyl diethoxysilane, γ-mercaptopropylmethyl-dimethoxysilane, γ-mercaptopropyl-methyl-diethoxysilane, methyl-vinyl-dimethoxysilane, and methyl-vinyl-diethoxysilane.

Metal oxide colloidal particles are generally fine metal oxide particles having a particle size between 1 and 500 nm. A suitable example is the colloid of tungsten oxide particles (WO₃), zinc oxide (ZnO), silicon dioxide (SiO₂), aluminum oxide (AI₂SHE₃), titanium oxide (TiO₂), zirconium oxide (ZrO₂), tin oxide (SnO₂), beryllium oxide (BeO), or antimony oxide (Sb₂0s) colloids of particles. Mixtures of two or more of these may be used or may be used alone.

Execution examples

The invention will now be described in greater detail by the following examples, which, however, are not intended to limit the scope of the invention in any way.

The physical properties of the optical devices developed in the following examples, as well as the physical properties of the optical devices in the comparative examples, were evaluated as described below. The abbreviation pbw used is parts by weight.

-12• · *·/« ·* &lt;

(1) Light transmission and light reflectance

Light transmission (Y_T) and reflectivity (Y_R), as an example, was determined on both surfaces by an anti-reflection film coated plastic lens using a U-3410 spectrophotometer manufactured by Hitachi, Ltd.

(2) Film adhesion

Using a cutting tool, the surface layer of the plastic lens was cut to obtain 100 slices of 1 mm x 1 mm. Cellotape tape was applied to this sliced ​​area and then peeled off with a single motion. The remaining slices were counted and the film adhesion was expressed in the following table as the number of remaining slices per 100.

(3) Resistance to abrasion

The surface of the plastic lens was abraded with steel wool at 1 kg / cm² under pressure. After 20 abrasion cycles, the surface condition of the plastic lens was evaluated according to the following criteria:

UA: Slightly scratched.

A: Some thin scratches.

B: many thin and some thick scratches.

C: Lots of thin and thick scratches.

D: Peeled almost completely.

(4) Heat tolerance

The plastic lens was placed in a preheated oven at a preselected temperature and maintained for 1 hour. Different temperatures for this experiment • · »·&gt; · w *

- 13 was done, starting at 60 ° C in increments of 5 ° C. The temperature at which the lens was no longer resistant to heat treatment was measured and was approx. It broke after 1 hour. This temperature is the typical heat resistance in the following tables.

(5) Resistance to alkali metals

The plastic lens was immersed in 10% aqueous sodium hydroxide solution at 20 ° C for 1 hour, and its surface condition was evaluated according to the following criteria:

(JA: slightly changed.

A: Some peeling points.

B: many peeling points.

C: many peeled points and some peeled areas.

D: Peeled almost completely.

(6) Impact resistance

A plastic lens with a central thickness of 2 mm and a luminance of 0.00 was prepared and then subjected to a drop ball test according to the FDA. A '0' indicates a good result, while a 'x' indicates a poor result.

(7) Thickness of layers and films

The thickness of the niobium backing layer and the thickness of each sub-layer of the anti-reflection film were measured using λ = 500 nm light.

1st-12th EXAMPLES By weight units of colloidal silicon (Snowtex-40, manufactured by Nissan Chemical Industries, Ltd.), 81.6 parts by weight of methyl trimethoxysilane and 176 parts by weight of γ-glycidoxypropyltrimethoxysilane were used

As a compound of -14 · · ·, 2.0 units of 0.5 N hydrochloric acid, 20 units of acetic acid and 90 units of water were poured into a glass container and stirred for 8 hours at room temperature. The resulting solution was then allowed to stand at room temperature for 16 hours to obtain a hydrolyzed solution. To this solution were added 120 parts of isopropyl alcohol, 120 parts by weight of n-butyl alcohol, 16 parts by weight of aluminum acetylacetone, 0.2 parts by weight of silicon surfactant and 0.1 parts by weight of UV-absorber. The mixture was stirred at room temperature for 8 hours and then aged at room temperature for 24 hours to obtain a coating solution.

A plastic lens (made from diethylene glycol bisallyl carbonate and having a refractive index of 1.50, a central thickness of 2.0 mm and a brightness of 0.00) was pretreated with an aqueous basic solution and immersed in the coating solution. After full immersion, the plastic lens was removed at a rate of 20 cm / min. Subsequently, the plastic lens was heated to 120 ° C for 2 hours to obtain a hardened film.

Subsequently, the resulting plastic lens was subjected to ion-gun treatment by ion-beam deposition! using an argon gas such that the ionic accelerator voltage and exposure time were shown in Tables 1-6 and thus a hardened hard coating layer (hereinafter referred to as Layer A) was obtained.

Thereafter, Tables 1-7 show Tables 1-7. formed a sub-layer film layer and a base layer on the hard A coating layer,

-15 ion beam separation! under the conditions shown in Tables 1-6 to obtain a plastic lens.

The lenses were evaluated according to the procedures indicated by numbers (1) to (7) above, and the results are shown in Tables 1-6.

1st-4th Comparative examples

Plastic lenses were formed in the same manner as in Examples 1 to 12 except that the base layer was not formed and the hard coating layer and the film layer shown in Examples 1-7 were formed. made up of layers, not ion beam separation! method, but also by steaming.

Plastic lenses were evaluated according to procedures (1) to (6) above, and the results are shown in Tables 7 and 8.

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As in Figures 1-6. Tables 1-12. The plastic lenses of Examples 1 to 4 have a particularly low reflectance of 0.68-0.82% and a very high light transmittance ranging from 99.0 to 99.3%. In addition, their films had good adhesion, abrasion resistance, heat resistance, alkali metal resistance and impact resistance.

In contrast, Figs. plastic lenses according to the Comparative Examples had very high light transmittance, i.e., 1.1 to 1.2%, and very low light transmittance, which means 98.6 to 98.7%, as shown in Tables 7 and 8. also stands out. In addition, their film adhesion, abrasion resistance, heat resistance, alkali metal resistance, and impact resistance were below those of Examples 1-12.

As described in more detail above, the optical device of the present invention has a low reflectivity and high light transmission antireflection film, and exhibits excellent adhesion between the plastic substrate and the antireflection film, as well as excellent abrasion resistance, heat resistance, and resistance to alkali metals. and impact resistance.