U.S. patent application number 11/225317 was filed with the patent office on 2006-01-19 for radiation-curable anti-reflective coating system.
Invention is credited to Liu He, Sung-Soon Park, Grace Tang, Aylin Vance, Haixing Zheng.
Application Number | 20060014101 11/225317 |
Document ID | / |
Family ID | 21697091 |
Filed Date | 2006-01-19 |
United States Patent
Application |
20060014101 |
Kind Code |
A1 |
He; Liu ; et al. |
January 19, 2006 |
Radiation-curable anti-reflective coating system
Abstract
A radiation-curable anti-reflective coating is disclosed. The
coating may be deposited on a substrate by spinning, dipping or
rolling. The anti-reflective coating may have two layers in which
case the anti-reflective coating has a V-shaped reflectance pattern
in the visible wavelength spectrum. The anti-reflective coating may
have three layers in which case the anti-reflective coating has a
broadband reflectance pattern in the visible wavelength
spectrum.
Inventors: |
He; Liu; (Pleasanton,
CA) ; Park; Sung-Soon; (Los Angeles, CA) ;
Zheng; Haixing; (Oak Park, CA) ; Tang; Grace;
(Sylman, CA) ; Vance; Aylin; (Reseda, CA) |
Correspondence
Address: |
BLAKELY SOKOLOFF TAYLOR & ZAFMAN
12400 WILSHIRE BOULEVARD
SEVENTH FLOOR
LOS ANGELES
CA
90025-1030
US
|
Family ID: |
21697091 |
Appl. No.: |
11/225317 |
Filed: |
September 12, 2005 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
|
|
10001639 |
Oct 31, 2001 |
6942924 |
|
|
11225317 |
Sep 12, 2005 |
|
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Current U.S.
Class: |
430/270.1 |
Current CPC
Class: |
Y10T 428/31612 20150401;
Y10T 428/31645 20150401; Y10T 428/31507 20150401; G02B 1/111
20130101 |
Class at
Publication: |
430/270.1 |
International
Class: |
G03C 1/492 20060101
G03C001/492 |
Claims
1. A method comprising: depositing a plurality of layers on a
substrate, at least one of which comprises a radiation-curable
material; and curing at least one deposited layer by exposure to a
radiation source.
2. The method of claim 1, wherein the plurality of layers comprises
at least two layers, and relative to one another, a first layer has
a high refractive index and a second layer has a low refractive
index.
3. The method of claim 1, wherein the plurality of layers comprises
at least three layers, and relative to one another, a first layer
has a medium refractive index, a second layer has a high refractive
index and a third layer has a low refractive index.
4. The method of claim 1, wherein the radiation source comprises an
electron beam.
5. The method of claim 1, wherein the radiation source comprises
ultraviolet light.
6. The method of claim 1, wherein depositing a plurality of layers
on a substrate comprises one of a spinning process, a dipping
process, and a rolling process.
7. The method of claim 1, wherein depositing a plurality of layers
comprises depositing a radiation-curable layer of at least one
acrylic monomer.
8. The method of claim 7, wherein the radiation-curable layer
comprises at least one (meth)acrylate monomer and a silicon
compound.
Description
CROSS-REFERENCE TO RELATED APPLICATION
[0001] The application is a Divisional of co-pending U.S. Pat.
Application Ser. No. 10/001,639, filed Oct. 31, 2001.
BACKGROUND
[0002] 1. Field of the Invention
[0003] The invention relates to coating compositions and more
particularly to the radiation curable coating compositions.
[0004] 2. Description of Related Art
[0005] Uncoated, optically transparent plastic and glass substrates
such as ophthalmic lenses and cathode ray tube (CRT) screens
reflect a portion of incident light. The amount of reflection
varies with the wavelength, polarization, and angle of incidence of
the light as well as the wavelength-dependent refractive index, n,
of the material. Usually, the light loss reflected from the
surfaces of uncoated substrates is on the order of about seven
percent. Significantly more light loss occurs in transparent
substrates having a high refractive index (e.g., refractive index
on the order of 1.55 or higher).
[0006] One method for reducing light reflection from optically
transparent substrates is to coat the surfaces of the substrates
with anti-reflective coatings. As described in Optical Thin Films
User's Handbook by James D. Rancourt, Macmillan Publishing Company,
1987, there are two common anti-reflective coating designs. One is
the double layer structure of a first or bottom layer having a high
refractive index and a second or top layer having a low refractive
index with the corresponding thickness of quarter and quarter
wavelength. The second anti-reflective coating design is the three
layer structure of a first or bottom layer having a middle
refractive index, a second or middle layer having a high refractive
index, and a third or top layer having a low refractive index with
the corresponding thickness of quarter, half, and quarter
wavelength, respectively. The double layer anti-reflective coating
has a V-shape pattern of reflectance in the visible wavelength
spectrum, while the three layer anti-reflective coating has a
broadband pattern of reflectance in the visible wavelength
spectrum. The materials used for such anti-reflective coatings
include oxides, nitrides, and fluorides of silicon (Si), titanium
(Ti), aluminum (Al), zirconium (Zr), ashmony (Sb), boyillium (Be),
bismuth (Bi), cerium (Ce), magnesium (Mg), hafnium (Hf), lanthanum
(La), prascodymium (Pr), tantalum (Ta), etc. Numerous
anti-reflective coating systems have been disclosed in the U.S.
Pat. No. 4,130,672; U.S. Pat. No. 4,172,156; and U.S. Pat.
No.5,172,812. The anti-reflective coatings in these documents are
generally applied on transparent substrates primarily by a vacuum
deposition processes, such as evaporation and sputtering. Although
vacuum deposition techniques produce high quality anti-reflective
coatings, they suffer from high cost limits in small optical
laboratories.
[0007] Non-vacuum cost-effective coating processes, such as
solution coating, have been developed to replace vacuum deposition
processes. Solution coating processes are disclosed in the U.S.
Pat. No. 4,361,598; U.S. Pat. No. 4,966,812; U.S. Pat. No.
5,476,717; U.S. Pat. No. 5,580,819; and U.S. Pat. No. 5,858,526.
Such anti-reflective coatings made by a coating solution process
generally must be cured for a certain amount of time at high
temperature (e.g., up to 300.degree. C. or even higher
temperatures) to get enough hardness to be suitable. This high
curing temperature and long curing process limits the application
of the anti-reflective coatings only to glass substrates which are
generally not deformed during thermal curing at high temperature.
Plastic substrates, such as ophthalmic lenses, are easily deformed
or burned at temperatures up to 300.degree. C.
[0008] Radiation curing is used in the coating industry. Under high
energy radiation such as ultraviolet (UV) light or electron beam
radiation, the monomer-containing solution polymerizes to form a
hard layer. UV-curable monomer-containing coating formulations
typically contain a photoinitiator which starts the polymerization
reaction of the monomers under UV light. Following radiation
curing, the coatings become hard and have good chemical resistance.
Compared with thermal curing processes, radiation curing processes
have more economic advantages such as fast cure of a few seconds,
less heat generation, and low energy consumption. Radiation-curable
compositions for abrasion and scratch resistant coatings are
disclosed in the U.S. Pat. No. 3,989,609; U.S. Pat. No. 6,165,564;
U.S. Patent No. 6,228,433; U.S. Pat. No. 6,232,360; and U.S. Pat.
No. 6,241,505.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] FIG. 1 is a schematic cross-sectional side view of an
anti-reflective coating having a stack of at least two layers on a
substrate.
[0010] FIG. 2 is a schematic cross-sectional side view of an
anti-reflective coating having a stack of at least three layers on
a substrate.
[0011] FIG. 3 is a diagram of the reflectance of the ophthalmic
lens without an anti-reflective coating and with an ultraviolet
(UV)-cured anti-reflective coating.
DETAILED DESCRIPTION
[0012] An apparatus comprising a substrate having a coating
composition formed thereon is disclosed. In one embodiment, the
coating composition comprises a plurality of layers at least one of
which is a radiation-curable layer. The coating composition is
suitable for coating transparent substrates such as glass and
plastics, especially ophthalmic lenses. Such a coating composition
may be selected to have a variety of different reflectance patterns
in visible wavelengths. One reflectance pattern is a V-shape
indicating a relatively narrow reflectance band and another pattern
has broader reflectance pattern. Generally speaking, a V-shaped
reflectance pattern describes a reflectance pattern that minimizes
reflectance of light (e.g., visible light) at a particular
wavelength or around a particular wavelength, for example, at or
around 550 nanometers (nm). A broader reflectance pattern describes
a reflectance pattern that minimizes reflectance of light among a
range of wavelengths (e.g., 450 nm to 650 nm). It is appreciate
that with the techniques described herein for forming
anti-reflective coatings, the V-shape and the broadband shape are
optimizable for particular wavelengths or ranges of wavelengths by,
for example, modifying the refractive index and thickness of the
deposited layers that make-up the coatings.
[0013] The V-shape anti-reflective coating composition described
herein may be comprised of two layers: one having, relative to the
other, a high refractive index and the other having a low
refractive index. One arrangement of the layers is the high
refractive index layer covered (coated) with the low refractive
index layer. A broadband anti-reflective coating, in one
embodiment, may be composed of three layers: one or a first layer,
for example, closest to the transparent substrate having, relative
to the other layers, a medium refractive index, the one above it,
or a second layer having a higher refractive index, and the top or
third one having a low refractive index.
[0014] FIG. 1 shows a schematic, cross-sectional view of an
apparatus comprising a substrate having a coating composition
formed thereon. The coating composition, in this embodiment, is
formed of a plurality of deposited layers at least one of which
comprises a radiation-curable (e.g., ultraviolet curable,
electron-beam radiation curable, etc.) material. FIG. 1 shows
apparatus 100 including a substrate with two deposited layers
selected to have a V-shape (or single) reflectance pattern in the
visible wavelength spectrum.
[0015] Referring to FIG. 1, in one embodiment, substrate 110 is an
organic polymer (e.g., plastic), glass, ceramic, or metal material.
In one embodiment, substrate 110 is a transparent material such as
an organic polymer or glass. Optionally formed over a surface of
substrate 110 (in FIG. 1, a superior surface) is hardcoat layer 115
of a material that may be known in the industry. One suitable
material for hardcoat layer 115 is polysiloxane.
[0016] Overlying a surface of substrate 110 (e.g., a superior
surface as shown) and optional hardcoat layer 115 is first
deposited layer 120. First deposited layer 120, in one example, is
selected to have a relatively high index of refraction (e.g.,
relative to a subsequent layer). In one embodiment, first deposited
layer 120 is a colloid material of a metal compound, including, but
not limited to, metal oxides, metal carbides, and metal nitrides
combined/modified with a condensation product of an organosilane
(e.g., tetramethoxysilane). Suitable metal oxides include, but are
not limited to, aluminum oxide (Al.sub.2O.sub.3), titanium oxide
(e.g., TiO.sub.2), zinc oxide, and iron oxide. Suitable metal
carbides include, but are not limited to, titanium carbide.
Suitable metal nitrides include, but are not limited to, titanium
nitride. The metal compounds are preferably crystalline powders
made, for example, by vacuum processes or wet processes. Through,
for example, a grinding process, the particles are selected to have
a particle size suitable for forming a transparent layer or film.
One particle size is less than one micron and on the order of one
hundred to several hundred nanometers.
[0017] The concentration of the colloids are preferably controlled
between 10 and 20 weight percent. The colloidal coating solutions
that are used to form first deposited layer 120 are made by
dispersing the metal compound particles (combined/modified with a
condensation product of an organosilane) with a dispersing agent
such as an amide-based dispersing agent, e.g., dimethylformamide,
and subsequently, diluting the concentrated colloids to 1 to 5
weight percent with solvents. Suitable solvents are those that do
not destroy the colloidal properties of the colloid, such as
alcohols and water.
[0018] The refractive indices of the layers made of the colloids
may be adjusted by varying the amount of organosilanes contained
therein. The organosilanes used for modification of the metal
oxides, nitrides, or carbides include, but are not limited to,
organosilanes such as tetraalkoxysilane, trialkoxysilane or
dialkoxysilane. Organosilanes tend to reduce the refractive index
of the colloidal particles. In general, the greater the quantity of
organosilanes in the surface of the colloidal particles, the lower
refractive index of the layer. In one embodiment, first deposited
layer 120 of a V-shape anti-reflective coating has a refractive
index that varies, in one example, from 1.45 to 1.75 (e.g.,
relatively high refractive index).
[0019] In one example, first deposited layer 120 of, for example, a
colloid is introduced by a spinning process. Spinning continues for
about one minute to form a stable layer over a surface of substrate
110 having a thickness on the order of 50 to 150 nm (e.g., 90
nm).
[0020] Referring to FIG. 1, overlying first deposited layer 120 on
substrate 110 is second deposited layer 130. In an embodiment where
apparatus 100 of FIG. 1 is selected to have a. V-shape reflectance
band (and first layer 120 is selected to have a relatively high
index of refraction (e.g., 1.45 to 1.75) over a transparent
substrate), second deposited layer 130 is selected to have a
relatively low refractive index, on the order of 1.30 to 1.50.
[0021] Selected material for second deposited layer 130 is a
radiation-curable material. Acrylate monomers, preferably
multi-functional (meth)acrylate monomers can be used as binders of
the top layer. Any multifunctional (meth)acrylate can be used as
long as the selected monomer does not create stability ("gelling")
or viscosity problems of the corresponding coating solution. In
order to make a hard anti-reflective coating, however, it is
desired that second deposited layer 130 composition include at
least one multifunctional (meth)acrylate monomer that has a
functionality of at least three. Typical (meth)acrylates include,
but are not limited to, propoxylated trimethylolpropane triacrylate
(CD 501, SARTOMER), ethoxylated trimethyolpropane triacrylate
(SR-502, SARTOMET), highly propoxylated (5.5) glyceryl triacrylate
(CD9021, SARTOMER), ethoxylated trimethlolprone triacrylate
(SR-454HP, SARTOMER), dipentaerythritol pentaacrylate (SR 399,
SARTOMER). Among the acrylates, dipentaerythritol pentaacrylate (SR
399), propoxylated trimethylolpropane triacrylate (CD 501),
glyceryl triacrylate (CD9021) are preferred. These monomers may be
used alone. However, to adjust the refractive index, hardness and
adhesion of the layer, it is preferred to employ two or more
monomers. In one embodiment, the composition of second deposited
layer 130 contains one to ten weight percent of multifunctional
(meth)acrylate monomers, preferably, three to six weight percent of
the multifinctional (meth)acrylate monomers.
[0022] In one embodiment, the monomers polymerize without catalysis
under electron beam irradiation. In another embodiment, a
photoinitiator may be included into the top coating solution to
initiate or catalyze the polymerization reaction of the monomers
when they are placed under ultraviolet (UV) light radiation. In one
embodiment, the top coating compositions contain on the order of
about 10 percent by weight of a photoinitiator. In another
embodiment the top coating composition contains preferably 0.5 to 5
percent by weight photoinitiator.
[0023] In one embodiment, suitable photoinitiators used include,
but are not limited to, 2-butoxy-1,2 diphenylethanone,
2,2-dimethoxy-1,2-diphenylethanone and 2,4,6-trimethylbenzophenone,
benzophenone, hydroxycyclohexyl phenylketone, acetophenone,
acenaphthenequinone, o-methoxy benzophenone, thioxanthen-9-one,
xanthen-9-one, 7H-Benz(de)anthracen-7-one, dibenzosuberone,
1-naphthaldehyde, 4,4'-bis(dimethylamino) benzophenone,
fluorine-9-one, 1'-acetonaphthane anthraquinone, 1-indanone,
2-tertbutylanthraquinone, valerophenone, hexanophenone,
3-phenylbutyrophenone, p-morpholinopropiophenone,
4-morpholinobenzophenone, p-diacetyl-benzene, 4-amino-benzophenone,
4'methoxyacetophenone, benzaldehyde, 9-acetylphenanthrene,
2-acetylphenanthrone, 10-thioxanthenone, 3-acetylphenanthrene,
3-acetylindole, 1,3,5-triacetylbenzene and like, including blends
thereof. In one embodiment, the photoinitiators, 2-butoxy-1,2
diphenylethanone, 2,2-dimethoxy-1,2-diphenylethanone,
2,4,6-trimethylbenzophenone, and benzophenone are preferable.
[0024] In another embodiment, other additives, such as
fluoroalkyl-containing compounds, may be incorporated into the
formulation of second deposited layer 130. It is believed that
fluoroalkyl-containing compounds tend to decrease the refractive
index of the top layer. Suitable fluoroalkyl-containing compounds
are the polycondensed products of a mixture of alkoxysilanes. In
one embodiment, the mixture may be, but is not limited to,
tetraethoxysilane or tetramethoxysilane, and a trialkoxysilane or
dialkoxysilane having a perfluoroalkyl group containing from 3 to
20 carbon atoms. The chemical structure of a trialkoxysilane is
representatively given as follows:
C.sub.xF.sub.2x+1Si(OR).sub.3
[0025] wherein R represents, in one example, a lower C1-C4 alkoxy
group selected from the group consisting of methoxy, ethoxy,
isopropoxy and n-butoxy, and x varies from 3 to 20.
[0026] In one embodiment, the fluoroalkyl-containing silicon
compounds are prepared in such a manner that the mixture of the
tetraalkoxysilane and the trialkoxysilane or dialkoxysilane having
a perfluoroalkyl group is hydrolyzed with water in a single or
mixed alcoholic solvent, and then polycondensed. An acid, such as
nitric acid, may be added into the mixture before hydrolysis to act
as a catalyst. In one embodiment, the hydrolysis and
polycondensation reaction may run at 30-50.degree. C. for 10-20
hours. The polycondensed fluoroalkyl-containing silicon compound is
then added into the second deposited layer 130 formulation, wherein
the solid content of the fluoroalkyl-containing silicon compound
may be at least 0.5 percent by weight. In another embodiment, the
solid content of the fluoroalkyl-containing silicon compound may be
2 percent by weight.
[0027] A solvent may further be added into the formulation of
second deposited layer 130. The solvent for the top coating
composition may be a mixture of an alcohol solvent having a lower
boiling point, such as C1-C4 alcohol (methanol and ethanol being
preferred), a ketone such as methyl ethyl ketone and methyl propyl
ketone, and a viscous solvent having higher boiling point, such as
ethylene glycol monomethyl ether and ethylene glycol.
[0028] In one example, second deposited layer 130 is introduced by
a spinning process. Spinning continues for about one minute to form
a stable layer having a thickness on the order of 50 to 150 nm
(e.g., 100 nm). Following deposition, the composite structure may
be cured to harden the deposited layers, particularly second
deposited layer 130. In one embodiment, the cure is accomplished by
exposing apparatus 100 to a radiation source such as an UV or
e-beam radiation source (dependent, to an extend on the material
selected for second deposited layer 130).
[0029] In one embodiment, shown in FIG. 1, the composite structure
(apparatus 100) has an anti-reflective property. The composite
structure is formed of a substrate (e.g., substrate 110) of, for
example, a transparent material. Overlying substrate 110 (and
optional hard coat layer 115) is first deposited layer 120 and
radiation-curable second deposited layer 130. In an embodiment
where the composite structure has a V-shape reflectance pattern in
the visible wavelength spectrum, first deposited layer 120 is
selected to have a relatively high refractive index (relative to
the individual layers) of, for example, 1.45 to 1.55. Overlying
first deposited layer 120 is second deposited layer 130 of, for
example, a radiation curable material having a relatively low
refractive index on the order of 1.30 to 1.50.
[0030] FIG. 2 shows a schematic, cross-sectional view of an
apparatus comprising a coating composition formed thereon. In this
example, the coating composition is selected to have a broadband
reflectance pattern in the visible wavelength spectrum.
[0031] Referring to FIG. 2, apparatus 200 includes substrate 210 of
an organic polymer (e.g., plastic), glass, ceramic or metal
materials. In one example, substrate 210 is a transparent material
such as an organic polymer or glass.
[0032] Optionally formed over a surface of substrate 210 (in FIG.
2, a superior surface) is hardcoat layer 215 such a polysiloxane.
Overlying optional hardcoat layer 215 is first deposited layer 220.
In one embodiment, first deposited layer 220 is a colloid of a
metal compound (e.g., metal oxide, metal nitride, metal carbide,
etc.) combined/modified with an organosilane (e.g.,
tetraoxysilane). In this regard, the material of first deposited
layer 220 is similar to the first deposited layer 120 of FIG. 1. In
one embodiment, the refractive index of first deposited layer 220
is selected to be on the order of 1.45 to 1.55. The refractive
index may be adjusted by varying the amount of organosilanes
contained in the coating solution used to form first deposited
layer 220. The concentration of the colloids in the coating
solution are preferably controlled between 10 and 20 weight percent
and the coating solution may be made by diluting the concentrated
colloids with solvents on the order of one to five weight
percent.
[0033] The coating solution used to form first deposited layer 220
may be introduced by a spinning process, continuing for about one
minute, to form a layer having a thickness on the order of 50to
150nm.
[0034] Overlying first deposited layer in the structure (apparatus
200) of FIG. 2 is second deposited layer 230. In one embodiment,
second deposited layer 230 is also formed from a colloid
composition combined/modified with a condensation product of
organosilanes. In the example of forming a composite coating (of
three deposited layers and a broadband spectrum), second deposited
layer 230 is selected to have a refractive index on the order of
1.50 to 1.75. Like first deposited layer 220, second deposited
layer 230 may be formed from a coating solution introduced, in one
example, by spinning (for about one minute) to a thickness on the
order of 90 to 200 nm.
[0035] Overlying second deposited layer 230 in the structure
(apparatus 200) shown in FIG. 2 is third deposited layer 240. In
one example, third deposited layer 240 is selected to be a
radiation-curable (e.g., e-beam or UV curable material) similar to
second deposited layer 130 described with reference to FIG. 1 and
the accompanying text. Multi-functional acrylate monomers (e.g.,
(meth)acrylate monomers), possibly two or more combined with a
photoinitiator (e.g., in the case of UV curable monomers) and
possibly containing additives, such as fluoro-alkyl-containing
additives, are suitable. Third deposited layer 240 is selected, in
an example of forming a composite coating (of three deposited
layers), to have a refractive index on the order of 1.30 to 1.50. A
coating solution may be introduced by spinning onto the surface of
substrate 200 (e.g., the superior surface) to a thickness on the
order of 50 to 150 nm.
[0036] FIG. 3 shows a representative example of the reflectance of
an ophthalmic lens without an anti-reflective coating and with a UV
curable anti-reflective coating selected to have a broadband
reflectance in the visible spectrum similar to the three layer
coating described above with reference to FIG. 2 and the
accompanying text.
[0037] In the above examples, the composite structures are
described as including a plurality of layers on a substrate. It is
appreciated that the individual layers thought possibly distinctly
deposited, do not necessarily overlie one another with a distinct
interface between each layer. Instead, particularly with spin
operations, the plurality of layers may blend together to some
extent.
[0038] The method described above to form a composite substrate is
a relatively inexpensive, generally simpler method compared to
prior techniques as it eliminates the need for expensive
evaporators or plasma equipment. The formulating of the deposited
layer materials do not require complex or expensive equipment.
Simple film application techniques, including spinning, dipping,
rolling, or spraying permit the coating of large complicated
shapes, and even simultaneous coating of the inner and outer
surfaces of a tube. The large scale application of a surface
coating is possible without a limit on the size of the part to be
coated. As noted above, there are many prior art anti-reflective
surface coatings applied to vitreous substrates. However, the
method described above and the materials selected eliminate the
necessity to heat and/or etch the coating to produce an
anti-reflecting film on a substrate.
[0039] The composite coating of the invention is particularly
useful for coating various substrates such as glass, ceramics,
metals, and organic polymeric materials to increase light
transmission, without a need to subject the coating or the
substrate to high temperature curing processes. Substrates coated
with the coating of the invention may be used, for example, in
ophthalmic lenses, display filters and solar photovoltaic
applications.
[0040] Having been generally described, the following example
describes a particular embodiment, to illustrate some of the
properties and demonstrate the practical advantages thereof, and to
allow one skilled in the art to utilize the invention. It is
understood that these examples are to be construed as merely
illustrative.
EXAMPLE 1
[0041] In one embodiment, the antireflection coating may be
fabricated as follows.
[0042] 1) The Preparation of Coating Composition of the First Layer
with Medium Refractive Index.
[0043] 350 grams of tetraethoxysilane (TEOS) was dropped into water
based 20 weight percent TiO.sub.2 colloid during stirring. The
mixture was then stirred at 70 degree C. for 5 hours. The mixture
was dried at 150 degree C. for 6 hours to get SiO.sub.2-modified
TiO.sub.2 powder. The powder was crystallized at 700 degree C. for
2 hours. The powder was then dispersed into colloid by grinding.
The solid content of the SiO.sub.2 modified TiO.sub.2 colloid was
controlled from 10 to 20 weight percent. The colloid was diluted
into 1 to 5 weight percent with the solvent mixture of methanol,
ethanol, methyl ethyl ketone, and ethylene glycol.
[0044] 2) The Preparation of the Coating Composition of the Second
Layer with High Refractive Index.
[0045] The preparation of coating composition of the first layer
was repeated except that less amount of tetraehoxysilane was added
into the TiO.sub.2 colloid. 120 gram of tetraethoxysilane (TEOS)
was dropped into 3370 gram of TiO.sub.2, colloid.
[0046] 3) Preparation of the UV-Curable Coating Composition of the
Top Layer with Low Refractive Index.
[0047] The polycondensed fluorine-containing silicon compounds are
prepared as follows:
[0048] 25 grams of (tridecafluoro-1,1,2,2-tetrahydrooctyl)
triethoxysilane was mixed with 100 grams of tetraethoxysilane
(TEOS) and 90 grams of HNO.sub.3 aqueous solution (containing 1
gram HNO.sub.3). The mixture was left in a closed glass container
at 50.degree. C. for 12 hours and then cooled slowly to room
temperature. The product was named as FCSC and kept in a
refrigerate prior to use. The following ingredients were added in
the sequence listed to a plastic container and were mixed gently
for 20 minutes. TABLE-US-00001 FCSC 5 grams Methanol 10 grams
ethylene glycol monomethyl ether 40 grams Dipentaerythritol
pentaacrylate (SR-399, Sartomer) 3.5 grams Highly propoxylatd
glyceryl triacrylate 2.5 grams (SR-9021, Sartomer) Finally other
two ingredients were added into the mixture:
2,4,6-trimethylbenzophenone 0.5 grams Eethylene glycol monomethyl
ether 20 grams
[0049] The resulting product was mixed to form a transparent
UV-curable composition for the top layer.
[0050] 4) Application and Curing of an Anti-Reflective Coating on
an Ophthalmic Lens.
[0051] The coating solution for first layer was injected on the
front side of the polycarbonate ophthalmic lens during spinning the
lens with the speed of 500 to 1500 RPM and then the coated lens was
spun more for 1 minute to stabilize the first layer. Without
interruption the coating solution for second layer was injected on
the surface of the first layer during spinning the lens with the
speed of 500 to 1500 RPM and then the coated lens was spun more for
1 minute to stabilize the second layer. Finally the coating
solution for top layer was injected on the surface of the second
layer during spinning the lens with the speed of 500 to 1500 RPM
and then the coated lens was spun more for 1 minute to stabilize
the top layer. The coated lens was cured for 30 seconds with the UV
(ultraviolet) light of a medium pressure mercury. The coating
process for the front side of the lens was repeated to apply
coatings on the backside of the lens. FIG. 2 shows the reflectance
pattern of the ophthalmic lens with the invented UV
(ultraviolet)-cured anti-reflective coating. The reflectance of the
coated lens was broad and less than 2 percent in the visible
wavelength.
[0052] In the preceding detailed description, the invention is
described with reference to specific embodiments thereof. It will,
however, be evident that various modifications and changes may be
made thereto without departing from the broader spirit and scope of
the invention as set forth in the claims. The specification and
drawings are, accordingly, to be regarded in an illustrative rather
than a restrictive sense.
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