CN114959591A - Substrate vacuum dyeing method, dyed substrate and glasses - Google Patents
Substrate vacuum dyeing method, dyed substrate and glasses Download PDFInfo
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- CN114959591A CN114959591A CN202210526323.9A CN202210526323A CN114959591A CN 114959591 A CN114959591 A CN 114959591A CN 202210526323 A CN202210526323 A CN 202210526323A CN 114959591 A CN114959591 A CN 114959591A
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- 239000000758 substrate Substances 0.000 title claims abstract description 226
- 238000004043 dyeing Methods 0.000 title claims abstract description 123
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000011521 glass Substances 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 101
- 239000010410 layer Substances 0.000 claims abstract description 67
- 230000001681 protective effect Effects 0.000 claims abstract description 56
- 238000001771 vacuum deposition Methods 0.000 claims abstract description 38
- 239000011241 protective layer Substances 0.000 claims abstract description 37
- 238000002834 transmittance Methods 0.000 claims abstract description 32
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910000484 niobium oxide Inorganic materials 0.000 claims abstract description 28
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 28
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000004140 cleaning Methods 0.000 claims abstract description 27
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000001704 evaporation Methods 0.000 claims description 15
- 230000008020 evaporation Effects 0.000 claims description 13
- 150000002500 ions Chemical class 0.000 claims description 13
- 239000004677 Nylon Substances 0.000 claims description 3
- -1 acryl Chemical group 0.000 claims description 3
- 229920001778 nylon Polymers 0.000 claims description 3
- 229920000515 polycarbonate Polymers 0.000 claims description 3
- 239000004417 polycarbonate Substances 0.000 claims description 3
- 238000007740 vapor deposition Methods 0.000 claims description 2
- 239000010408 film Substances 0.000 description 13
- XUIMIQQOPSSXEZ-NJFSPNSNSA-N silicon-30 atom Chemical compound [30Si] XUIMIQQOPSSXEZ-NJFSPNSNSA-N 0.000 description 8
- 238000001228 spectrum Methods 0.000 description 6
- 238000005336 cracking Methods 0.000 description 4
- 239000003086 colorant Substances 0.000 description 3
- 230000002950 deficient Effects 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/081—Oxides of aluminium, magnesium or beryllium
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/10—Glass or silica
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/113—Anti-reflection coatings using inorganic layer materials only
- G02B1/115—Multilayers
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- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Inorganic Chemistry (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The invention relates to a substrate vacuum dyeing method, a dyed substrate and glasses, wherein the substrate vacuum dyeing method comprises the following steps: s1, cleaning and drying the substrate to obtain a clean substrate; s2, baking the clean substrate to obtain a baked substrate; s3, placing the baked substrate on a jig, feeding the baked substrate into a vacuum coating machine chamber, vacuumizing the chamber, bombarding a protective material by using an electron gun, wherein the protective material is a mixture of silicon oxide and aluminum oxide, and forming an inner protective layer on the surface of the baked substrate; s4, bombarding a dyeing material by using an electron gun, wherein the dyeing material is a mixture of titanium oxide and niobium oxide, and a dyeing layer is formed on the surface of the inner protection layer; and S5, bombarding the protective material by adopting an electron gun, and forming an outer protective layer on the surface of the dyeing layer. The transmittance of the vacuum color substrate is adjustable, the grading requirement of the substrate is met, meanwhile, the substrate has uniform color, the yield is high, and the subsequent diversified processing requirement can be met.
Description
Technical Field
The invention relates to a preparation method of a lens substrate, in particular to a substrate vacuum dyeing method, a dyed substrate and glasses.
Background
The lens is widely used in life and production as an optical element. The lens is usually improved on a substrate based on the function difference, and the common substrate is made of glass, nylon, polycarbonate, acrylic and other materials.
In order to make the lens have different colors, a colored substrate needs to be used for improvement, and the existing method is to introduce toner during substrate manufacturing to obtain a dyed substrate, however, the compatibility of the toner and different substrate materials is different, and all substrates cannot be used.
Patent application CN107011500A discloses a photochromic substrate material, which comprises the following components in parts by mass: epoxy compounds: 50-70 parts; polyether polyol compounds: 30-40 parts; catalyst: 1-5 parts; releasing agent: 0.08-0.1 part; color changing powder: 0.03-0.05 part. The substrate is a polyester color-changing substrate, but the materials such as glass, acrylic and the like are not suitable.
Disclosure of Invention
The invention aims to overcome the problems in the existing color substrate preparation, and provides a substrate vacuum dyeing method which can be suitable for substrates of different materials to obtain target colors, simultaneously meets the corresponding transmittance requirement, can replace the existing dyed substrates, and can be used for strengthening, plating functional films and the like.
Conventional vacuum coating is to form a film layer with specific functions, such as an anti-reflection layer, an infrared ray resistant layer, a blue light resistant layer, etc., on a substrate, and the vacuum coating layer is usually colorless. There is also a colored functional layer, but this sheet is not suitable as a substrate because the substrate has a requirement for transmittance, which is greater than 80% in terms of transmittance, including 0 grade; grade 1, the transmittance is 43-80%; grade 2, the transmittance is 18-43%; grade 3, 8-18% of transmittance, and grade 4, less than 8% of transmittance. The existing effect layer cannot meet the requirement of transmittance grading.
The invention forms the dyeing substrate with specific color by evaporating the dyeing material under the vacuum condition. Conventional (B) isThe organic dyeing material is not high temperature resistant, has unstable performance after being bombarded by an electron gun, and cannot form a stable film layer. Conventional vacuum coating materials such as SiO 2 、MgF 2 、Ti 3 O 5 、ZrO 2 And the problem that the base color is transparent exists, and the requirement of the substrate on various colors cannot be met. For example, although the requirement of 2 to 3 levels of transmittance can be satisfied by evaporating a metal material under vacuum conditions, the metal film layer has poor deformability and is easily subjected to stress at high temperature, and thus film cracking easily occurs.
The invention adopts the mixture of titanium oxide and niobium oxide, obtains the specific substrate color by adjusting the proportion of the titanium oxide and the niobium oxide and the thickness of the film layer, and simultaneously meets the requirement of graded change of transmittance. The transmittance of the tawny lens can be distributed in 1 and 2 grades; the transmission of the gray substrate can be distributed in 2 and 3 grades; the transmittance of the black matrix can be distributed between 3 and 4 levels.
Specifically, when the content of titanium oxide in the dyeing material is 25-45 wt%, the content of niobium oxide is 55-75 wt%, and the thickness of the formed dyeing layer is 500-2000 angstroms, the brown substrate is obtained. Preferably, the content of titanium oxide is 30-40 wt%, the content of niobium oxide is 60-70 wt%, and the thickness of the formed dyed layer is 1300-1900 angstroms.
When the content of titanium oxide in the dyeing material is 15-35 wt%, the content of niobium oxide is 65-85 wt%, the thickness of the formed dyeing layer is 2050-3500 angstrom, and a gray substrate is obtained. Preferably, the content of titanium oxide is 20-30 wt%, the content of niobium oxide is 70-80 wt%, and the thickness of the formed dyeing layer is 2300-3300 angstroms.
When the content of titanium oxide in the dyeing material is 5-25 wt%, the content of niobium oxide is 75-95 wt%, and the thickness of the formed dyeing layer is 3550-5000 angstroms, the black substrate is obtained. Preferably, the content of titanium oxide is 10-20 wt%, the content of niobium oxide is 80-90 wt%, and the thickness of the formed dyed layer is 3800-4500 angstroms.
The specific scheme is as follows:
a method of vacuum dyeing a substrate comprising the steps of:
s1, cleaning and drying the substrate to obtain a clean substrate;
s2, baking the clean substrate to obtain a baked substrate;
s3, placing the baked substrate on a jig, sending the baked substrate into a vacuum coating machine chamber, vacuumizing, bombarding a protective material by using an electron gun, wherein the protective material is a mixture of silicon oxide and aluminum oxide, and forming an inner protective layer on the surface of the baked substrate;
s4, bombarding a dyeing material by using an electron gun, wherein the dyeing material is a mixture of titanium oxide and niobium oxide, and a dyeing layer is formed on the surface of the inner protection layer;
and S5, bombarding the protective material by adopting an electron gun, and forming an outer protective layer on the surface of the dyeing layer to obtain the vacuum dyeing substrate.
Further, in step S1, the substrate is any one of a glass substrate, an acryl substrate, a polycarbonate substrate, a nylon substrate, and a CR-39 substrate.
Further, in step S2, the clean substrate is baked at a temperature of 50-70 ℃ for 1-3 hours.
Further, in step S3, the evacuating includes: when the vacuum degree in the vacuum chamber reaches 3 x 10 -5 When the temperature is below Torr, starting an ion source, and performing surface cleaning treatment on the baked substrate, wherein when the vacuum degree in the vacuum chamber reaches 1.5 x 10 - 5 Controlling the temperature in the vacuum chamber to 50-70 deg.C and the evaporation rate below Torr
Preferably, the vacuum degree is 1.5 x 10 -5 Torr-1.0*10 -7 Torr was used for vapor deposition.
Further, in the step S3 and/or S5, the content of silicon oxide is 70-85 wt%, and the content of aluminum oxide is 15-30 wt%; preferably, the thickness of the inner protective layer and/or the outer protective layer is 2000-3000 angstroms.
Further, in step S4, in the dyeing material, the content of titanium oxide is 25 to 45 wt%, and the content of niobium oxide is 55 to 75 wt%; the thickness of the dyeing layer is 500-2000 angstroms, preferably 1300-1900 angstroms, and the brown substrate is obtained.
Further, in step S4, in the dyeing material, the content of titanium oxide is 15 to 35 wt%, and the content of niobium oxide is 65 to 85 wt%; the thickness of the dyeing layer is 2050-.
Further, in step S4, in the dyeing material, the content of titanium oxide is 5 to 25 wt%, and the content of niobium oxide is 75 to 95 wt%; the thickness of the dyeing layer is 3550-.
The invention also protects the dyed substrate prepared by the substrate vacuum dyeing method, wherein the dyed substrate has the transmittance of 18-60%, preferably 20-50% in the visible light range and is brown, or has the transmittance of 8-43%, preferably 10-30% in the visible light range and is gray, or has the transmittance of 1-18%, preferably 2-8% in the visible light range and is black.
The invention also protects a pair of glasses, which comprises the dyed substrate, wherein the glasses are obtained by processing the functional thin film layer by using the dyed substrate as a base material.
Has the advantages that:
in the invention, the substrate vacuum dyeing method works under the vacuum condition, so that the using amount of dyeing agents can be saved, and the environment is protected; meanwhile, the thickness of the formed dyeing layer and the thickness of the formed protective layer film can be controlled to be in the Hermitian level, and the yield of the lenses is improved.
In the invention, the transmittance of the dyed substrate obtained by the substrate vacuum dyeing method meets the substrate grading requirement, the dyed substrate can replace the existing dyed sheet for subsequent processing, and the substrate has a specific color, so that the requirement of lens diversification can be met.
Drawings
In order to illustrate the technical solution of the present invention more clearly, the drawings will be briefly described below, and it is apparent that the drawings in the following description relate only to some embodiments of the present invention and are not intended to limit the present invention.
FIG. 1 is a spectrum of a lens provided in accordance with an embodiment 1 of the present invention;
FIG. 2 is a spectrum of a lens provided in accordance with one embodiment of the present invention 2;
FIG. 3 is a spectrum of a lens provided in accordance with an embodiment 3 of the present invention.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available. In the following examples, "%" means weight percent, unless otherwise specified.
Example 1
A method of vacuum dyeing a substrate comprising the steps of:
s1, cleaning and drying the substrate to obtain a clean substrate;
s2, putting the clean substrate into an oven, and baking for 2 hours at the temperature of 55-60 ℃ to obtain a baked substrate;
s3, placing the baked substrate on a jig, feeding the baked substrate into a vacuum coating machine cavity, vacuumizing the vacuum coating machine cavity, and when the vacuum degree in the vacuum coating machine cavity reaches 3 x 10 -5 Below Torr, starting ion source, cleaning the surface of the substrate, and maintaining the vacuum degree in the vacuum chamber at 1.5 x 10 -5 Controlling the temperature in the vacuum chamber to 55-60 deg.C and the evaporation rate below Torr
Bombarding a protective material by adopting an electron gun, wherein the protective material consists of 80% of silicon oxide and 20% of aluminum oxide, and an inner protective layer is formed on the surface of the baked substrate and has the thickness of 2400 angstroms;
s4, bombarding a dyeing material by using an electron gun, wherein the dyeing material consists of 35% of titanium oxide and 65% of niobium oxide, and a dyeing layer with the thickness of 1600 angstroms is formed on the surface of the inner protection layer;
and S5, bombarding the protective material by adopting an electron gun, wherein the protective material consists of 80% of silicon oxide and 20% of aluminum oxide, and an outer protective layer is formed on the surface of the dyeing layer and has the thickness of 2000 angstroms to obtain the vacuum dyeing substrate.
The vacuum dyed substrate prepared in this example was brown, and fig. 1 is a spectrum of the vacuum dyed substrate, which had a transmittance of 48% in the visible light range.
Example 2
A method of vacuum dyeing a substrate comprising the steps of:
s1, cleaning and drying the substrate to obtain a clean substrate;
s2, putting the clean substrate into an oven, and baking for 1 hour at the temperature of 65-70 ℃ to obtain a baked substrate;
s3, placing the baked substrate on a jig, feeding the baked substrate into a vacuum coating machine cavity, vacuumizing the vacuum coating machine cavity, and when the vacuum degree in the vacuum coating machine cavity reaches 3 x 10 -5 Below Torr, starting ion source, and cleaning surface of the substrate to vacuum degree of 1.5 × 10 -5 Controlling the temperature in the vacuum chamber to 60-65 deg.C and the evaporation rate below Torr
Bombarding a protective material by using an electron gun, wherein the protective material consists of 85% of silicon oxide and 15% of aluminum oxide, and an inner protective layer with the thickness of 2200 angstroms is formed on the surface of the baked substrate;
s4, bombarding a dyeing material by using an electron gun, wherein the dyeing material consists of 25% of titanium oxide and 75% of niobium oxide, and a dyeing layer with the thickness of 2500 angstroms is formed on the surface of the inner protection layer;
and S5, bombarding the protective material by using an electron gun, wherein the protective material consists of 85% of silicon oxide and 15% of aluminum oxide, and an outer protective layer is formed on the surface of the dyeing layer and has the thickness of 2500 angstroms to obtain the vacuum dyeing substrate.
The vacuum dyed substrate prepared in this example was gray, and fig. 2 is a spectrum diagram of the vacuum dyed substrate, which has a transmittance of 9% in the visible light range.
Example 3
A method of vacuum dyeing a substrate comprising the steps of:
s1, cleaning the glass substrate and drying to obtain a clean substrate;
s2, putting the clean substrate into an oven, and baking for 3 hours at the temperature of 50-55 ℃ to obtain a baked substrate;
s3, placing the baked substrate on a jig, feeding the baked substrate into a vacuum coating machine cavity, vacuumizing the vacuum coating machine cavity, and when the vacuum degree in the vacuum coating machine cavity reaches 3 x 10 -5 Below Torr, starting ion source, cleaning the surface of the substrate, and maintaining the vacuum degree in the vacuum chamber at 1.5 x 10 -5 Controlling the temperature in the vacuum chamber to 65-70 deg.C and the evaporation rate below Torr
Bombarding a protective material by using an electron gun, wherein the protective material consists of 70% of silicon oxide and 30% of aluminum oxide, and an inner protective layer with the thickness of 2500 angstroms is formed on the surface of the baked substrate;
s4, bombarding a dyeing material by using an electron gun, wherein the dyeing material consists of 15% of titanium oxide and 85% of niobium oxide, and a dyeing layer is formed on the surface of the inner protection layer and has a thickness of 3800 angstroms;
s5, bombarding the protective material by using an electron gun, wherein the protective material consists of 70% of silicon oxide and 30% of aluminum oxide, and an outer protective layer is formed on the surface of the dyeing layer and has the thickness of 2500 angstroms to obtain the vacuum dyeing substrate.
The vacuum dyeing substrate prepared by the embodiment is black, the film layer binding force is high, the substrate can resist the high temperature of 200-300 ℃, and the stress problem and the film cracking defective products can not occur. Fig. 3 is a spectrum of a vacuum dyed substrate having a transmittance of 1.3% in the visible light range.
Example 4
A method of vacuum dyeing a substrate comprising the steps of:
s1, cleaning and drying the substrate to obtain a clean substrate;
s2, putting the clean substrate into an oven, and baking for 2 hours at the temperature of 55-60 ℃ to obtain a baked substrate;
s3, placing the baked substrate on a jig, feeding the baked substrate into a vacuum coating machine cavity, vacuumizing the vacuum coating machine cavity, and when the vacuum degree in the vacuum coating machine cavity reaches 3 x 10 -5 Below Torr, starting ion source, cleaning the surface of the substrate, and maintaining the vacuum degree in the vacuum chamber at 1.5 x 10 -5 When the temperature is below Torr, the temperature in the vacuum chamber is controlled to be 55-60 ℃ and the evaporation rate is controlled to be below Torr
Bombarding a protective material by using an electron gun, wherein the protective material consists of 70% of silicon oxide and 30% of aluminum oxide, and an inner protective layer is formed on the surface of the baked substrate and has the thickness of 2800 angstroms;
s4, bombarding a dyeing material by using an electron gun, wherein the dyeing material consists of 25% of titanium oxide and 75% of niobium oxide, and a dyeing layer is formed on the surface of the inner protection layer and has the thickness of 1900 angstroms;
and S5, bombarding the protective material by adopting an electron gun, wherein the protective material consists of 80% of silicon oxide and 20% of aluminum oxide, and an outer protective layer is formed on the surface of the dyeing layer, wherein the thickness of the outer protective layer is 3000 angstroms, so that the vacuum dyeing substrate is obtained.
The vacuum dyed substrate prepared in this example was brown in color and had a transmittance of 20% in the visible light range.
Example 5
A method of vacuum dyeing a substrate comprising the steps of:
s1, cleaning and drying the substrate to obtain a clean substrate;
s2, putting the clean substrate into an oven, and baking for 2 hours at the temperature of 55-60 ℃ to obtain a baked substrate;
s3, placing the baked substrate on a jig, feeding the baked substrate into a vacuum coating machine cavity, vacuumizing the vacuum coating machine cavity, and when the vacuum degree in the vacuum coating machine cavity reaches 3 x 10 -5 Starting ion source when the temperature is below Torr, performing surface cleaning treatment on the substrate, and vacuumizing the vacuum chamberThe degree reaches 1.5 x 10 -5 Controlling the temperature in the vacuum chamber to 55-60 deg.C and the evaporation rate below Torr
Bombarding a protective material by using an electron gun, wherein the protective material consists of 70% of silicon oxide and 30% of aluminum oxide, and an inner protective layer is formed on the surface of the baked substrate and has the thickness of 2800 angstroms;
s4, bombarding a dyeing material by using an electron gun, wherein the dyeing material consists of 45% of titanium oxide and 55% of niobium oxide, and a dyeing layer with the thickness of 1300 angstroms is formed on the surface of the inner protection layer;
and S5, bombarding the protective material by adopting an electron gun, wherein the protective material consists of 80% of silicon oxide and 20% of aluminum oxide, and an outer protective layer is formed on the surface of the dyeing layer, wherein the thickness of the outer protective layer is 3000 angstroms, so that the vacuum dyeing substrate is obtained.
The vacuum dyed substrate prepared in this example was brown in color and had a transmittance of 56% in the visible light range.
Example 6
A method of vacuum dyeing a substrate comprising the steps of:
s1, cleaning and drying the substrate to obtain a clean substrate;
s2, putting the clean substrate into an oven, and baking for 1 hour at the temperature of 65-70 ℃ to obtain a baked substrate;
s3, placing the baked substrate on a jig, feeding the baked substrate into a vacuum coating machine cavity, vacuumizing the vacuum coating machine cavity, and when the vacuum degree in the vacuum coating machine cavity reaches 3 x 10 -5 Below Torr, starting ion source, cleaning the surface of the substrate, and maintaining the vacuum degree in the vacuum chamber at 1.5 x 10 -5 Controlling the temperature in the vacuum chamber to 60-65 deg.C and the evaporation rate below Torr
Bombarding a protective material by using an electron gun, wherein the protective material consists of 80% of silicon oxide and 20% of aluminum oxide, and an inner protective layer with the thickness of 2200 angstroms is formed on the surface of the baked substrate;
s4, bombarding a dyeing material by using an electron gun, wherein the dyeing material consists of 15% of titanium oxide and 85% of niobium oxide, and a dyeing layer is formed on the surface of the inner protection layer and has the thickness of 2100 angstroms;
s5, bombarding the protective material by using an electron gun, wherein the protective material consists of 85% of silicon oxide and 15% of aluminum oxide, and an outer protective layer is formed on the surface of the dyeing layer and has the thickness of 2500 angstroms to obtain the vacuum dyeing substrate.
The vacuum dyed substrate prepared in this example was gray in color and had a transmittance of 27% in the visible range.
Example 7
A method of vacuum dyeing a substrate comprising the steps of:
s1, cleaning and drying the substrate to obtain a clean substrate;
s2, putting the clean substrate into an oven, and baking for 1 hour at the temperature of 65-70 ℃ to obtain a baked substrate;
s3, placing the baked substrate on a jig, feeding the baked substrate into a vacuum coating machine chamber, vacuumizing the vacuum coating machine chamber until the vacuum degree in the vacuum coating machine chamber reaches 3 x 10 -5 Below Torr, starting ion source, cleaning the surface of the substrate, and maintaining the vacuum degree in the vacuum chamber at 1.5 x 10 -5 Controlling the temperature in the vacuum chamber to 60-65 deg.C and the evaporation rate below Torr
Bombarding a protective material by using an electron gun, wherein the protective material consists of 80% of silicon oxide and 20% of aluminum oxide, and an inner protective layer with the thickness of 2500 angstroms is formed on the surface of the baked substrate;
s4, bombarding a dyeing material by using an electron gun, wherein the dyeing material consists of 35% of titanium oxide and 65% of niobium oxide, and a dyeing layer is formed on the surface of the inner protection layer and has the thickness of 3300 angstroms;
and S5, bombarding the protective material by adopting an electron gun, wherein the protective material consists of 85% of silicon oxide and 15% of aluminum oxide, and an outer protective layer with the thickness of 2000 angstroms is formed on the surface of the dyeing layer to obtain the vacuum dyeing substrate.
The vacuum dyed substrate prepared in this example was gray in color and had a 12% transmission in the visible range.
Example 8
A method of vacuum dyeing a substrate comprising the steps of:
s1, cleaning the glass substrate and drying to obtain a clean substrate;
s2, putting the clean substrate into an oven, and baking for 3 hours at the temperature of 50-55 ℃ to obtain a baked substrate;
s3, placing the baked substrate on a jig, feeding the baked substrate into a vacuum coating machine cavity, vacuumizing the vacuum coating machine cavity, and when the vacuum degree in the vacuum coating machine cavity reaches 3 x 10 -5 Below Torr, starting ion source, cleaning the surface of the substrate, and maintaining the vacuum degree in the vacuum chamber at 1.5 x 10 -5 Controlling the temperature in the vacuum chamber to 65-70 deg.C and the evaporation rate below Torr
Bombarding a protective material by adopting an electron gun, wherein the protective material consists of 70% of silicon oxide and 30% of aluminum oxide, and an inner protective layer with the thickness of 2000 angstroms is formed on the surface of the baked substrate;
s4, bombarding a dyeing material by using an electron gun, wherein the dyeing material consists of 25% of titanium oxide and 75% of niobium oxide, and a dyeing layer is formed on the surface of the inner protection layer and has the thickness of 4500 angstroms;
and S5, bombarding the protective material by using an electron gun, wherein the protective material consists of 70% of silicon oxide and 30% of aluminum oxide, and an outer protective layer is formed on the surface of the dyeing layer and has the thickness of 2800 angstroms to obtain the vacuum dyeing substrate.
The vacuum dyeing substrate prepared by the embodiment is black, the film layer binding force is high, the substrate can resist the high temperature of 200-300 ℃, and the stress problem and the film cracking defective products can not occur. The transmittance in the visible light range was 2%.
Example 9
A method of vacuum dyeing a substrate comprising the steps of:
s1, cleaning the glass substrate and drying to obtain a clean substrate;
s2, putting the clean substrate into an oven, and baking for 3 hours at the temperature of 50-55 ℃ to obtain a baked substrate;
s3, placing the baked substrate on a jig, feeding the baked substrate into a vacuum coating machine cavity, vacuumizing the vacuum coating machine cavity, and when the vacuum degree in the vacuum coating machine cavity reaches 3 x 10 -5 Below Torr, starting ion source, and cleaning surface of the substrate to vacuum degree of 1.5 × 10 -5 Controlling the temperature in the vacuum chamber to 65-70 deg.C and the evaporation rate below Torr
Bombarding a protective material by adopting an electron gun, wherein the protective material consists of 70% of silicon oxide and 30% of aluminum oxide, and an inner protective layer with the thickness of 2000 angstroms is formed on the surface of the baked substrate;
s4, bombarding a dyeing material by using an electron gun, wherein the dyeing material consists of 25% of titanium oxide and 75% of niobium oxide, and a dyeing layer is formed on the surface of the inner protection layer and has the thickness of 3600 angstroms;
and S5, bombarding the protective material by adopting an electron gun, wherein the protective material consists of 70% of silicon oxide and 30% of aluminum oxide, and an outer protective layer with the thickness of 2000 angstroms is formed on the surface of the dyeing layer to obtain the vacuum dyeing substrate.
The vacuum dyeing substrate prepared by the embodiment is black, the film layer binding force is high, the substrate can resist the high temperature of 200-300 ℃, and the stress problem and the film cracking defective products can not occur. The transmittance in the visible light range was 10%.
Comparative example 1
Referring to example 1, the ratio of the dyes was varied, otherwise unchanged, including the following steps:
s1, cleaning and drying the substrate to obtain a clean substrate;
s2, putting the clean substrate into an oven, and baking for 2 hours at the temperature of 55-60 ℃ to obtain a baked substrate;
s3, placing the baking substrate in a baking machineThe vacuum coating device is put into a vacuum coating machine chamber and vacuumized, and when the vacuum degree in the vacuum chamber reaches 3 x 10 -5 Below Torr, starting ion source, cleaning the surface of the substrate, and maintaining the vacuum degree in the vacuum chamber at 1.5 x 10 -5 When the temperature is below Torr, the temperature in the vacuum chamber is controlled to be 55-60 ℃ and the evaporation rate is controlled to be below Torr
Bombarding a protective material by adopting an electron gun, wherein the protective material consists of 80% of silicon oxide and 20% of aluminum oxide, and an inner protective layer with the thickness of 1400 angstroms is formed on the surface of the baked substrate;
s4, bombarding a dyeing material by using an electron gun, wherein the dyeing material consists of 0% of titanium oxide and 100% of niobium oxide, and a dyeing layer with the thickness of 1600 angstroms is formed on the surface of the inner protection layer;
and S5, bombarding the protective material by adopting an electron gun, wherein the protective material consists of 80% of silicon oxide and 20% of aluminum oxide, and an outer protective layer is formed on the surface of the dyeing layer, wherein the thickness of the outer protective layer is 1000 angstroms, so that the vacuum dyeing substrate is obtained.
The color of the vacuum dyed substrate was close to a transparent color, and the transmittance in the visible range was 45%, which was close to the lens transmittance of example 1.
Comparative example 2
Referring to example 1, the ratio of the dyes was varied, otherwise unchanged, including the following steps:
s1, cleaning and drying the substrate to obtain a clean substrate;
s2, putting the clean substrate into an oven, and baking for 2 hours at the temperature of 55-60 ℃ to obtain a baked substrate;
s3, placing the baked substrate on a jig, feeding the baked substrate into a vacuum coating machine cavity, vacuumizing the vacuum coating machine cavity, and when the vacuum degree in the vacuum coating machine cavity reaches 3 x 10 -5 Below Torr, starting ion source, cleaning the surface of the substrate, and maintaining the vacuum degree in the vacuum chamber at 1.5 x 10 -5 Controlling the temperature in the vacuum chamber to 55-60 deg.C and the evaporation rate below Torr
Bombarding a protective material by adopting an electron gun, wherein the protective material consists of 80% of silicon oxide and 20% of aluminum oxide, and an inner protective layer with the thickness of 1400 angstroms is formed on the surface of the baked substrate;
s4, bombarding a dyeing material by using an electron gun, wherein the dyeing material consists of 100% of titanium oxide and 0% of niobium oxide, and a dyeing layer with the thickness of 1600 angstroms is formed on the surface of the inner protection layer;
and S5, bombarding the protective material by adopting an electron gun, wherein the protective material consists of 80% of silicon oxide and 20% of aluminum oxide, and an outer protective layer is formed on the surface of the dyeing layer, wherein the thickness of the outer protective layer is 1000 angstroms, so that the vacuum dyeing substrate is obtained.
The color of the vacuum dyed substrate was close to a transparent color, and the transmittance in the visible range was 47%, which was close to the lens transmittance of example 1.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. A method of vacuum dyeing a substrate, comprising: the method comprises the following steps:
s1, cleaning and drying the substrate to obtain a clean substrate;
s2, baking the clean substrate to obtain a baked substrate;
s3, placing the baked substrate on a jig, feeding the baked substrate into a vacuum coating machine chamber, vacuumizing the chamber, bombarding a protective material by using an electron gun, wherein the protective material is a mixture of silicon oxide and aluminum oxide, and forming an inner protective layer on the surface of the baked substrate;
s4, bombarding a dyeing material by using an electron gun, wherein the dyeing material is a mixture of titanium oxide and niobium oxide, and a dyeing layer is formed on the surface of the inner protection layer;
and S5, bombarding the protective material by adopting an electron gun, and forming an outer protective layer on the surface of the dyeing layer to obtain the vacuum dyeing substrate.
2. The method for vacuum dyeing a substrate according to claim 1, wherein: in step S1, the substrate is any one of a glass substrate, an acryl substrate, a polycarbonate substrate, a nylon substrate, and a CR-39 substrate.
3. The method of vacuum dyeing a substrate according to claim 1, characterized in that: in step S2, the clean substrate is baked at a temperature of 50-70 ℃ for 1-3 hours.
4. The method for vacuum dyeing a substrate according to claim 1, wherein: in step S3, the evacuating includes: when the vacuum degree in the vacuum chamber reaches 3 x 10 -5 Starting an ion source when the temperature is below Torr, and performing surface cleaning treatment on the baked substrate until the vacuum degree in the vacuum chamber reaches 1.5 x 10 -5 Controlling the temperature in the vacuum chamber to 50-70 deg.C and the evaporation rate below Torr
Preferably, the vacuum degree is 1.5 x 10 -5 Torr-1.0*10 -7 Torr was used for vapor deposition.
5. A method for vacuum dyeing a substrate according to any one of claims 1 to 4, characterized in that: in the step S3 and/or S5, the content of the silicon oxide in the protective material is 70-85 wt%, and the content of the aluminum oxide in the protective material is 15-30 wt%; preferably, the thickness of the inner protective layer and/or the outer protective layer is 2000-3000 angstroms.
6. A method for vacuum dyeing a substrate according to any one of claims 1 to 4, characterized in that: in step S4, in the dyeing material, the content of titanium oxide is 25-45 wt%, and the content of niobium oxide is 55-75 wt%; the thickness of the dyeing layer is 500-2000 angstroms, preferably 1300-1900 angstroms, and the brown substrate is obtained.
7. A method for vacuum dyeing a substrate according to any one of claims 1 to 4, characterized in that: in step S4, in the dyeing material, the content of titanium oxide is 15-35 wt%, and the content of niobium oxide is 65-85 wt%; the thickness of the dyeing layer is 2050-.
8. A method for vacuum dyeing a substrate according to any one of claims 1 to 4, characterized in that: in step S4, in the dyeing material, the content of titanium oxide is 5-25 wt%, and the content of niobium oxide is 75-95 wt%; the thickness of the dyeing layer is 3550-.
9. A dyed substrate produced by the substrate vacuum dyeing method of any one of claims 1 to 8, wherein: the dyed substrate has a transmittance of 18-60% in the visible range and a brown color, or has a transmittance of 8-43% in the visible range and a gray color, or has a transmittance of 1-18% in the visible range and a black color.
10. An ophthalmic lens comprising the dyed substrate of claim 9.
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| JP2016186661A (en) * | 2016-07-19 | 2016-10-27 | Hoya株式会社 | Optical member |
| CN111381299A (en) * | 2020-04-23 | 2020-07-07 | 江苏万新光学有限公司 | Low-reflection color neutral low-stress resin lens and preparation method thereof |
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| CN113552658A (en) * | 2021-07-14 | 2021-10-26 | 江苏康耐特光学有限公司 | High-temperature-resistant anti-reflection resin lens and preparation method thereof |
| CN215895150U (en) * | 2021-04-07 | 2022-02-22 | 江苏万新光学有限公司 | Ultra-low reflective clear ground color blue light-proof resin lens |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2016186661A (en) * | 2016-07-19 | 2016-10-27 | Hoya株式会社 | Optical member |
| CN111381299A (en) * | 2020-04-23 | 2020-07-07 | 江苏万新光学有限公司 | Low-reflection color neutral low-stress resin lens and preparation method thereof |
| CN112609161A (en) * | 2020-11-20 | 2021-04-06 | 厦门腾诺光学科技有限公司 | Preparation method of seawater corrosion resistant coated lens |
| CN112415640A (en) * | 2020-11-27 | 2021-02-26 | 江苏万新光学有限公司 | Resin lens for protecting green laser pen and preparation method thereof |
| CN215895150U (en) * | 2021-04-07 | 2022-02-22 | 江苏万新光学有限公司 | Ultra-low reflective clear ground color blue light-proof resin lens |
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