CN112415639A - Low-reflection infrared-proof high-temperature-resistant resin lens and preparation method thereof - Google Patents
Low-reflection infrared-proof high-temperature-resistant resin lens and preparation method thereof Download PDFInfo
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- CN112415639A CN112415639A CN202011356007.9A CN202011356007A CN112415639A CN 112415639 A CN112415639 A CN 112415639A CN 202011356007 A CN202011356007 A CN 202011356007A CN 112415639 A CN112415639 A CN 112415639A
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- 229920005989 resin Polymers 0.000 title claims abstract description 267
- 239000011347 resin Substances 0.000 title claims abstract description 267
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000002131 composite material Substances 0.000 claims abstract description 258
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims abstract description 134
- 239000000463 material Substances 0.000 claims abstract description 121
- 238000000034 method Methods 0.000 claims abstract description 98
- RJSRQTFBFAJJIL-UHFFFAOYSA-N niobium titanium Chemical compound [Ti].[Nb] RJSRQTFBFAJJIL-UHFFFAOYSA-N 0.000 claims abstract description 96
- 239000000758 substrate Substances 0.000 claims abstract description 67
- 239000011248 coating agent Substances 0.000 claims abstract description 45
- 238000000576 coating method Methods 0.000 claims abstract description 45
- 239000010408 film Substances 0.000 claims description 63
- 150000002500 ions Chemical class 0.000 claims description 51
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 48
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 46
- 238000010894 electron beam technology Methods 0.000 claims description 40
- 238000001771 vacuum deposition Methods 0.000 claims description 40
- 229910052681 coesite Inorganic materials 0.000 claims description 39
- 229910052906 cristobalite Inorganic materials 0.000 claims description 39
- 239000000377 silicon dioxide Substances 0.000 claims description 39
- 229910052682 stishovite Inorganic materials 0.000 claims description 39
- 229910052905 tridymite Inorganic materials 0.000 claims description 39
- 238000000151 deposition Methods 0.000 claims description 37
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 34
- 238000001035 drying Methods 0.000 claims description 30
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 21
- 229910052593 corundum Inorganic materials 0.000 claims description 21
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 19
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 13
- 239000005871 repellent Substances 0.000 claims description 13
- 230000005540 biological transmission Effects 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 238000005137 deposition process Methods 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 239000010409 thin film Substances 0.000 claims description 10
- 229910003437 indium oxide Inorganic materials 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 238000002310 reflectometry Methods 0.000 claims description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 5
- 229910052731 fluorine Inorganic materials 0.000 claims description 5
- 239000011737 fluorine Substances 0.000 claims description 5
- 230000002265 prevention Effects 0.000 claims description 5
- 125000005010 perfluoroalkyl group Chemical group 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 239000012808 vapor phase Substances 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims 2
- 229920001296 polysiloxane Polymers 0.000 claims 2
- 230000000007 visual effect Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 16
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 16
- 238000012360 testing method Methods 0.000 description 13
- 238000005516 engineering process Methods 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 11
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 239000012071 phase Substances 0.000 description 8
- 230000003287 optical effect Effects 0.000 description 7
- 239000010955 niobium Substances 0.000 description 6
- 238000002834 transmittance Methods 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
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- 229910002796 Si–Al Inorganic materials 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- -1 ITO) layer Chemical compound 0.000 description 2
- OBOYOXRQUWVUFU-UHFFFAOYSA-N [O-2].[Ti+4].[Nb+5] Chemical compound [O-2].[Ti+4].[Nb+5] OBOYOXRQUWVUFU-UHFFFAOYSA-N 0.000 description 2
- YAIQCYZCSGLAAN-UHFFFAOYSA-N [Si+4].[O-2].[Al+3] Chemical compound [Si+4].[O-2].[Al+3] YAIQCYZCSGLAAN-UHFFFAOYSA-N 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000002952 polymeric resin Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 230000006750 UV protection Effects 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
- 210000004087 cornea Anatomy 0.000 description 1
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- 238000004043 dyeing Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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Images
Classifications
-
- 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
- G02B1/14—Protective coatings, e.g. hard coatings
-
- 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
-
- 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
- G02B1/18—Coatings for keeping optical surfaces clean, e.g. hydrophobic or photo-catalytic films
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/208—Filters for use with infrared or ultraviolet radiation, e.g. for separating visible light from infrared and/or ultraviolet radiation
-
- G—PHYSICS
- G02—OPTICS
- G02C—SPECTACLES; SUNGLASSES OR GOGGLES INSOFAR AS THEY HAVE THE SAME FEATURES AS SPECTACLES; CONTACT LENSES
- G02C7/00—Optical parts
-
- G—PHYSICS
- G02—OPTICS
- G02C—SPECTACLES; SUNGLASSES OR GOGGLES INSOFAR AS THEY HAVE THE SAME FEATURES AS SPECTACLES; CONTACT LENSES
- G02C7/00—Optical parts
- G02C7/10—Filters, e.g. for facilitating adaptation of the eyes to the dark; Sunglasses
Abstract
The invention provides a low-reflection infrared-proof high-temperature-resistant resin lens and a preparation method thereof, wherein the preparation method comprises the following steps: the low-reflection infrared-proof film comprises a resin lens substrate, a hard coating, a low-reflection infrared-proof film layer and a waterproof layer; the substrate, the hardened layer and the low-reflection infrared-proof layer are sequentially arranged, the hardened layer is positioned on the surface of the resin lens substrate, and the low-reflection infrared-proof layer is positioned on the surface of the hardened layer; and the low-reflection infrared-proof layer is composed of a high-refractive-index material titanium niobium composite oxide and a low-refractive-index material silicon-aluminum composite oxide. According to the invention, by adjusting the structure of the low-reflection infrared-proof film layer and an appropriate process, the infrared-proof lens with good visual effect is obtained while the low reflection is satisfied, the high temperature resistance and the environmental resistance of the resin lens are greatly improved, and the resin lens has good market application prospect.
Description
Technical Field
The invention relates to the technical field of resin lens preparation, in particular to a low-reflection infrared-proof high-temperature-resistant resin lens and a preparation method thereof.
Background
In recent years, there is an increasing demand for optical resin lenses in the domestic and foreign eyeglass markets, and resin lenses have the advantages of light weight, good dyeing property, easy processing and the like compared with glass lenses, and medium and high refractive index optical resin lenses are favored by users with the unique advantages of high light transmittance, ultraviolet resistance, ultra-thinness and the like.
In the lens industry, high refractive index is generally used when the refractive index of the lens is 1.60 or more, medium refractive index is generally used when the refractive index is 1.56 or less, and low refractive index is generally used when the refractive index is 1.56 or less. In order to meet the requirement of optical performance of resin lenses, a film is generally coated on the surface of the resin lenses to reduce the reflection of light and enhance the transmission of light, i.e. an optical low-reflection film. Near infrared is not sensitive to light of human eyes, is mainly absorbed by cornea and has potential damage to human eyes. This requires low reflection and infrared protection on the optical film layers, which are much thicker than conventional optical film layers. In addition, because the main material of the optical film is inorganic material, and the polymer resin lens substrate is organic material, the stress of the coated lens is higher due to the difference of the physical and chemical properties of the optical film and the polymer resin lens, and further the temperature resistance and the durability are poor, especially the film layer with the low-reflection infrared-proof function is generally thicker, the stress of the coated lens is particularly obviously influenced, and the normal use of the coated lens is influenced. Therefore, how to provide a low-reflection infrared-proof high-temperature-resistant durable resin lens becomes a problem to be solved in the field.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a low-reflection infrared-proof high-temperature-resistant resin lens and a preparation method thereof, so that the infrared resistance is effectively realized, the reflectivity of the resin lens is reduced, and the high temperature resistance and the durability of the resin lens are improved by reducing stress.
The invention is realized by the following technical scheme:
the invention provides a low-reflection anti-infrared high-temperature-resistant resin lens in a first aspect, which comprises: the low-reflection infrared-proof lens comprises a resin lens substrate, a hardening layer and a low-reflection infrared-proof film layer; the resin lens substrate, the hardened layer and the low-reflection infrared-proof film layer are sequentially arranged, the hardened layer is located on the surface of the resin lens substrate, and the low-reflection infrared-proof film layer is located on the surface of the hardened layer;
further, the low-reflection infrared-proof high-temperature-resistant resin lens also comprises a waterproof layer, and the waterproof layer is positioned on the surface of the low-reflection infrared-proof film layer;
further, the material of the hard layer is organic silicon; more preferably, the organosilicon contains at least Ti;
further, the low-reflection infrared-proof layer comprises a silicon-aluminum composite oxide layer, a titanium-niobium composite oxide layer and a tin-doped indium oxide (ITO) layer; furthermore, the low-reflection infrared-proof layer comprises three silicon-aluminum composite oxide layers, two titanium-niobium composite oxide layers and a tin-doped indium oxide (ITO) layer; the low-reflection infrared-proof layer comprises four silicon-aluminum composite oxide layers, three titanium-niobium composite oxide layers and a tin-doped indium oxide (ITO) layer;
further, the silicon-aluminum composite oxide layer is made of SiO2And Al2O3Composite material composition, and SiO therein2The composite material accounts for 70 to 95 percent of the molar fraction of the composite material; further preferred, wherein SiO292% of the mole fraction of the composite material;
further, the titanium-niobium composite oxide layer is made of TiO2And Nb2O5Composite material composition of TiO2Accounting for 10 to 90 percent of the mole fraction of the composite material; preferably, wherein TiO280% of the mole fraction of the composite material;
further, the thickness of the hardening layer is 1-5 μm;
further, the thickness of the low-reflection infrared-proof film layer is 290-930 nm;
further, the thickness of the waterproof layer is 4-20 nm;
furthermore, the average reflectivity of the low-reflection infrared-proof resin high-temperature-resistant lens is less than or equal to 1.5 percent;
furthermore, the single-side peak reflectivity of the near infrared region of the low-reflection infrared-proof resin high-temperature-resistant lens is more than 40 percent; even more preferably, the near infrared wavelength is about 1000 nm;
the second aspect of the invention provides a preparation method of the low-reflection infrared-proof resin high-temperature-resistant lens, which comprises the following steps:
s1 preparing a stiffening layer: forming a hardening layer on the surface of the resin lens substrate to obtain a resin lens containing the hardening layer;
s2, preparing a low-reflection infrared-proof film layer: forming the low-reflection infrared-proof film layer on the surface of the resin lens obtained in the step S1, namely obtaining the resin lens containing the low-reflection infrared-proof film layer, specifically including:
s21: sequentially and alternately forming a silicon-aluminum composite oxide layer and a titanium-niobium composite oxide layer on the surface of the resin lens obtained in the step S1, namely obtaining the resin lens comprising the silicon-aluminum composite oxide layer and the titanium-niobium composite oxide layer;
s22: forming a resin lens containing an ITO layer on the surface of the resin lens obtained in step S21;
s23: forming a resin lens containing a silicon-aluminum composite oxide layer on the surface of the resin lens obtained in the step S22;
s3 preparing a waterproof layer: the water-repellent layer is formed on the surface of the resin lens obtained in step S2.
Advantageous effects
1. The titanium-niobium composite oxide material is adopted to prepare the film layer, so that the film layer has an infrared-proof effect, improves the temperature resistance and durability of the product, and simultaneously improves the repeatability and the mass production of the product:
(1) good optical effects are obtained: the film material adopts TiO2And Nb2O5Composite material and optical refractive index close to TiO2Nb to Nb2O5The refractive index of the materials is higher, so that the infrared cut-off prevention effect is better, the reflectivity of the low-reflection film is lower, the infrared cut-off is deeper than that of other existing products, and the light transmittance of the resin lens is improved, so that the lens prepared by the invention has a good visual effect while the human eyes are protected to reduce near infrared radiation.
(2) The temperature resistance and the durability of the lens are obviously improved: hair brushObviously adopts a high-refractive-index titanium-niobium composite oxide material with strict molar consumption ratio as a film material and TiO2Mixing Nb with a certain mol ratio2O5Can effectively avoid TiO2The easy crystallization characteristic of the film layer can also effectively avoid compact Nb2O5The film layer is easy to crack on the resin lens, the film layer is ensured to be in an amorphous state under the condition of low ion source energy of the resin glasses coated film, and the film layer is prevented from cracking due to crystallization, so that the high temperature resistance and high humidity resistance of the film layer and the lens are improved, and the durability of the product is further improved;
(3) the repeatability and the mass production of the product are improved: when the low-reflection titanium-niobium composite oxide film layer is prepared, the film layer is made of TiO2And Nb2O5Doping and reducing TiO2For O in IAD auxiliary process2The sensitivity of the flow reduces the process difficulty and effectively improves the repeatability and the mass production of the product.
2. The high temperature resistance of the product is improved: the invention adopts the silicon-aluminum composite oxide layer, thereby effectively avoiding SiO2The long column is easy to form, which leads to high stress of the film, maintains the glass state structure of the film and improves the high temperature resistance of the film.
Drawings
FIG. 1 is a schematic view of the layers of a low-reflection infrared-blocking resin lens prepared in example 1 of the present invention; the glass comprises a resin lens substrate 1, a hardening layer 2, a low-reflection infrared-proof film layer 3 and a waterproof layer 4; wherein, low reflection prevents infrared rete 3 includes: 3-1 parts of silicon-aluminum composite oxide layer, 3-2 parts of titanium-niobium composite oxide layer, 3-3 parts of silicon-aluminum composite oxide layer, 3-4 parts of titanium-niobium composite oxide layer, 3-5 parts of ITO layer and 3-6 parts of silicon-aluminum composite oxide layer
FIG. 2 is a schematic view of the layers of a low-reflection infrared-proof resin lens prepared in example 2 of the present invention; the glass comprises a resin lens substrate 1, a hardening layer 2, a low-reflection infrared-proof film layer 3 and a waterproof layer 4; wherein, low reflection prevents infrared rete 3 includes: 3-1 parts of silicon-aluminum composite oxide layer, 3-2 parts of titanium-niobium composite oxide layer, 3-3 parts of silicon-aluminum composite oxide layer, 3-4 parts of titanium-niobium composite oxide layer, 3-5 parts of silicon-aluminum composite oxide layer, 3-6 parts of titanium-niobium composite oxide layer, 3-7 parts of ITO layer and 3-8 parts of silicon-aluminum composite oxide layer
Detailed Description
In a specific embodiment, the low-reflection infrared-proof film layer comprises three silicon-aluminum composite oxide layers, two titanium-niobium composite oxide layers and one tin-doped indium oxide (i.e., ITO) layer, wherein the two silicon-aluminum composite oxide layers and the two titanium-niobium composite oxide layers are alternately and sequentially arranged, the first silicon-aluminum composite oxide layer is positioned on the surface of the hardened layer, the fifth ITO layer is positioned on the surface of the fourth titanium-niobium composite oxide layer, and the sixth silicon-aluminum composite oxide layer is positioned on the surface of the fifth ITO layer;
further, in a specific embodiment, the thickness of each layer of the low-reflection infrared-proof film layer is as follows:
the thickness of the first silicon-aluminum composite oxide layer is 0-180 nm, preferably 5-30 nm;
the thickness of the second titanium-niobium composite oxide layer is 60-130 nm, preferably 80-115 nm;
the thickness of the third silicon-aluminum composite oxide layer is 90-250 nm, preferably 140-210 nm;
the thickness of the fourth titanium-niobium composite oxide layer is 60-130 nm, preferably 80-110 nm;
the thickness of the fifth ITO layer is 2-10 nm, and preferably 5 nm;
the thickness of the sixth silicon-aluminum composite oxide layer is 60-130 nm, and preferably 70-95 nm;
in another parallel specific embodiment, the low-reflection infrared-proof film layer includes four silicon aluminum composite oxide layers, three titanium niobium composite oxide layers and one tin-doped indium oxide (i.e., ITO) layer, wherein in the low-reflection infrared-proof film layer, the three silicon aluminum composite oxide layers and the three titanium niobium composite oxide layers are alternately and sequentially arranged, the first silicon aluminum composite oxide layer is located on the surface of the hardened layer, the seventh ITO layer is located on the surface of the sixth titanium niobium composite oxide layer, and the eighth silicon aluminum composite oxide layer is located on the surface of the seventh ITO layer;
further, in a specific embodiment, the thickness of each layer of the low-reflection infrared-proof film layer is as follows:
the thickness of the first silicon-aluminum composite oxide layer is 0-180 nm, preferably 5-30 nm;
the thickness of the second titanium-niobium composite oxide layer is 10-40 nm, and preferably 12-30 nm;
the thickness of the third silicon-aluminum composite oxide layer is 10-60 nm, preferably 15-40 nm;
the thickness of the fourth titanium-niobium composite oxide layer is 60-130 nm, preferably 80-110 nm;
the thickness of the fifth silicon-aluminum composite oxide layer is 90-250 nm, preferably 140-210 nm;
the thickness of the sixth titanium-niobium composite oxide layer is 60-130 nm, preferably 80-110 nm;
the thickness of the seventh ITO layer is 2-10 nm, and preferably 5 nm;
the thickness of the eighth silicon-aluminum composite oxide layer is 60-130 nm, and preferably 70-95 nm;
in a specific embodiment, the step of S1 preparing the hardened layer comprises the steps of immersing a resin lens substrate cleaned by ultrasonic waves into 25-30% by mass of a hardening liquid aqueous solution, immersing at 10-20 ℃ for 5 seconds, then pulling out the solution at a speed of 1.0-3.0 mm/S, drying the solution at 70-90 ℃ for 3 hours, taking out the substrate, drying and curing the substrate in a drying oven at a curing temperature of 100-150 ℃ for 120-180 min, and thus obtaining the resin lens containing the hardened layer;
in a specific embodiment, the process of preparing the low-reflection infrared-proof film layer in step S2 includes:
in a vacuum coating machine, a vacuum coating process is adopted, after a silicon-aluminum composite oxide layer, a titanium-niobium composite oxide and an ITO solid film layer material are evaporated, vapor phase transmission is carried out, a thin film is deposited on the surface of the resin lens obtained in the step S1, and a low-reflection infrared-proof layer is formed, and the method specifically comprises the following steps:
s21: forming a silicon-aluminum composite oxide layer and a titanium-niobium composite oxide layer alternately and respectively on the surface of the resin lens obtained in step S1, namely obtaining the resin lens comprising the silicon-aluminum composite oxide layer and the titanium-niobium composite oxide layer, and specifically comprising:
s211: the surface of the resin lens obtained in S1 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 50-70 ℃, and the high-energy electron beam is adopted to heat the silicon-aluminum composite oxide under the condition of an ion source auxiliary process, wherein the speed isDepositing the evaporated silicon-aluminum composite oxide in a nanoscale molecular form to obtain a resin lens containing a first silicon-aluminum composite oxide layer;
s212: the surface of the resin lens obtained in S211 is not more than 3X 10 in the background vacuum degree-3Pa, the temperature in the coating chamber is 50-70 ℃, and the titanium-niobium composite oxide is heated by high-energy electron beams at the speed of 50-70 ℃ under the condition of an ion source auxiliary processDepositing the evaporated titanium-niobium composite oxide in a nano-scale molecular form to obtain a resin lens containing a second titanium-niobium composite oxide layer;
s213: repeating the steps S211 and S212, and respectively and alternately forming a third silicon-aluminum composite oxide layer and a fourth titanium-niobium composite oxide layer, namely forming the resin lens comprising the third silicon-aluminum composite oxide layer and the fourth titanium-niobium composite oxide layer; or alternately forming a third silicon-aluminum composite oxide layer, a fourth titanium-niobium composite oxide layer, a fifth silicon-aluminum composite oxide layer and a sixth titanium-niobium composite oxide layer respectively, namely forming the resin lens comprising the third silicon-aluminum composite oxide layer, the fourth titanium-niobium composite oxide layer, the fifth silicon-aluminum composite oxide layer and the sixth titanium-niobium composite oxide layer;
s22: the surface of the resin lens obtained in S21 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 50-70 ℃, and under the condition of an ion source auxiliary process, the temperature is highCapable of electron beam heating ITO at a rate ofDepositing the evaporated ITO in a nanoscale molecular form to obtain a resin lens containing an ITO layer;
s23: continuously adopting a vacuum coating process on the surface of the resin lens obtained in the step S22, repeating the process step S211, and forming a layer of resin lens containing the silicon-aluminum composite oxide layer;
further, in a specific embodiment, in the step S2, the ion source assisted deposition process parameters are: the ion source is a Hall source, and the anode voltage: 90-140V, anode current: 2.5-5A, and the auxiliary gas is O2The flow rate is 10-30 sccm; preferably, the ion source assisted deposition process parameters are as follows: the ion source is a Hall source, and the anode voltage: 110V, anode current: 3A, the auxiliary gas is O2The flow rate is 15 sccm;
in a specific embodiment, the step S3: the step of forming a water-repellent layer on the surface of the resin lens obtained in step S2 includes the steps of: continuously adopting a vacuum coating process on the surface of the lens obtained in the step S23, wherein the vacuum degree of the background is less than or equal to 3 multiplied by 10- 3Pa, and the temperature in the coating chamber is 50-70 ℃, adopting high-energy electron beams to heat the material at the speed ofEvaporating the fluorine-containing waterproof material (preferably containing perfluoroalkyl (C)12F27N) is deposited in a nanometer molecular form to obtain the resin lens containing the waterproof layer.
In one specific embodiment, the silicon-aluminum composite oxide is developed and produced by the company Summit photoelectric technology, Inc., of Yokou city, Yokou province, and the silicon-aluminum composite oxide layer is made of SiO2And Al2O3Composite material composition, and SiO therein2The composite material accounts for 70-95% of the mole fraction of the composite material, and the specific models refer to examples and comparative examples;
in a specific embodiment, theTitanium niobium composite oxide is developed and produced by Changzhou city Chi photoelectricity technology limited company, titanium niobium composite oxide is TiO2And Nb2O5Composition of, wherein TiO2The mole fraction of the compound is 10-90%, and the specific types refer to examples and comparative examples;
in one embodiment, a resin lens with a refractive index of 1.60 is selected as a substrate, for example, the lens substrate preparation monomer is MR-8 from Mitsui chemical corporation of Japan, hereinafter referred to as "MR-8";
in one embodiment, a hardening liquid of type Z117 (hereinafter referred to as "Z117") from Ito optics, Inc. is selected to prepare the lens of the invention, which greatly improves the tight adhesion between the layers.
Example (A)
Example 1
A low-reflection infrared-proof resin lens, which comprises the following components in sequence: a resin lens substrate 1 (MR-8); hardening layer 2 (Z117)/2.6-3 μm; the low-reflection infrared-proof layer 3 includes: silicon-aluminum composite oxide layer 3-1 (wherein SiO2And Al2O3Molar weight percentage: 92% SiO2:8%Al2O3(ii) a The material model is SA 56/26 nm, titanium-niobium composite oxide layer 3-2 (wherein TiO) and is produced by Yoghu photonics corporation2And Nb2O5The molar weight percentage is as follows: 80% TiO2:20%Nb2O5(ii) a The material model is PTN28)/111.34nm, the silicon-aluminum composite oxide layer is 3-3/166nm (the material is the same as 3-1), the titanium-niobium composite oxide layer is 3-4 (the material is the same as 3-2)/93.44nm, and the ITO layer is 3-5/5 nm; the silicon-aluminum composite oxide layer is 3-6/75.8nm (the material is the same as 3-1); waterproof layer 4 (adopting C-containing)12F27Waterproof material of N/10 nm);
the preparation method of the resin lens comprises the following steps:
s1: manufacturing a hardening layer: immersing the resin lens substrate cleaned by ultrasonic waves into hardening liquid aqueous solution with the mass percentage of 27% and the model of Z117, immersing at the temperature of 15 ℃, and pulling out the solution at the speed of 2.0mm/s after immersing for 5 seconds; drying the substrate for 3 hours at the temperature of 80 ℃, taking out the substrate, and sending the substrate into a drying oven for drying and curing, wherein the curing temperature is 120 ℃, and the curing time is 150min, so that the resin lens containing the hardened layer is obtained;
s2 preparation of the low-reflection infrared-proof layer: in a vacuum coating machine, a vacuum coating process is adopted, solid film layer materials are evaporated and then are subjected to gas phase transmission, a thin film is deposited on the surface of the resin lens obtained in the step S1, and the low-reflection infrared-proof layer is formed, and the method specifically comprises the following steps:
s21: the method comprises the following steps:
s211: the surface of the resin lens obtained in S1 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 60 ℃, and high-energy electron beams are adopted to heat the silicon-aluminum composite oxide under the condition of an ion source auxiliary process, and the speed is the speedDepositing the evaporated silicon-aluminum composite oxide in a nanoscale molecular form to obtain a resin lens containing a first silicon-aluminum composite oxide layer;
s212: the surface of the resin lens obtained in S211 is not more than 3X 10 in the background vacuum degree-3Pa, the temperature in the coating chamber is 60 ℃, and the titanium-niobium composite oxide is heated by high-energy electron beams at the speed of 60 ℃ under the condition of an ion source auxiliary processDepositing the evaporated titanium-niobium composite oxide in a nano-scale molecular form to obtain a resin lens containing a second titanium-niobium composite oxide layer;
s213: repeating the steps S211 and S212, and respectively and alternately forming a third silicon-aluminum composite oxide layer and a fourth titanium-niobium composite oxide layer, namely forming the resin lens comprising the third silicon-aluminum composite oxide layer and the fourth titanium-niobium composite oxide layer;
s22: the surface of the resin lens obtained in S21 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 60 ℃ and the ion existsUnder the condition of a sub-source auxiliary process, a high-energy electron beam is adopted to heat ITO at a speed ofDepositing the evaporated ITO in a nanoscale molecular form to obtain a resin lens containing a fifth ITO layer;
s23: continuously adopting a vacuum coating process on the surface of the resin lens obtained in the step S22, repeating the process step S211, and forming the resin lens containing the sixth silicon-aluminum composite oxide layer;
in step S2, the ion source assisted deposition process parameters are: the ion source is a Hall source, and the anode voltage: 110V, anode current: 3A, the auxiliary gas is O2The flow rate is 15 sccm;
s3 preparing a waterproof layer: forming a water-repellent layer on the surface of the resin lens obtained in S23: continuously adopting a vacuum coating process on the surface of the lens obtained in the step S2, wherein the vacuum degree of the background is less than or equal to 3 multiplied by 10-3Pa, and the temperature in the coating chamber is 60 ℃, adopting high-energy electron beams to heat the material at the speed ofThe evaporated liquid contains C12F27And (3) depositing the waterproof material of N on the surface of the resin lens obtained in the S24 in a nano-scale molecular form to obtain the waterproof resin lens.
Example 2
A low-reflection infrared-proof resin lens, which comprises the following components in sequence: a resin lens substrate 1 (MR-8); hardening layer 2 (Z117)/2.6-3 μm; the low-reflection infrared-proof layer 3 includes: silicon-aluminum composite oxide layer 3-1 (wherein SiO2And Al2O3Molar weight percentage: 92% SiO2:8%Al2O3(ii) a The material model is SA 56/27.6 nm, and the titanium-niobium composite oxide layer 3-2 (TiO in the material) is developed and produced by Yoghu photoelectric technology corporation of Changzhou city2And Nb2O5The molar weight percentage is as follows: 80% TiO2:20%Nb2O5(ii) a The material model is PTN28)/15.45nm, developed and produced by Yokou Yoghhi photoelectric technology corporationThe composite silicon-aluminum oxide layer is 3-3/31.42nm (same as 3-1), the composite titanium-niobium oxide layer is 3-4 (same as 3-2)/98.9nm, the composite silicon-aluminum oxide layer is 3-5/171.92nm (same as 3-1), the composite titanium-niobium oxide layer is 3-6 (same as 3-2)/91.96nm, and the ITO layer is 3-7/5 nm; the silicon-aluminum composite oxide layer is 3-8/75.8nm (the material is the same as 3-1); waterproof layer 4 (adopting a material containing C)12F27Waterproof material of N/10 nm);
the preparation method of the resin lens comprises the following steps:
s1: manufacturing a hardening layer: immersing the resin lens substrate cleaned by ultrasonic waves into hardening liquid aqueous solution with the mass percentage of 27% and the model of Z117, immersing at the temperature of 15 ℃, and pulling out the solution at the speed of 2.0mm/s after immersing for 5 seconds; drying the substrate for 3 hours at the temperature of 80 ℃, taking out the substrate, and sending the substrate into a drying oven for drying and curing, wherein the curing temperature is 120 ℃, and the curing time is 150min, so that the resin lens containing the hardened layer is obtained;
s2 preparation of the low-reflection infrared-proof layer: in a vacuum coating machine, a vacuum coating process is adopted, solid film layer materials are evaporated and then are subjected to gas phase transmission, a thin film is deposited on the surface of the resin lens obtained in the step S1, and the low-reflection infrared-proof layer is formed, and the method specifically comprises the following steps:
s21: the method comprises the following steps:
s211: the surface of the resin lens obtained in S1 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 60 ℃, and high-energy electron beams are adopted to heat the silicon-aluminum composite oxide under the condition of an ion source auxiliary process, and the speed is the speedDepositing the evaporated silicon-aluminum composite oxide in a nanoscale molecular form to obtain a resin lens containing a first silicon-aluminum composite oxide layer;
s212: the surface of the resin lens obtained in S211 is not more than 3X 10 in the background vacuum degree-3Pa, the temperature in the coating chamber is 60 ℃, and the titanium-niobium composite oxide is heated by high-energy electron beams at the speed of 60 ℃ under the condition of an ion source auxiliary processDepositing the evaporated titanium-niobium composite oxide in a nano-scale molecular form to obtain a resin lens containing a second titanium-niobium composite oxide layer;
s213: repeating the steps S211 and S212, and alternately forming a third silicon-aluminum composite oxide layer, a fourth titanium-niobium composite oxide layer, a fifth silicon-aluminum composite oxide layer and a sixth titanium-niobium composite oxide layer respectively, namely forming the resin lens comprising the third silicon-aluminum composite oxide layer, the fourth titanium-niobium composite oxide layer, the fifth silicon-aluminum composite oxide layer and the sixth titanium-niobium composite oxide layer;
s22: the surface of the resin lens obtained in S21 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 60 ℃, and ITO is heated by high-energy electron beams at the speed of 60 ℃ under the condition of an ion source auxiliary processDepositing the evaporated ITO in a nano-scale molecular form to obtain a resin lens containing a seventh ITO layer;
s23: continuously adopting a vacuum coating process on the surface of the resin lens obtained in the step S22, repeating the process step S211, and forming the resin lens containing the eighth silicon-aluminum composite oxide layer;
in step S2, the ion source assisted deposition process parameters are: the ion source is a Hall source, and the anode voltage: 110V, anode current: 3A, the auxiliary gas is O2The flow rate is 15 sccm;
s3 preparing a waterproof layer: forming a water-repellent layer on the surface of the resin lens obtained in S23: continuously adopting a vacuum coating process on the surface of the lens obtained in the step S2, wherein the vacuum degree of the background is less than or equal to 3 multiplied by 10-3Pa, and the temperature in the coating chamber is 60 ℃, adopting high-energy electron beams to heat the material at the speed ofThe evaporated liquid contains C12F27The waterproof material of N is deposited on the surface of the resin lens obtained in S24 in the form of nano-scale molecules,and (5) obtaining the product.
Example 3
A low-reflection infrared-proof resin lens, which comprises the following components in sequence: a resin lens substrate 1 (MR-8); hardening layer 2 (Z117)/1-2.6 μm; the low-reflection infrared-proof layer 3 includes: silicon-aluminum composite oxide layer 3-1 (wherein SiO2And Al2O3Molar weight percentage: 92% SiO2:8%Al2O3(ii) a The material model is SA 56/27.6 nm, and the titanium-niobium composite oxide layer 3-2 (TiO in the material) is developed and produced by Yoghu photoelectric technology corporation of Changzhou city2And Nb2O5The molar weight percentage is as follows: 50% TiO2:50%Nb2O5(ii) a The material model is PTN55)/15.47nm, the silicon-aluminum composite oxide layer is 3-3/30.04nm (the material is the same as 3-1), the titanium-niobium composite oxide layer is 3-4 (the material is the same as 3-2)/96.66nm, the silicon-aluminum composite oxide layer is 3-5/176.75nm (the material is the same as 3-1), the titanium-niobium composite oxide layer is 3-6 (the material is the same as 3-2)/89.16nm, and the ITO layer is 3-7/3 nm; the silicon-aluminum composite oxide layer is 3-8/76.69nm (the material is the same as 3-1); waterproof layer 4 (adopting C-containing)12F27Waterproof material of N/10 nm); the preparation method is the same as that of example 2.
Example 4
A low-reflection infrared-proof resin lens, which comprises the following components in sequence: a resin lens substrate 1 (MR-8); adding a hard layer 2 (Z117)/3-5 μm; the low-reflection infrared-proof layer 3 includes: silicon-aluminum composite oxide layer 3-1 (wherein SiO2And Al2O3Molar weight percentage: 92% SiO2:8%Al2O3(ii) a The material model is SA 56/28.8 nm, and the titanium-niobium composite oxide layer 3-2 (TiO in the material) is developed and produced by Yoghu photoelectric technology corporation of Changzhou city2And Nb2O5The molar weight percentage is as follows: 20% TiO2:80%Nb2O5(ii) a The material model is PTN57)/14.62nm, the silicon-aluminum composite oxide layer is 3-3/31.82nm (the material is the same as 3-1), the titanium-niobium composite oxide layer is 3-4 (the material is the same as 3-2)/101.06nm, the silicon-aluminum composite oxide layer is 3-5/171.04nm (the material is the same as 3-1), and the titanium-niobium composite oxide layer is developed and produced by the Yoghu photoelectric science and technology Limited company in Changzhou city3-6 (the same material as 3-2)/93.59nm of the composite oxide layer and 3-7/8nm of the ITO layer; the silicon-aluminum composite oxide layer is 3-8/75.74nm (the material is the same as 3-1); waterproof layer 4 (adopting a material containing C)12F27Waterproof material of N/15 nm); the preparation method is the same as that of example 2.
Example 5
A low-reflection infrared-proof resin lens, which comprises the following components in sequence: a resin lens substrate 1 (MR-8); hardening layer 2 (Z117)/2.6-3 μm; the low-reflection infrared-proof layer 3 includes: silicon-aluminum composite oxide layer 3-1 (wherein SiO2And Al2O3Molar weight percentage: 80% SiO2:20%Al2O3(ii) a The material model is SA 86/27.6 nm, and the titanium-niobium composite oxide layer 3-2 (TiO in the material) is developed and produced by Yoghu photoelectric technology corporation of Changzhou city2And Nb2O5The molar weight percentage is as follows: 80% TiO2:20%Nb2O5(ii) a The material model is PTN28)/15.45nm, 3-3/31.42nm of silicon-aluminum composite oxide layer (the material is the same as 3-1), 3-4 of titanium-niobium composite oxide layer (the material is the same as 3-2)/98.9nm, 3-5/171.92nm of silicon-aluminum composite oxide layer (the material is the same as 3-1), 3-6 of titanium-niobium composite oxide layer (the material is the same as 3-2)/91.96nm and 3-7/5 nm; the silicon-aluminum composite oxide layer is 3-8/75.8nm (the material is the same as 3-1); waterproof layer 4 (made of fluorine-containing waterproof material (e.g. containing perfluoroalkane (C))12F27N))/10 nm); the preparation method is the same as that of example 2.
(II) comparative example
Comparative example 1
A low-reflection infrared-proof resin lens, which comprises the following components in sequence: a resin lens substrate 1 (MR-8); hardening layer 2 (Z117)/2.6-3 μm; the low-reflection infrared-proof layer 3 includes: SiO 22Layer 3-1/26.6nm, ZrO2Layer 3-2/17.12nm, SiO2Layer 3-3/16.05nm, ZrO2Layer 3-4/111.76nm, SiO2Layer 3-5/163.07nm, ZrO2Layer 3-6/100.59nm, ITO layer 3-7/5 nm; SiO 22Layer 3-8/64.24 nm; waterproof layer 4 (adopting a material containing C)12F27Waterproof material of N/10 nm);
the preparation method comprises the following steps:
s1: manufacturing a hardening layer: immersing the resin lens substrate cleaned by ultrasonic waves into hardening liquid aqueous solution with the mass percentage of 27% and the model of Z117, immersing at the temperature of 15 ℃, and pulling out the solution at the speed of 2.0mm/s after immersing for 5 seconds; drying the substrate for 3 hours at the temperature of 80 ℃, taking out the substrate, and sending the substrate into a drying oven for drying and curing, wherein the curing temperature is 120 ℃, and the curing time is 150min, so that the resin lens containing the hardened layer is obtained;
s2 preparation of the low-reflection infrared-proof layer: in a vacuum coating machine, a vacuum coating process is adopted, solid film layer materials are evaporated and then are subjected to gas phase transmission, a thin film is deposited on the surface of the resin lens obtained in the step S1, and the low-reflection infrared-proof layer is formed, and the method specifically comprises the following steps:
s21: the method comprises the following steps:
s211: the surface of the resin lens obtained in S1 was maintained at a vacuum degree of not more than 3X 10 in the background-3Heating SiO by high-energy electron beams under the conditions of Pa, 60 ℃ of temperature in a coating chamber and no ion source auxiliary process2At a rate ofThe evaporated SiO2Depositing in the form of nano-scale molecules to obtain SiO containing the first layer2A resin lens of the layer;
s212: the surface of the resin lens obtained in S211 is not more than 3X 10 in the background vacuum degree-3Pa, the temperature in the coating chamber is 60 ℃, and ZrO is heated by high-energy electron beams under the condition of no ion source auxiliary process2At a rate ofThe evaporated ZrO2Deposited in the form of nanoscale molecules to obtain a layer containing ZrO2A resin lens of the layer;
s213: repeating the steps S211 and S212 to respectively and alternately form a third SiO layer2And a fourth layer of ZrO2Layer and fifth layer of SiO2Layer and sixth layer ZrO2Layers, i.e. forming SiO comprising a third layer2Layer, fourth layer ZrO2Layer, fifth layer of SiO2Layer and sixth layer ZrO2A resin lens of the layer;
s22: the surface of the resin lens obtained in S21 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 60 ℃, and ITO is heated by high-energy electron beams at the speed of 60 ℃ under the condition of an ion source auxiliary processDepositing the evaporated ITO in a nano-scale molecular form to obtain a resin lens containing a seventh ITO layer;
s23: continuing to adopt the vacuum coating process on the surface of the resin lens obtained in the step S22, repeating the process step S211, and forming the SiO-containing eighth layer2A resin lens of the layer;
s3 preparing a waterproof layer: forming a water-repellent layer on the surface of the resin lens obtained in S23: continuously adopting a vacuum coating process on the surface of the lens obtained in the step S2, wherein the vacuum degree of the background is less than or equal to 3 multiplied by 10-3Pa, and the temperature in the coating chamber is 60 ℃, adopting high-energy electron beams to heat the material at the speed ofThe evaporated liquid contains C12F27And (3) depositing the waterproof material of N on the surface of the resin lens obtained in the S24 in a nano-scale molecular form to obtain the waterproof resin lens.
Comparative example 2
A low-reflection infrared-proof resin lens, which comprises the following components in sequence: a resin lens substrate 1 (MR-8); hardening layer 2 (Z117)/2.6-3 μm; the low-reflection infrared-proof layer 3 includes: silicon-aluminum composite oxide layer 3-1 (wherein SiO2And Al2O3Molar weight percentage: 92% SiO2:8%Al2O3(ii) a The material model is SA56)/26nm and TiO, developed and produced by Youth Chihua Xiichi photoelectric technology corporation2Layer 3-2/111.34nm, silicon-aluminum composite oxide layer 3-3/166nm (same material as 3-1), TiO2Layer 3-4/93.44nm, ITO layer 3-5/5nm, and silicon-aluminum composite oxide layer 3-6/75.8nm (the same material as 3-1); waterproof layer 4 (adopting a material containing C)12F27Waterproof material of N/10 nm);the preparation method comprises the following steps:
the preparation method of the resin lens comprises the following steps:
s1: manufacturing a hardening layer: immersing the resin lens substrate cleaned by ultrasonic waves into hardening liquid aqueous solution with the mass percentage of 27% and the model of Z117, immersing at the temperature of 15 ℃, and pulling out the solution at the speed of 2.0mm/s after immersing for 5 seconds; drying the substrate for 3 hours at the temperature of 80 ℃, taking out the substrate, and sending the substrate into a drying oven for drying and curing, wherein the curing temperature is 120 ℃, and the curing time is 150min, so that the resin lens containing the hardened layer is obtained;
s2 preparation of the low-reflection infrared-proof layer: in a vacuum coating machine, a vacuum coating process is adopted, solid film layer materials are evaporated and then are subjected to gas phase transmission, a thin film is deposited on the surface of the resin lens obtained in the step S1, and the low-reflection infrared-proof layer is formed, and the method specifically comprises the following steps:
s21: the method comprises the following steps:
s211: the surface of the resin lens obtained in S1 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 60 ℃, and high-energy electron beams are adopted to heat the silicon-aluminum composite oxide under the condition of an ion source auxiliary process, and the speed is the speedDepositing the evaporated silicon-aluminum composite oxide in a nanoscale molecular form to obtain a resin lens containing a first silicon-aluminum composite oxide layer;
s212: the surface of the resin lens obtained in S211 is not more than 3X 10 in the background vacuum degree-3Pa, the temperature in the coating chamber is 60 ℃, and high-energy electron beams are adopted to heat TiO under the condition of ion source auxiliary process2At a rate ofEvaporating the TiO2Depositing in the form of nano-scale molecules to obtain a second layer containing TiO2A resin lens of the layer;
s213: repeating the steps S211 and S212 to respectively and alternately form a third layer of silicon-aluminum composite oxide and a fourth layer of TiO2Layer formationComprises a third silicon-aluminum composite oxide layer and a fourth TiO layer2A resin lens of the layer;
s22: the surface of the resin lens obtained in S21 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 60 ℃, and ITO is heated by high-energy electron beams at the speed of 60 ℃ under the condition of an ion source auxiliary processDepositing the evaporated ITO in a nanoscale molecular form to obtain a resin lens containing a fifth ITO layer;
s23: continuously adopting a vacuum coating process on the surface of the resin lens obtained in the step S22, repeating the process step S211, and forming the resin lens containing the sixth silicon-aluminum composite oxide layer;
in step S2, the ion source assisted deposition process parameters are: the ion source is a Hall source, and the anode voltage: 110V, anode current: 3A, the auxiliary gas is O2The flow rate is 15 sccm;
s3 preparing a waterproof layer: forming a water-repellent layer on the surface of the resin lens obtained in S23: continuously adopting a vacuum coating process on the surface of the lens obtained in the step S2, wherein the vacuum degree of the background is less than or equal to 3 multiplied by 10-3Pa, and the temperature in the coating chamber is 60 ℃, adopting high-energy electron beams to heat the material at the speed ofThe evaporated liquid contains C12F27And (3) depositing the waterproof material of N on the surface of the resin lens obtained in the S24 in a nano-scale molecular form to obtain the waterproof resin lens.
Comparative example 3
A low-reflection infrared-proof resin lens, which comprises the following components in sequence: a resin lens substrate 1 (MR-8); hardening layer 2 (Z117)/2.6-3 μm; the low-reflection infrared-proof layer 3 includes: silicon-aluminum composite oxide layer 3-1 (wherein SiO2And Al2O3Molar weight percentage: 92% SiO2:8%Al2O3(ii) a The material model is SA56)/27.6nm and TiO, developed and produced by Yoghu photoelectric technology corporation2Layer 3-2/15.45nm, Si-Al composite oxide layer 3-3/31.42nm (same material as 3-1), and TiO2Layer 3-4/98.9nm, Si-Al composite oxide layer 3-5/171.92nm (same material as 3-1), and TiO2Layer 3-6/91.96nm, ITO layer 3-7/5 nm; the silicon-aluminum composite oxide layer is 3-8/75.8nm (the material is the same as 3-1); waterproof layer 4 (adopting C-containing)12F27Waterproof material of N/10 nm);
the preparation method comprises the following steps:
s1: manufacturing a hardening layer: immersing the resin lens substrate cleaned by ultrasonic waves into hardening liquid aqueous solution with the mass percentage of 27% and the model of Z117, immersing at the temperature of 15 ℃, and pulling out the solution at the speed of 2.0mm/s after immersing for 5 seconds; drying the substrate for 3 hours at the temperature of 80 ℃, taking out the substrate, and sending the substrate into a drying oven for drying and curing, wherein the curing temperature is 120 ℃, and the curing time is 150min, so that the resin lens containing the hardened layer is obtained;
s2 preparation of the low-reflection infrared-proof layer: in a vacuum coating machine, a vacuum coating process is adopted, solid film layer materials are evaporated and then are subjected to gas phase transmission, a thin film is deposited on the surface of the resin lens obtained in the step S1, and the low-reflection infrared-proof layer is formed, and the method specifically comprises the following steps:
s21: the method comprises the following steps:
s211: the surface of the resin lens obtained in S1 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 60 ℃, and high-energy electron beams are adopted to heat the silicon-aluminum composite oxide under the condition of an ion source auxiliary process, and the speed is the speedDepositing the evaporated silicon-aluminum composite oxide in a nanoscale molecular form to obtain a resin lens containing a first silicon-aluminum composite oxide layer;
s212: the surface of the resin lens obtained in S211 is not more than 3X 10 in the background vacuum degree-3Pa, the temperature in the coating chamber is 60 ℃, and high-energy electron beams are adopted to heat TiO under the condition of ion source auxiliary process2At a rate ofEvaporating the TiO2Depositing in the form of nano-scale molecules to obtain a second layer containing TiO2A resin lens of the layer;
s213: repeating the steps S211 and S212 to respectively and alternately form a third layer of silicon-aluminum composite oxide and a fourth layer of TiO2Layer, fifth silicon-aluminum composite oxide layer and sixth TiO layer2Layer, namely a third silicon-aluminum composite oxide layer and a fourth TiO layer are formed2Layer, fifth silicon-aluminum composite oxide layer and sixth TiO layer2A resin lens of the layer;
s22: the surface of the resin lens obtained in S21 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 60 ℃, and ITO is heated by high-energy electron beams at the speed of 60 ℃ under the condition of an ion source auxiliary processDepositing the evaporated ITO in a nano-scale molecular form to obtain a resin lens containing a seventh ITO layer;
s23: continuously adopting a vacuum coating process on the surface of the resin lens obtained in the step S22, repeating the process step S211, and forming the resin lens containing the eighth silicon-aluminum composite oxide layer;
in step S2, the ion source assisted deposition process parameters are: the ion source is a Hall source, and the anode voltage: 110V, anode current: 3A, the auxiliary gas is O2The flow rate is 15 sccm;
s3 preparing a waterproof layer: forming a water-repellent layer on the surface of the resin lens obtained in S23: continuously adopting a vacuum coating process on the surface of the lens obtained in the step S2, wherein the vacuum degree of the background is less than or equal to 3 multiplied by 10-3Pa, and the temperature in the coating chamber is 60 ℃, adopting high-energy electron beams to heat the material at the speed ofThe evaporated liquid contains C12F27And (3) depositing the waterproof material of N on the surface of the resin lens obtained in the S24 in a nano-scale molecular form to obtain the waterproof resin lens.
Comparative example 4
A low-reflection infrared-proof resin lens, which comprises the following components in sequence: a resin lens substrate 1 (MR-8); hardening layer 2 (Z117)/2.6-3 μm; the low-reflection infrared-proof layer 3 includes: SiO 22Layer 3-1/27.6nm, TiO2Layer 3-2/15.45nm, SiO2Layer 3-3/31.42nm, TiO2Layer 3-4/98.9nm, SiO2Layer 3-5/171.92nm, TiO2Layer 3-6/91.96nm, ITO layer 3-7/5 nm; SiO 22Layer 3-8/75.8 nm; waterproof layer 4 (adopting C-containing)12F27Waterproof material of N/10 nm); the preparation method comprises the following steps:
s1: manufacturing a hardening layer: immersing the resin lens substrate cleaned by ultrasonic waves into hardening liquid aqueous solution with the mass percentage of 27% and the model of Z117, immersing at the temperature of 15 ℃, and pulling out the solution at the speed of 2.0mm/s after immersing for 5 seconds; drying the substrate for 3 hours at the temperature of 80 ℃, taking out the substrate, and sending the substrate into a drying oven for drying and curing, wherein the curing temperature is 120 ℃, and the curing time is 150min, so that the resin lens containing the hardened layer is obtained;
s2 preparation of the low-reflection infrared-proof layer: in a vacuum coating machine, a vacuum coating process is adopted, solid film layer materials are evaporated and then are subjected to gas phase transmission, a thin film is deposited on the surface of the resin lens obtained in the step S1, and the low-reflection infrared-proof layer is formed, and the method specifically comprises the following steps:
s21: the method comprises the following steps:
s211: the surface of the resin lens obtained in S1 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 60 ℃, and high-energy electron beams are adopted to heat SiO under the condition of ion source auxiliary process2At a rate ofThe evaporated SiO2Depositing in the form of nano-scale molecules to obtain SiO containing the first layer2A resin lens of the layer;
s212: the surface of the resin lens obtained in S211 is not more than 3X 10 in the background vacuum degree-3Pa, the temperature in the coating chamber is 60 ℃, and high-energy electron beams are adopted to heat TiO under the condition of ion source auxiliary process2At a rate ofEvaporating the TiO2Depositing in the form of nano-scale molecules to obtain a second layer containing TiO2A resin lens of the layer;
s213: repeating the steps S211 and S212 to respectively and alternately form a third SiO layer2Layer and fourth layer of TiO2Layer and fifth layer of SiO2Layer and sixth layer of TiO2Layers, i.e. forming SiO comprising a third layer2Layer, fourth layer TiO2Layer, fifth layer of SiO2Layer and sixth layer of TiO2A resin lens of the layer;
s22: the surface of the resin lens obtained in S21 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 60 ℃, and ITO is heated by high-energy electron beams at the speed of 60 ℃ under the condition of an ion source auxiliary processDepositing the evaporated ITO in a nano-scale molecular form to obtain a resin lens containing a seventh ITO layer;
s23: continuing to adopt the vacuum coating process on the surface of the resin lens obtained in the step S22, repeating the process step S211, and forming the SiO-containing eighth layer2A resin lens of the layer;
in step S2, the ion source assisted deposition process parameters are: the ion source is a Hall source, and the anode voltage: 110V, anode current: 3A, the auxiliary gas is O2The flow rate is 15 sccm;
s3 preparing a waterproof layer: forming a water-repellent layer on the surface of the resin lens obtained in S23: continuously adopting a vacuum coating process on the surface of the lens obtained in the step S2, wherein the vacuum degree of the background is less than or equal to 3 multiplied by 10-3Pa, and the temperature in the coating chamber is 60 ℃, adopting high-energy electron beams to heat the material at the speed ofThe evaporated liquid contains C12F27And (3) depositing the waterproof material of N on the surface of the resin lens obtained in the S24 in a nano-scale molecular form to obtain the waterproof resin lens.
Comparative example 5
A low-reflection infrared-proof resin lens, which comprises the following components in sequence: a resin lens substrate 1 (MR-8); hardening layer 2 (Z117)/2.6-3 μm; the low-reflection infrared-proof layer 3 includes: SiO 22Layer 3-1(/27.6nm, titanium niobium composite oxide layer 3-2 (where TiO)2And Nb2O5The molar weight percentage is as follows: 80% TiO2:20%Nb2O5(ii) a The material model is PTN28)/15.45nm SiO2Layer 3-3/31.42nm, titanium-niobium composite oxide layer 3-4 (same material as 3-2)/98.9nm, SiO2The layer is 3-5/171.92nm, the titanium niobium composite oxide layer is 3-6 (the material is the same as 3-2)/91.96nm, and the ITO layer is 3-7/5 nm; SiO 22Layer 3-8/75.8 nm; waterproof layer 4 (adopting C-containing)12F27Waterproof material of N/10 nm); the preparation method comprises the following steps:
s1: manufacturing a hardening layer: immersing the resin lens substrate cleaned by ultrasonic waves into hardening liquid aqueous solution with the mass percentage of 27% and the model of Z117, immersing at the temperature of 15 ℃, and pulling out the solution at the speed of 2.0mm/s after immersing for 5 seconds; drying the substrate for 3 hours at the temperature of 80 ℃, taking out the substrate, and sending the substrate into a drying oven for drying and curing, wherein the curing temperature is 120 ℃, and the curing time is 150min, so that the resin lens containing the hardened layer is obtained;
s2 preparation of the low-reflection infrared-proof layer: in a vacuum coating machine, a vacuum coating process is adopted, solid film layer materials are evaporated and then are subjected to gas phase transmission, a thin film is deposited on the surface of the resin lens obtained in the step S1, and the low-reflection infrared-proof layer is formed, and the method specifically comprises the following steps:
s21: the method comprises the following steps:
s211: the surface of the resin lens obtained in S1 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 60 ℃, and high-energy electron beams are adopted to heat SiO under the condition of ion source auxiliary process2At a rate ofThe evaporated SiO2Depositing in the form of nanoscale molecules to obtain a first layerSiO2A resin lens of the layer;
s212: the surface of the resin lens obtained in S211 is not more than 3X 10 in the background vacuum degree-3Pa, the temperature in the coating chamber is 60 ℃, and the titanium-niobium composite oxide is heated by high-energy electron beams at the speed of 60 ℃ under the condition of an ion source auxiliary processDepositing the evaporated titanium-niobium composite oxide in a nano-scale molecular form to obtain a resin lens containing a second titanium-niobium composite oxide layer;
s213: repeating the steps S211 and S212 to respectively and alternately form a third SiO layer2Layer, fourth titanium niobium composite oxide layer and fifth SiO2Layer and a sixth titanium niobium composite oxide layer, i.e. formed to include a third SiO layer2Layer, fourth titanium niobium composite oxide layer, fifth SiO2A resin lens comprising a layer and a sixth titanium-niobium composite oxide layer;
s22: the surface of the resin lens obtained in S21 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 60 ℃, and ITO is heated by high-energy electron beams at the speed of 60 ℃ under the condition of an ion source auxiliary processDepositing the evaporated ITO in a nano-scale molecular form to obtain a resin lens containing a seventh ITO layer;
s23: continuing to adopt the vacuum coating process on the surface of the resin lens obtained in the step S22, repeating the process step S211, and forming the SiO-containing eighth layer2A resin lens of the layer;
in step S2, the ion source assisted deposition process parameters are: the ion source is a Hall source, and the anode voltage: 110V, anode current: 3A, the auxiliary gas is O2The flow rate is 15 sccm;
s3 preparing a waterproof layer: forming a water-repellent layer on the surface of the resin lens obtained in S23: continuously adopting a vacuum coating process on the surface of the lens obtained in the step S2, wherein the vacuum degree of the background is less than or equal to 3 multiplied by 10-3Pa and platingHeating the material with high-energy electron beam at a temperature of 60 deg.C in the film chamber at a rate ofThe evaporated liquid contains C12F27And (3) depositing the waterproof material of N on the surface of the resin lens obtained in the S24 in a nano-scale molecular form to obtain the waterproof resin lens.
Comparative example 6
A low-reflection infrared-proof resin lens, which comprises the following components in sequence: a resin lens substrate 1 (MR-8); adding a hard layer 2 (Z117)/3-5 μm; the low-reflection infrared-proof layer 3 includes: silicon-aluminum composite oxide layer 3-1 (wherein SiO2And Al2O3Molar weight percentage: 92% SiO2:8%Al2O3(ii) a The material model is SA56)/28.8nm, which is developed and produced by Changzhou Yoghhi photoelectric technology GmbH; nb2O5Layer 3-2/14.62nm, silicon-aluminum composite oxide layer 3-3/31.82nm (same material as 3-1), Nb2O5Layer 3-4/101.06nm, silicon-aluminum composite oxide layer 3-5/171.04nm (same material as 3-1), Nb2O5Layer 3-6/93.59nm, ITO layer 3-7/8 nm; the silicon-aluminum composite oxide layer is 3-8/75.74nm (the material is the same as 3-1); waterproof layer 4 (adopting C-containing)12F27Waterproof material of N/15 nm);
the preparation method comprises the following steps:
s1: manufacturing a hardening layer: immersing the resin lens substrate cleaned by ultrasonic waves into hardening liquid aqueous solution with the mass percentage of 27% and the model of Z117, immersing at the temperature of 15 ℃, and pulling out the solution at the speed of 2.0mm/s after immersing for 5 seconds; drying the substrate for 3 hours at the temperature of 80 ℃, taking out the substrate, and sending the substrate into a drying oven for drying and curing, wherein the curing temperature is 120 ℃, and the curing time is 150min, so that the resin lens containing the hardened layer is obtained;
s2 preparation of the low-reflection infrared-proof layer: in a vacuum coating machine, a vacuum coating process is adopted, solid film layer materials are evaporated and then are subjected to gas phase transmission, a thin film is deposited on the surface of the resin lens obtained in the step S1, and the low-reflection infrared-proof layer is formed, and the method specifically comprises the following steps:
s21: the method comprises the following steps:
s211: the surface of the resin lens obtained in S1 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 60 ℃, and high-energy electron beams are adopted to heat the silicon-aluminum composite oxide under the condition of an ion source auxiliary process, and the speed is the speedDepositing the evaporated silicon-aluminum composite oxide in a nanoscale molecular form to obtain a resin lens containing a first silicon-aluminum composite oxide layer;
s212: the surface of the resin lens obtained in S211 is not more than 3X 10 in the background vacuum degree-3Pa, the temperature in the coating chamber is 60 ℃, and Nb is heated by adopting high-energy electron beams under the condition of an ion source auxiliary process2O5At a rate ofEvaporating Nb2O5Depositing in a nanoscale molecular form to obtain a second Nb-containing layer2O5A resin lens of the layer;
s213: repeating the steps S211 and S212 to respectively and alternately form a third layer of silicon-aluminum composite oxide and a fourth layer of Nb2O5Layer, fifth silicon-aluminum composite oxide layer and sixth layer Nb2O5Layer, namely a third silicon-aluminum composite oxide layer and a fourth Nb layer are formed2O5Layer, fifth silicon-aluminum composite oxide layer and sixth layer Nb2O5A resin lens of the layer;
s22: the surface of the resin lens obtained in S21 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 60 ℃, and ITO is heated by high-energy electron beams at the speed of 60 ℃ under the condition of an ion source auxiliary processDepositing the evaporated ITO in a nano-scale molecular form to obtain a resin lens containing a seventh ITO layer;
s23: continuously adopting a vacuum coating process on the surface of the resin lens obtained in the step S22, repeating the process step S211, and forming the resin lens containing the eighth silicon-aluminum composite oxide layer;
in step S2, the ion source assisted deposition process parameters are: the ion source is a Hall source, and the anode voltage: 110V, anode current: 3A, the auxiliary gas is O2The flow rate is 15 sccm;
s3 preparing a waterproof layer: forming a water-repellent layer on the surface of the resin lens obtained in S23: continuously adopting a vacuum coating process on the surface of the lens obtained in the step S2, wherein the vacuum degree of the background is less than or equal to 3 multiplied by 10-3Pa, and the temperature in the coating chamber is 60 ℃, adopting high-energy electron beams to heat the material at the speed ofThe evaporated liquid contains C12F27And (3) depositing the waterproof material of N on the surface of the resin lens obtained in the S24 in a nano-scale molecular form to obtain the waterproof resin lens.
Comparative example 7
A low-reflection infrared-proof resin lens, which comprises the following components in sequence: a resin lens substrate 1 (MR-8); hardening layer 2 (Z117)/2.6-3 μm; the low-reflection infrared-proof layer 3 includes: silicon-aluminum composite oxide layer 3-1 (wherein SiO2And Al2O3Molar weight percentage: 60% SiO2:40%Al2O3(ii) a The material model is SA 66/27.6 nm, and the titanium-niobium composite oxide layer 3-2 (TiO in the material) is developed and produced by Yoghu photoelectric technology corporation of Changzhou city2And Nb2O5The molar weight percentage is as follows: 80% TiO2:20%Nb2O5(ii) a The material model is PTN28)/15.45nm, 3-3/31.42nm of silicon-aluminum composite oxide layer (the material is the same as 3-1), 3-4 of titanium-niobium composite oxide layer (the material is the same as 3-2)/98.9nm, 3-5/171.92nm of silicon-aluminum composite oxide layer (the material is the same as 3-1), 3-6 of titanium-niobium composite oxide layer (the material is the same as 3-2)/91.96nm and 3-7/5 nm; the silicon-aluminum composite oxide layer is 3-8/75.8nm (the material is the same as 3-1); waterproof layer 4 (made of fluorine-containing waterproof material (e.g. containing perfluoroalkane (C))12F27N))/10 nm); preparation of the resin lensThe procedure is as in example 2.
Second, Experimental example
1. Determination of average reflectance and anti-infrared effects of lenses
(1) Pre-experiment: we have conducted the refractive indices of the examples and the materials selected for the proportion
Measuring
The results are shown in table 1 below:
TABLE 1
Therefore, the titanium-niobium composite oxide material has a high refractive index, and can meet the requirement of preparing a low-reflection anti-infrared coating film.
TABLE 2
Thus, it can be seen that the SiO of the Si-Al composite oxide material2When the proportion is higher, the refractive index is lower, and the requirement of preparing the low-reflection anti-infrared coating film can be met. When SiO is reduced2When the ratio is high, the composite refractive index is high, the spectral performance effect of the low-reflection infrared-resistant coating film is influenced, and the aim of the invention cannot be achieved.
(2) Determination of average reflectance and anti-infrared effects of examples 1 to 5 and comparative examples 1 to 7 average reflectance (average reflectance: means visual average reflectance under illumination of C light (light source of color temperature 6774K defined in CIE) and reflectance of one side herein) and transmittance of near infrared (near infrared average transmittance: means arithmetic average transmittance of 900 to 1100nm of lens after both sides are plated) were determined for the lenses prepared in examples 1 to 5 and comparative examples 1 to 7, and the measurement results are recorded in the following table 3:
TABLE 3
And (4) conclusion: examples 1 to 5 all had a low visible light average reflectance of 0.7% to 1.1% and a low near infrared average transmittance of 30 to 33%; while comparative examples 1 and 7 did not achieve the above technical effects, i.e., did not achieve good low reflection and infrared cut-off effects.
2. High temperature resistance, durability and high temperature adhesion testing
2.1 temperature resistance experiment:
after the samples (examples 1 to 5 and comparative examples 1 to 7) were completed, the temperature resistance of the samples was tested after storage for one week. The test method for temperature resistance is as per item 5.8 in the national resin lens temperature resistance standard (GB 10810.4-2012): pass the bake test at 55 ℃ for 30 minutes. And (4) performing a test by adding 5 ℃ baking for 30 minutes each time in the same way until the lens has a film crack or orange peel failure phenomenon, and recording the qualified highest temperature. The results are reported in table 4 below.
2.2 high-temperature adhesion experiment:
the adhesion test refers to the film adhesion test of 5.9 th item in GB 10810.4-2012. The high-temperature film layer adhesion test refers to that the boiling condition of a brand new company is changed into 90 +/-2 ℃ for 60 minutes according to the 5.9 th item in the national standard GB 10810.4-2012, and other test methods are the same. Adhesion and high temperature adhesion test results: the grade A means that the demoulding area is less than 5 percent or the demoulding area is not less than 5 percent, the grade B means that the demoulding area is between 5 percent and 15 percent, and the grade C (unqualified) means that the demoulding area is obviously more than 15 percent. In order to verify the adhesive force distribution of the product, high-temperature adhesive force tests were performed from 5 different positions in the coating chamber. The test results for examples 1-5 and comparative examples 1-7 are reported in Table 4 below.
2.3 high temperature high humidity test
The photovoltaic industry and the optical communication industry use high temperature and high humidity to evaluate the durability of products. Referring to the Test method of the photovoltaic industry Test standard (GB/T18911-: storing for 12 hours at 85 ℃ and 85% humidity, and checking whether the prepared lens has obvious failure phenomena such as film cracking or orange peel and the like; 3 resin lenses placed in different positions for each high temperature and humidity test. The test results for examples 1-5 and comparative examples 1-7 are reported in Table 4 below.
TABLE 4
Therefore, under the condition that other conditions are not changed, the high-refractive-index material of the lens is better than other conventional materials in high-temperature resistance, high-temperature adhesive force and durability of the titanium-niobium composite oxide; the low refractive index material adopts silicon-aluminum composite oxide, and the high temperature resistance, high temperature adhesive force and durability of the silicon-aluminum composite oxide are better than those of other conventional materials; the two materials with specific mixture ratio are adopted to prepare a film system and a proper process thereof so as to ensure the high temperature resistance and durability of the low-reflection infrared-proof product.
Claims (16)
1. A low-reflection anti-infrared high-temperature-resistant resin lens is characterized by comprising: the low-reflection infrared-proof lens comprises a resin lens substrate, a hardening layer and a low-reflection infrared-proof film layer; the resin lens substrate, the hardening layer and the low-reflection infrared-proof film layer are sequentially arranged, the hardening layer is located on the surface of the resin lens substrate, and the low-reflection infrared-proof film layer is located on the surface of the hardening layer.
2. The resin lens for low reflection, infrared prevention and high temperature resistance according to claim 1, wherein the resin lens for low reflection, infrared prevention and high temperature resistance further comprises a waterproof layer, and the waterproof layer is located on the surface of the low reflection, infrared prevention film layer.
3. The resin lens with low reflection, infrared resistance and high temperature resistance as claimed in claim 1 or 2, wherein the material of the hard coating is silicone; more preferably, the silicone contains at least Ti element.
4. The resin lens with low reflection, anti-infrared and high temperature resistance as claimed in claim 1 or 2, wherein the low reflection, anti-infrared layer comprises a silicon-aluminum composite oxide layer, a titanium-niobium composite oxide layer and a tin-doped indium oxide (i.e. ITO) layer; furthermore, the low-reflection infrared-proof layer comprises three silicon-aluminum composite oxide layers, two titanium-niobium composite oxide layers and a tin-doped indium oxide (ITO) layer; or further, the low-reflection infrared-proof layer comprises four silicon-aluminum composite oxide layers, three titanium-niobium composite oxide layers and one tin-doped indium oxide (ITO) layer.
5. The resin lens with low reflection, infrared resistance and high temperature resistance as claimed in claim 4, wherein the silicon-aluminum composite oxide layer is made of SiO2And Al2O3Composite material composition, and SiO therein2The composite material accounts for 70 to 95 percent of the molar fraction of the composite material; further preferred, wherein SiO2Representing 92% of the mole fraction of the composite.
6. The resin lens with low reflection, infrared prevention and high temperature resistance as claimed in claim 4, wherein the titanium niobium composite oxide layer is made of TiO2And Nb2O5Composite material composition of TiO2Accounting for 10 to 90 percent of the mole fraction of the composite material; preferably, wherein TiO2Accounting for 80 percent of the mole fraction of the composite material.
7. The resin lens with low reflection, anti-infrared and high temperature resistance as claimed in any one of claims 1 to 2 and 5 to 6, wherein the thickness of the hardened layer is 1 to 5 μm.
8. The resin lens with low reflection, anti-infrared and high temperature resistance as claimed in any one of claims 1 to 2 and 5 to 6, wherein the thickness of the low reflection, anti-infrared film layer is 290 to 930 nm.
9. The resin lens with low reflection, infrared resistance and high temperature resistance according to any one of claims 1 to 2 and 5 to 6, wherein the thickness of the waterproof layer is 4 to 20 nm.
10. The resin lens with low reflection, anti-infrared and high temperature resistance as claimed in any one of claims 1-2 and 5-6, wherein the average reflectivity of the resin lens with low reflection, anti-infrared and high temperature resistance is less than or equal to 1.5%.
11. The resin lens with low reflection, anti-infrared and high temperature resistance as claimed in any one of claims 1 to 2 and 5 to 6, wherein the single-sided peak reflectivity of the resin lens with low reflection, anti-infrared and high temperature resistance in the near infrared region is more than 40%.
12. The preparation method of the low-reflection infrared-proof resin high-temperature-resistant resin lens as claimed in any one of claims 1 to 11, characterized by comprising the following steps:
s1 preparing a stiffening layer: forming a hardening layer on the surface of the resin lens substrate to obtain a resin lens containing the hardening layer;
s2, preparing a low-reflection infrared-proof film layer: forming the low-reflection infrared-proof film layer on the surface of the resin lens obtained in the step S1, namely obtaining the resin lens containing the low-reflection infrared-proof film layer, specifically including:
s21: sequentially and alternately forming a silicon-aluminum composite oxide layer and a titanium-niobium composite oxide layer on the surface of the resin lens obtained in the step S1, namely obtaining the resin lens comprising the silicon-aluminum composite oxide layer and the titanium-niobium composite oxide layer;
s22: forming a resin lens containing an ITO layer on the surface of the resin lens obtained in step S21;
s23: forming a resin lens containing a silicon-aluminum composite oxide layer on the surface of the resin lens obtained in the step S22;
s3 preparing a waterproof layer: the water-repellent layer is formed on the surface of the resin lens obtained in step S2.
13. The method for preparing the low-reflection infrared-proof resin high-temperature-resistant resin lens as claimed in claim 12, wherein the step of S1 preparing the hardening layer comprises:
immersing a resin lens substrate cleaned by ultrasonic waves into a hardening liquid aqueous solution with the mass percentage of 25-30%, wherein the immersion temperature is 10-20 ℃, after 5 seconds of immersion, the solution is pulled out at the speed of 1.0-3.0 mm/s, then drying the resin lens substrate at the temperature of 70-90 ℃ for 2-4 hours, then taking out the substrate, and sending the substrate into a drying box for drying and curing, wherein the curing temperature is 100-150 ℃, and the curing time is 120-180 min, thus obtaining the resin lens containing the hardening layer.
14. The method for preparing the low-reflection infrared-proof resin high-temperature-resistant resin lens as claimed in claim 12, wherein the step S2 of preparing the low-reflection infrared-proof film layer comprises the following steps:
in a vacuum coating machine, a vacuum coating process is adopted, after a silicon-aluminum composite oxide layer, a titanium-niobium composite oxide and an ITO solid film layer material are evaporated, vapor phase transmission is carried out, a thin film is deposited on the surface of the resin lens obtained in the step S1, and a low-reflection infrared-proof layer is formed, and the method specifically comprises the following steps:
s21: forming a silicon-aluminum composite oxide layer and a titanium-niobium composite oxide layer alternately and respectively on the surface of the resin lens obtained in step S1, namely obtaining the resin lens comprising the silicon-aluminum composite oxide layer and the titanium-niobium composite oxide layer, and specifically comprising:
s211: the surface of the resin lens obtained in S1 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 50-70 ℃, and the high-energy electron beam is adopted to heat the silicon-aluminum composite oxide under the condition of an ion source auxiliary process, wherein the speed isDepositing the evaporated silicon-aluminum composite oxide in a nanoscale molecular form to obtain a resin lens containing a first silicon-aluminum composite oxide layer;
s212: the surface of the resin lens obtained in S211 is not more than 3X 10 in the background vacuum degree-3Pa and the temperature in the coating chamber is 50 DEGHeating the titanium-niobium composite oxide by adopting high-energy electron beams at the speed of 70 ℃ below zero under the condition of an ion source auxiliary processDepositing the evaporated titanium-niobium composite oxide in a nano-scale molecular form to obtain a resin lens containing a second titanium-niobium composite oxide layer;
s213: repeating the steps S211 and S212, and respectively and alternately forming a third silicon-aluminum composite oxide layer and a fourth titanium-niobium composite oxide layer, namely forming the resin lens comprising the third silicon-aluminum composite oxide layer and the fourth titanium-niobium composite oxide layer; or alternately forming a third silicon-aluminum composite oxide layer, a fourth titanium-niobium composite oxide layer, a fifth silicon-aluminum composite oxide layer and a sixth titanium-niobium composite oxide layer respectively, namely forming the resin lens comprising the third silicon-aluminum composite oxide layer, the fourth titanium-niobium composite oxide layer, the fifth silicon-aluminum composite oxide layer and the sixth titanium-niobium composite oxide layer;
s22: the surface of the resin lens obtained in S21 was maintained at a vacuum degree of not more than 3X 10 in the background-3Pa, the temperature in the coating chamber is 50-70 ℃, and an ion source auxiliary process is adopted, high-energy electron beams are adopted to heat the ITO, and the speed isDepositing the evaporated ITO in a nanoscale molecular form to obtain a resin lens containing an ITO layer;
s23: and (5) continuously adopting a vacuum coating process on the surface of the resin lens obtained in the step S22, repeating the process step S211, and forming a layer of resin lens containing the silicon-aluminum composite oxide layer.
15. The method for preparing a low-reflection infrared-proof resin high-temperature-resistant resin lens as claimed in claim 14, wherein in the step S2, the ion source assisted deposition process parameters are as follows: the ion source is a Hall source, and the anode voltage: 90-140V, anode current: 2.5-5A, and the auxiliary gas is O2The flow rate is 10 to 30sccm。
16. The method for preparing the low-reflection infrared-proof resin high-temperature-resistant resin lens as claimed in claim 12, wherein the step S3: the step of forming a water-repellent layer on the surface of the resin lens obtained in step S2 includes the steps of: continuously adopting a vacuum coating process on the surface of the lens obtained in the step S23, wherein the vacuum degree of the background is less than or equal to 3 multiplied by 10-3Pa, and the temperature in the coating chamber is 50-70 ℃, adopting high-energy electron beams to heat the material at the speed ofDepositing the evaporated fluorine-containing waterproof material in a nano-scale molecular form to obtain a resin lens containing a waterproof layer; preferably, the fluorine-containing waterproof material contains perfluoroalkyl (namely C)12F27N) a water-repellent material.
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CN208207410U (en) * | 2018-06-08 | 2018-12-07 | 江苏康耐特光学有限公司 | A kind of plated film resin lens containing sieve and silica-sesquioxide layer |
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