CN116716035A - Filtering coating material capable of accurately regulating and controlling protection - Google Patents
Filtering coating material capable of accurately regulating and controlling protection Download PDFInfo
- Publication number
- CN116716035A CN116716035A CN202310686422.8A CN202310686422A CN116716035A CN 116716035 A CN116716035 A CN 116716035A CN 202310686422 A CN202310686422 A CN 202310686422A CN 116716035 A CN116716035 A CN 116716035A
- Authority
- CN
- China
- Prior art keywords
- core
- oxide
- selenide
- shell
- filter coating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 239000011248 coating agent Substances 0.000 title claims abstract description 80
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- 230000001276 controlling effect Effects 0.000 title description 5
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- 239000002184 metal Substances 0.000 claims abstract description 43
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- HNVAGBIANFAIIL-UHFFFAOYSA-N 2-hydroxy-2-methylpropanal Chemical compound CC(C)(O)C=O HNVAGBIANFAIIL-UHFFFAOYSA-N 0.000 claims description 2
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- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 2
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- 229910052691 Erbium Inorganic materials 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229940011182 cobalt acetate Drugs 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- VBXWCGWXDOBUQZ-UHFFFAOYSA-K diacetyloxyindiganyl acetate Chemical compound [In+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VBXWCGWXDOBUQZ-UHFFFAOYSA-K 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000012921 fluorescence analysis Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 230000004297 night vision Effects 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000921 polyethylene adipate Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/44—Polycarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/664—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/671—Unsaturated compounds having only one group containing active hydrogen
- C08G18/672—Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/73—Polyisocyanates or polyisothiocyanates acyclic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- 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
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2262—Oxides; Hydroxides of metals of manganese
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
A filter coating material with precise regulation and control protection comprises a A, B component and an A component comprising: 72-90% of polyurethane acrylate prepolymer; 0-5.5% core-shell metal selenide nanoparticles; 0-5.5% core-shell metal oxide nanoparticles; 9.5 to 19 percent of active diluent; 0.1 to 1 percent of defoaming agent; the component B is 0.4-4% of photoinitiator. The polyurethane acrylate segmented copolymer is obtained through the polyaddition reaction of diisocyanate, dihydric alcohol and hydroxy acrylate, then is compounded with a nano material with a specific spectrum function, reactive groups, metal selenides and metal oxide nano particles are introduced into a polymer structure, and the spectrum characteristics of different nano particles in polyurethane acrylate resin are utilized, so that the light filtering and color can be accurately regulated and controlled by selectively transmitting the spectrum of a required wave band.
Description
Technical Field
The invention belongs to the technical field of optical filter materials, and particularly relates to a functional optical filter coating material capable of accurately regulating and controlling optical filter wave bands and coating colors.
Background
The nano composite filter material is a new material with excellent optical properties and special functions in the field of light prevention and control, and is an optical component for selecting a required radiation wave band. The method is widely applied to the optical fields of lasers, sensors, filters, 3D scanning, intelligent driving, biomedical treatment, fluorescence analysis, biological identification, security monitoring, laser radar, aerospace, monitoring systems, infrared cameras, machine vision, window materials, night vision devices and the like. The common optical filter materials are acrylic and optical glass, and the manufacturing process and physical properties of the optical filter materials are relatively large in difference. The acrylic filter is generally prepared by adding particles with different proportions in the production process through pouring or extrusion, so that the acrylic filter has different color light transmission effects, such as red light, green light and the like; the glass filter is usually manufactured by coating a film on the surface of an optical glass to interfere with the light transmission property of the lens, so that a specific wavelength is transmitted or cut off, the wavelength range is also wider, and the glass filter can be manufactured from ultraviolet rays to visible light, near infrared rays and middle and far infrared rays.
Conventional fabrication techniques for existing filters include stamp dyeing, high temperature doping, and electrophoretic deposition (EPD): (1) a filtering technology formed by dyeing a plastic sheet: the plastic sheet with accurate size is boiled in hot water with organic dye or heated and mixed with polymer particle material to produce color with the color being selected based on the wavelength band. The disadvantage is that the light transmittance of the filter is poor and the spectrum band is wide due to the dyeing technology. (2) The filtering technology formed by doping metal oxide into glass sheet is to dope cobalt oxide and copper oxide according to the requirements of different filtering wave bands to prepare blue glass and dope transition metal oxide such as ferric oxide to prepare red filtering glass. The method has the defects of high energy consumption and serious environmental pollution. (3) The filtering technology for forming the white film adopts a film coating deposition method to design the intercepting wave band range, has narrow spectrum band distribution, but has high product cost, high reject ratio and limited mass production.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a filter coating material capable of accurately regulating and protecting, which is characterized in that polyurethane acrylate segmented copolymer is obtained through the polyaddition reaction of diisocyanate, dihydric alcohol and hydroxy acrylate, then the polyurethane acrylate segmented copolymer is finely compounded with a nano material with a specific spectrum function, reactive groups, metal selenide and metal oxide nano particles are introduced into a polymer structure, and the spectrum characteristics of different nano particles in polyurethane acrylate resin are utilized, so that specific band spectrums can be selectively transmitted or cut off to accurately regulate and control the filter and color. The optical filtering coating material has the characteristics of excellent optical filtering effect, accurate spectrum interception, high washing fastness, good ageing resistance and rich colors, can be used for various base materials made of different materials, and provides a wider material selection range for the application of optical filtering products.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the filter coating material for precise regulation and protection comprises a component A and a component B, wherein the components comprise the following components in percentage by mass:
and (3) a component A:
72-90% of polyurethane acrylate prepolymer;
0-4% core-shell metal selenide nanoparticles;
0-4% core-shell metal oxide nanoparticles;
9.5 to 19 percent of active diluent;
0.1 to 1 percent of defoaming agent;
wherein the total amount of the core-shell metal selenide particles and the core-shell metal oxide particles is (0.5-4)%;
the polyurethane acrylic ester prepolymer is prepared by carrying out addition reaction on diisocyanate and polyester polyol and then carrying out end capping on hydroxyl acrylic ester;
the core of the core-shell metal selenide nanoparticle is metal selenide, the shell is a surfactant, and the mass ratio of the core to the shell is 1: (0.1-0.3), the particle size of the core-shell metal selenide nano particles is 3-10 nm;
the core of the core-shell metal oxide particle is metal oxide, the shell is surfactant, and the mass ratio of the core to the shell is 1: (0.1-0.5), the particle size of the core-shell metal oxide nano particles is 4-10 nm;
and the component B comprises the following components:
0.4 to 4 percent of photoinitiator.
The filter coating material as described above, preferably, the reactive diluent is at least one of benzyl acrylate, ethoxyphenol acrylate, biphenylmethanol acrylate, o-phenylphenoxyethyl acrylate, 1, 6-hexanediol diacrylate, pentaerythritol triacrylate, or trimethylolpropane triacrylate;
the filter coating material as described above, preferably, the defoaming agent is AT least one of T-1000A type defoaming agent, DS100 silicone oil type defoaming agent, AT350 polyether type defoaming agent, and D90 acrylic polymeric type defoaming agent;
the filter coating material as described above, preferably, the photoinitiator is a radical polymerization photoinitiator.
The filter coating material as described above, preferably, the photoinitiator is selected from: 2-hydroxy-2-methyl-1-phenylpropion, 1-hydroxycyclohexylphenyl ketone, 2-dimethyl-1-phenyl-1-propanone, ethyl 2,4, 6-trimethylbenzoyl phenylphosphonate, 2-dimethylamino-2-benzyl-1-butanone, 2-hydroxy-2-methyl-1-propanone, and 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide; more preferably, the photoinitiator is 2-hydroxy-2-methyl-1-phenylpropionic acid.
The filter coating material as described above, preferably, the diisocyanate is selected from toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate, hexamethylene diisocyanate and/or lysine diisocyanate;
the filter coating material as described above, preferably the polyester polyol is selected from polycaprolactone diol, polyethylene adipate diol, phthalic anhydride polyester diol, and/or polycarbonate diol;
the filter coating material as described above, preferably, the hydroxy acrylate is selected from the group consisting of hydroxyethyl acrylate, hydroxypropyl acrylate and/or hydroxyethyl methacrylate.
The filter coating material as described above, preferably, the metal selenide is at least one of cadmium selenide, zinc selenide, copper selenide, barium selenide, indium selenide, and zirconium selenide;
the surfactant of the core-shell metal selenide particle is as follows: at least one of lauroyl ampholytic sodium acetate, sodium laurylsulfate, lauroyl glutamic acid and fatty alcohol polyoxyethylene ether.
The filter coating material as described above, preferably, the metal oxide is at least one of cadmium oxide, zinc oxide, copper oxide, cobalt oxide, indium oxide, iron oxide, erbium oxide, manganese oxide, titanium oxide, and barium oxide;
the surfactant of the core-shell metal oxide particles is as follows: at least one of stearic acid, alkyl glucoside, sodium dodecyl benzene sulfonate, fatty glyceride and polysorbate.
The filter coating material as described above is preferably a yellow filter coating liquid, the metal selenides are ZnSe and BaSe, and the metal oxides are TiO 2 ；ZnSe、BaSe、TiO 2 The mass ratio of the three is (2-3): 1: (1-2).
The filter coating material as described above is preferably a green filter coating liquid, the metal selenide is CuSe, and the metal oxide is MnO 2 The method comprises the steps of carrying out a first treatment on the surface of the CuSe and MnO 2 The mass ratio of (2) is 1: (3-7).
The filter coating material as described above is preferably a cyan-yellow filter coating liquid, the metal selenide is ZnSe, and the metal oxide is TiO 2 And MnO 2 ；ZnSe、TiO 2 、MnO 2 The mass ratio of the three is (1-2): 1: (1-2).
The filter coating material is preferably blue-green filter coating liquid, wherein the metal selenide is InSe, and the oxide is MnO 2 The method comprises the steps of carrying out a first treatment on the surface of the InSe and MnO 2 The mass ratio of (1-2): 1.
the preparation method of the polyurethane acrylate prepolymer comprises the following steps: polyester polyol and diisocyanate are reacted, the reaction rate is controlled by a catalyst, and then the reaction is blocked by hydroxyethyl acrylate (HEA).
In a preferred embodiment of the present invention, the following urethane acrylate prepolymers are employed and a process for their preparation is provided:
1. polyurethane acrylate prepolymer (PUA-2) Synthesis reaction
2. The preparation method of the polyurethane acrylate prepolymer comprises the following steps: adding polyester diol into a reaction vessel, adding diisocyanate and solvent, and slowly dripping dibutyl tin dilaurate catalyst, N 2 Protecting, controlling the temperature to be 65-80 ℃ for reaction for 60-90min, adding hydroxy acrylic ester and chain extender, cooling to 40-60 ℃, reacting for 2-6h, sampling and detecting the-NCO content, and detecting infrared spectrum 2230-2240 cm -1 The telescopic vibration absorption peak of the-NCO disappears, which shows that the-NCO has completely reacted with the-OH to obtain the polyurethane acrylate prepolymer shown in the formula I; wherein, the mass ratio of the hydroxyl acrylic ester, the diisocyanate and the polyester diol is (1-3): (2-5): (8-10), the mass ratio of the polyester polyol to the solvent is 1: (9-30).
The synthesis of polyurethane acrylic ester (PUA) is a violent exothermic process, and the viscosity increases very fast, if the system viscosity is too big, then the heat is difficult to in time give off, can lead to the system to explode and gather, consequently, replace the polymerization inhibitor through adding the solvent in the synthesis process, reduce the system viscosity on the one hand, help the heat to give off in time, avoid the long-time thermal polymerization of double bond, prevent from gathering, on the other hand, avoid the polymerization inhibitor to lengthen the adverse effect of photocuring time.
In a preferred embodiment of the present invention, the core-shell metal selenide nanoparticle is prepared using the following method:
a. adding sodium borohydride into deionized water, protecting with nitrogen, dissolving, and adding selenium powder, wherein the mass ratio of the sodium borohydride to the selenium powder is 1: (0.1-0.5), magnetically stirring and reacting until the solution becomes colorless transparent selenium-containing solution, wherein the content of selenium in the solution is (3-8) wt%;
b. dissolving soluble metal salt in deionized water, dropwise adding an alkali solution to adjust the pH value to 9-11, and then protecting with nitrogen to obtain a metal salt solution, wherein the concentration of the metal salt in the solution is (5-20) wt%;
c. rapidly adding the selenium-containing solution prepared in the step a into a metal salt solution, stirring and adding a phase transfer agent and a surfactant, wherein the mass ratio of selenium, metal salt, phase transfer agent and surfactant in the solution is 1: (1.5-3.5): (0.1-0.3): (1.5-3), heating and refluxing the mixed solution for 1.5-4.5 hours to obtain selenide nanocrystalline solution;
d. precipitating the prepared selenide nanocrystalline solution by using a precipitator, wherein the mass ratio of the precipitator to the selenium powder in the step a is 1: (0.6-2), washing with deionized water and ethanol as detergents, centrifuging, and drying in a constant temperature drying oven to obtain the core-shell selenide nanocrystalline powder.
The preparation method as described above, preferably, the soluble metal salt is cadmium chloride, zinc chloride, copper chloride, cobalt chloride, indium chloride, barium chloride, cadmium acetate, zinc acetate, copper acetate, cobalt acetate, barium acetate or indium acetate;
the phase transfer agent is at least one selected from sodium acetate, sodium sulfate, ammonia water and sorbitan fatty acid ester;
the surfactant is at least one selected from lauroyl ampholytic sodium acetate, sodium laurylsulfate, lauroyl glutamic acid and fatty alcohol polyoxyethylene ether;
the precipitant is at least one selected from acetone, methyl ethyl ketone, benzene, ethyl acetate and butyl acetate.
In a preferred embodiment of the present invention, the core-shell metal oxide nanoparticles are prepared by the following method:
dissolving metal salt in deionized water to obtain a solution with a concentration of 10 -4 10mol/L of metal salt solution; adding a surfactant aqueous solution and a template agent into a metal salt solution, wherein the mass ratio of the metal salt to the surfactant to the template agent is 1: (0.2-0.5): (0.03-0.1), stirring for 30-120 min to form nano particles with metal oxide nano particle grains as cores and surfactant as shells; and dehydrating, drying to obtain the core-shell metal oxide nano particles.
The preparation method as described above, preferably, the soluble metal salt is a soluble metal salt of metals cadmium, zinc, copper, cobalt, indium, iron, erbium, manganese, titanium and barium;
the surfactant is at least one selected from stearic acid, alkyl glucoside, sodium dodecyl benzene sulfonate, fatty glyceride and polysorbate;
the template agent can maintain template acting force through weak interaction among molecules, so that the size and aggregation of the nano material are precisely controlled, and ethylenediamine, n-butylamine and the like are preferred.
The filter coating formed by the filter coating material consists of polyurethane acrylate polymer, core-shell metal selenide nano particles and core-shell metal oxide nano particles. The surfactant shell of the nano particle ensures that the metal selenide/metal oxide has good dispersibility and fusion degree in the PUA, and meanwhile, the surfactant, the PUA, the metal selenide and the metal oxide cooperate to realize the absorption of light waves in a specific area. Selenide and oxide nanoparticles smaller than 10 nanometers can ensure good light transmittance of the coating while having characteristic light filtering characteristics.
The polyurethane acrylate prepolymer has flexible chain breakage formed by polyester polyol, so that the hardness of the polymerized coating is moderate, the expansion rate before and after polymerization is small, and the polyurethane acrylate prepolymer is suitable for various filter substrate materials. The two ends of the prepolymer are terminated by hydroxyethyl acrylate (HEA), and the terminal double bond can be used as a photopolymerization reaction site.
The invention has the beneficial effects that:
(1) The inorganic nano particles in the components of the filter coating material can enable the absorption spectrum line to migrate through compounding, and have the function of selectively transmitting or cutting off the spectrum with specific wavelength, and the prepared filter has bright color, rich color and high color fastness.
(2) The main polymer molecule of the filter coating material contains chain segments with three chemical structures: urethane blocks formed from diisocyanates, backbones formed from polyols and chain ends formed from hydroxyalkyl acrylates. The acrylic functional group has high transparency and light transmittance, the carbamate has good adhesion and flexibility, has good adhesion to different base materials, does not influence the firmness of the coating after being finely compounded with inorganic nano particles, and does not generate coating stripping and cracking.
(3) The inorganic nano particles in the components of the filter coating material can be prepared through simple reaction conditions, the material composition and the preparation process are simple and convenient, the application cost is reduced to a certain extent, and the product integration defective rate is low.
Drawings
FIG. 1 is a transmission electron micrograph of CdSe nanocrystals prepared in an embodiment.
FIG. 2 is an XRD pattern for CdSe nanoparticles prepared in the examples.
FIG. 3 is an infrared spectrum of urethane acrylate (PUA-2) prepared in example 1.
FIG. 4 is a graph showing the transmittance spectra of CdSe nanoparticles of different contents in polyurethane methyl acrylate.
FIG. 5 is a graph showing the transmittance spectra of iron oxide nanoparticles of different contents in polyurethane methyl acrylate.
FIG. 6 is a graph showing transmittance spectra of the optical filters prepared in example 1.
FIG. 7 is a graph showing transmittance spectra of the optical filters prepared in example 2.
FIG. 8 is a graph showing transmittance spectra of the optical filters prepared in example 3.
FIG. 9 is a graph showing transmittance spectra of the optical filters prepared in example 4.
Fig. 10 is an absorption spectrum of the optical filter prepared in example 4.
Fig. 11 is a transmission electron micrograph of cobalt oxide nanocrystals prepared in an embodiment.
Fig. 12 is an XRD pattern of cobalt oxide nanoparticles prepared in the specific embodiment.
Detailed Description
The invention is further illustrated by the following specific examples, which are not meant to limit the scope of the invention.
1. The nano selenide in each of the following examples was prepared by the following method:
(1) Preparing core-shell cadmium selenide nano particles:
adding 420g of sodium borohydride into 1100g of deionized water, protecting with nitrogen, dissolving, adding 60g of selenium powder, and magnetically stirring to react until no bubbles are generated, thus obtaining colorless transparent selenium-containing solution; adding 140g of cadmium chloride into a reaction container containing 850g of deionized water, and dropwise adding 20% sodium hydroxide alkali solution to adjust the pH value to 11 to obtain a cadmium-containing solution; adding the colorless transparent selenium-containing solution into the cadmium-containing solution, stirring, adding 9.5g of sorbitan fatty acid ester and 135g of lauroyl glutamic acid, heating the solution to 90 ℃ and refluxing for 2.5 hours; adding acetone to make CdSe generate flocculent precipitate, separating, washing and drying to obtain core-shell CdSe nanocrystalline (PX 01).
The obtained core-shell type CdSe nanocrystalline PX01 is observed by a JEM-2100 transmission electron microscope, and is shown in figure 1, the appearance is in the shape of a cubic crystal sphere, the obtained nanocrystalline is uniform in size and good in monodispersity, and the CdSe nanocrystalline grain size is about 4.6nm through analysis and calculation of a Shelle formula (D=K/beta cos theta) and Zeta potential.
XRD testing was performed on the prepared CdSe nanocrystals, and the results were shown in FIG. 2 using an X-ray diffractometer. It was observed that the strong diffraction peak of CdSe was in the 2θ (diffraction angle) range of 10 to 70 °,3 main diffraction peaks appeared, peak positions were located at 2θ≡25.3 °, 42.0 ° and 49.6 °, respectively, corresponding to the (111), (220) and (311) crystal planes of cubic phase CdSe, respectively, wherein the diffraction peak in the (111) direction was particularly strong. These characteristic peaks can correspond one-to-one to diffraction peaks possessed by CdSe nanospheres and are consistent with standard card (JCPLDS No. 65-2891), indicating that sample CdSe has a cubic crystal structure.
(2) Preparation of other core-shell selenide nanoparticles:
by the same method as above, core-shell type ZnSe nanocrystals (PX 02), cuSe nanocrystals (PX 03), baSe nanocrystals (PX 04) and InSe nanocrystals (PX 05) were prepared by replacing cadmium chloride with other metal chloride in equimolar amounts.
2. The nano-oxides in the following examples were prepared using the following methods:
(1) Preparing core-shell cobalt oxide nano particles:
1850mL of aqueous solution of cobalt sulfite with the concentration of 0.8mol/L is prepared, and 95mL of aqueous solution of sodium dodecyl benzene sulfonate with the concentration of 1.8mol/L and 12mL of template n-butylamine are added while stirring. Stirring for several minutes to obtain the final product. And separating, dehydrating and drying to obtain the core-shell CoO nanocrystalline (PS 01).
The obtained core-shell CoO nanocrystalline PS01 is observed by a JEM-2100 transmission electron microscope, and the appearance is similar to a sphere, the obtained nanocrystalline has uniform size, and the CoO nanocrystalline grain diameter is about 6.6nm through analysis and calculation of a Schle formula (D=K/beta cos theta) and Zeta potential.
XRD testing was performed on the prepared CoO nanocrystals, and the characteristic diffraction peaks, which appeared at the positions where 2. Theta. Were 19.0 °, 31.3 °, 36.8 °, 38.5 °, 44.8 °, 55.7 °, 59.4 ° and 65.2 °, were respectively corresponding to the (111), (220), (311), (222), (400), (422), (511) and (440) crystal planes of CoO using an X-ray diffractometer, see FIG. 12, were confirmed to be spinel structures.
(2) Preparation of other core-shell oxide nanoparticles:
by adopting the same method, only cobalt sulfite is replaced by other indissolvable metal salts with equimolar amounts, and core-shell CuO nanocrystalline (PS 02) and Fe are prepared 2 O 3 Nanocrystalline (PS 03), er 2 O 3 Nanocrystalline (PS 04), tiO 2 Nanocrystals (PS 05) and MnO nanocrystals (PS 06).
3. Determining the filter transmission or cut-off wavelength range
The spectrum of the ultraviolet, visible and infrared light is classified according to the spectral band and spectral characteristics of the filtering spectrum, and the light of the selected band passes through and the light outside the passband is cut off. See table one and table two for details.
Table-showing different wavelength filter transmission designs
Design for protecting wavelength of laser
4. Nanocomposite filter function design and chromaticity validation
Determining and grasping the spectral characteristics and the colors of different inorganic nano materials such as selenide, oxide and the like in resin, selecting nano particle colloid with the content of 2%, coating the colloid on the surface of a PC optical substrate, and measuring a cured coating, wherein the details are shown in a third table; finding the red shift relation between the content of the nano material in the resin monomer and the spectral line; the transmission relation between the compounding of different nano materials in the resin monomer and spectral lines is obtained by designing the function of the light filtering coating and matching the chromaticity. FIG. 4 is a graph showing the transmittance of the coating of CdSe nanoparticles with different contents in polyurethane acrylate, and FIG. 5 is a graph showing the transmittance of the coating of iron oxide nanoparticles with different contents in polyurethane acrylate. It can be seen from the figure that the concentration of the nanoparticles in the resin affects the absorption band and the absorption intensity.
Spectral characteristics of the ternary nanocomposite coating
Example 1: preparation of polyurethane acrylate prepolymer, color coating and optical filter
Polyurethane acrylate prepolymer (PUA-2):
(1) Adding 420g isophorone diisocyanate (IPDI) and 7.5Kg methyl ethyl ketone solvent into 380g polycarbonate diol (PCDL 355-6-9, product number: PCDL), slowly dripping 5g dibutyltin dilaurate, reacting for 85min under nitrogen protection at 70deg.C for 25min, sequentially adding 15g1, 4-butanediol, 12g 3-methyl-1, 5-pentanediol, reacting for 90min, adding 220g hydroxyethyl acrylate (HEA), cooling to 50deg.C, reacting for 4 hr and 57 min, and measuring 2236cm -1 at-NCOAnd (5) eliminating the absorption peak of the telescopic vibration, and evaporating the solvent to obtain the PUA-2.
(2) The polyurethane acrylate prepolymer (PUA-2) prepared in the step (1) was subjected to Fourier transform infrared spectroscopy, and as shown in the graph analysis of FIG. 3, 3320cm was obtained -1 The position is a stretching vibration peak of-NH in carbamate, 2955cm -1 is-CH 2 Is 2360cm -1 The peak disappeared, indicating that the-NCO group was substantially completely reacted, 1740cm -1 At C=0, all of which indicate that the-NCO in IPDI reacts with the hydroxyl groups in the diol to form polyurethane, 1640cm -1 There appears a telescopic vibration absorption peak of C=C double bond in hydroxyethyl acrylate, 1240cm -1 The anti-symmetrical stretching vibration peak of the polycarbonate diol O-C=O is shown, and the peak disappears after ultraviolet light curing, which shows that the carbon-carbon double bond effectively participates in the curing and crosslinking reaction.
(II) preparing yellow filter coating and filter
(1) Taking PX02 (ZnSe) 0.7g, PX04 (BaSe) 0.3g and PS05 (TiO) 2 ) 0.5g of the mixture was added to 4.5g of benzyl acrylate, stirred for 30 minutes to uniformly disperse and added to 40g of PUA-2 prepared in the above step, and 0.2g of T-A1000 type antifoaming agent was added to obtain component A.
(2) 1.2g of 1-hydroxycyclohexyl phenyl ketone is weighed and added into the component A, and the components A are uniformly mixed to obtain the prepolymer coating liquid.
(3) Filtering and degassing the pre-polymerized coating liquid through a filter membrane with the aperture of 0.5 mu m, spin-coating the pre-polymerized coating liquid on the surface of an optical glass substrate at the speed of 2500 rpm, and then placing the coating sheet on the surface of the optical glass substrate with the illumination intensity of 200mW/cm 2 The coating was fully cured by irradiation under a UV-LED light curing machine for 33 s. As shown in FIG. 6, the spectral chart of the transmittance of the filter is that the filter absorbs blue light and ultraviolet rays below the 480nm range and transmits visible light in the 570-780nm wavelength range.
Example 2: preparation of polyurethane acrylate prepolymer, color coating and optical filter
Polyurethane acrylate prepolymer (PUA-2):
(1) To 380g of polycarbonate diol, 420g of isophorone diisocyanate (IPDI) and 7.3 g ofKg methyl ethyl ketone solvent, slowly dropwise adding 5g dibutyl tin dilaurate, completely adding 25min, nitrogen protecting, controlling the temperature at 75 ℃ for reaction for 80min, sequentially adding 26g 3-methyl-1, 5-pentanediol for reaction for 90min, adding 210g hydroxyethyl acrylate (HEA), cooling to 50 ℃, reacting for 4 hours and 56 minutes, and measuring 2236cm -1 The stretching vibration absorption peak of the-NCO disappears, and the solvent is distilled off to obtain the PUA-2.
(II) preparing green filter coating and filter
(1) PX03 (CuSe) 0.1g and PS06 (MnO) 2 ) 0.5g of the mixture was added to 4.5g of benzyl acrylate, stirred for 30 minutes to uniformly disperse and added to 40g of PUA-2 prepared in the above step, and 0.2g of T-A1000 type antifoaming agent was added to obtain component A.
(2) 1.2g of 1-hydroxycyclohexyl phenyl ketone is weighed and added into the component A, and the components A are uniformly mixed to obtain the prepolymer coating liquid.
(3) Filtering and degassing the pre-polymerized coating liquid through a filter membrane with the aperture of 0.5 mu m, spin-coating the pre-polymerized coating liquid on the surface of an optical glass substrate at the speed of 2500 rpm, and placing the coating sheet on the surface of the optical glass substrate with the illumination intensity of 200mW/cm 2 The coating was fully cured by irradiation under a UV-LED light curing machine for 28S. As shown in FIG. 7, the spectral chart of the transmittance of the optical filter shows that the optical filter absorbs ultraviolet rays and visible light below 400nm, and transmits visible light in the wavelength range of 500-580nm, so that the absorption peak is narrow and the color is bright.
Example 3: preparation of polyurethane acrylate prepolymer, color coating and optical filter
Polyurethane acrylate prepolymer (PUA-2):
(1) Adding 420g of Hexamethylene Diisocyanate (HDI) and 7.4Kg of methyl ethyl ketone solvent into 380g of polycarbonate diol, slowly dripping 5g of dibutyl tin dilaurate, reacting for 85min at the temperature of 70 ℃ under the protection of nitrogen for 25min, sequentially adding 10g of 1, 4-butanediol and 15g of 3-methyl-1, 5-pentanediol for reacting for 90min, adding 230g of hydroxyethyl acrylate (HEA), cooling to 50 ℃, reacting for 5 h 07 min, and measuring 2236cm -1 the-NCO stretching vibration absorption peak disappears, and the solvent is removed by evaporation to obtain the PUA-2.
(II) preparing a cyan-yellow filter coating and a filter
(1) Taking PX02 (ZnSe) 0.5g、PS02(TiO 2 ) 0.3g and PS06 (MnO 2 ) 0.4g of the mixture was added to 4.5g of benzyl acrylate, stirred for 30 minutes to uniformly disperse and added to 40g of PUA-2 prepared in the above step, and 0.2g of T-A1000 type antifoaming agent was added to obtain component A.
(2) 1.2g of 1-hydroxycyclohexyl phenyl ketone is weighed and added into the component A, and the components A are uniformly mixed to obtain the prepolymer coating liquid.
(3) Filtering and degassing the pre-polymerized coating liquid through a filter membrane with the aperture of 0.5 mu m, spin-coating the pre-polymerized coating liquid on the surface of an optical PC substrate at the speed of 2500 rpm, and placing the coating sheet on the surface of the optical PC substrate with the illumination intensity of 200mW/cm 2 The coating was fully cured by irradiation under a UV-LED light curing machine for 32S. The transmittance spectrum of the filter is shown in figure 8, the filter absorbs ultraviolet light and visible light of 400-450nm, and transmits visible light of 500-570nm wavelength range, and the absorption peak is narrow and the color is bright.
Example 4: preparation of polyurethane acrylate prepolymer, color coating and optical filter
Polyurethane acrylate prepolymer (PUA-2):
(1) Adding 420g of Hexamethylene Diisocyanate (HDI) and 7.6Kg of methyl ethyl ketone solvent into 380g of polycarbonate diol, slowly dripping 5g of dibutyl tin dilaurate, reacting for 85min at the temperature of 70 ℃ under the protection of nitrogen for 25min, sequentially adding 15g of 1, 4-butanediol and 12g of 3-methyl-1, 5-pentanediol for reacting for 90min, adding 240g of hydroxyethyl acrylate (HEA), cooling to 50 ℃, reacting for 4 h and 49 min, and measuring 2236cm -1 The stretching vibration absorption peak of the-NCO disappears, and the solvent is distilled off to obtain the PUA-2.
(II) preparing blue-green filter coating and filter
(1) PX05 (InSe) 0.8g and PS04 (MnO) 2 ) 0.5g of the mixture was added to 4.5g of benzyl acrylate, stirred for 30 minutes to uniformly disperse and added to 40g of PUA-2 prepared in the above step, and 0.2g of T-A1000 type antifoaming agent was added to obtain component A.
(2) 1.2g of 1-hydroxycyclohexyl phenyl ketone is weighed and added into the component A, and the components A are uniformly mixed to obtain the prepolymer coating liquid.
(3) Filtering and degassing the pre-polymerized coating liquid through a filter membrane with the aperture of 0.5 mu m, spin-coating the pre-polymerized coating liquid on the surface of an optical glass substrate at the speed of 2500 rpm, and then placing the coating sheet under a UV-LED photo-curing machine with the illumination intensity of 200mW/cm < 2 >, irradiating for 34S, and completely curing the coating. The transmittance spectrum of the filter is shown in figure 9, the absorption spectrum of the filter is shown in figure 10, the filter absorbs laser beams with 660nm and 690nm wave bands, the absorbance is more than 5A, the visible light with 500-580nm is transmitted, the absorption peak is narrow, and the color is bright.
Example 5: optical Property and colorimetric detection experiments on coatings
The coatings prepared in examples 1-4 were each subjected to optical property testing, the light transmittance being one of the most important properties of the optical material, expressed in terms of transmittance (transmissivity), using a UV-8000 UV visible photometer from Shanghai Meter analysis instruments, inc., testing method: directly placing the sample on an ultraviolet-visible photometer to measure transmittance; the color detection is compared with the standard color plate by naked eyes. The test results are shown in Table IV and FIGS. 6 to 10.
Table IV test sample transmittance (tv) test case
Example 6: light fastness detection of optical filter coatings
The filters prepared in examples 1 to 4 were subjected to a light fastness test, respectively, using a water-cooled xenon lamp test box from Shanghai classical Nuo technology company, and the ultimate exposure conditions were selected, and the irradiation fading color difference reached a time (h) at which the color difference was distinguishable by the naked eye, and the results are shown in Table five.
Table five example samples color fastness to light detection results
Example 7: ageing resistance and stripping adhesion test for optical filter
1. The filters prepared in examples 1 to 4 were subjected to an aging test, respectively, and the samples were subjected to ultraviolet and visible light spectrum detection before and after irradiation in an aging test chamber for 24 hours, and it was found by comparison of the data that the samples detected in examples 1 to 4 were not significantly changed (see Table six).
Table six example samples anti-aging comparison
2. The method comprises the following steps of performing a cross-cut test of an aged sample by using an adhesive tape method, wherein the detection method comprises the following steps of: and (3) scratching the surface of the lens by using a blade, scratching the surface of the lens from a vertical angle, finally leaving 20 square small squares on the surface of the optical filter, adhering the square small squares on the surface of the optical filter by using a 3M invisible adhesive tape, tearing the adhesive tape in the backward direction at a slightly rapid and stable speed, and observing the falling condition of the coating at the cross intersection point cutting position of the grid by using a magnifying glass. The scratch experiment result shows that all the optical filter coatings are free from falling off and stripping, and the adhesive force is good.
Claims (10)
1. The filter coating material for precise regulation and protection is characterized by comprising a component A and a component B, wherein the components comprise the following components in percentage by mass:
and (3) a component A:
72-90% of polyurethane acrylate prepolymer;
0-4% core-shell metal selenide nanoparticles;
0-4% core-shell metal oxide nanoparticles;
9.5 to 19 percent of active diluent;
0.1 to 1 percent of defoaming agent;
wherein the total amount of the core-shell metal selenide particles and the core-shell metal oxide particles is (0.5-4)%;
the polyurethane acrylic ester prepolymer is prepared by carrying out addition reaction on diisocyanate and polyester polyol and then carrying out end capping on hydroxyl acrylic ester;
the core of the core-shell metal selenide nanoparticle is metal selenide, the shell is a surfactant, the mass ratio of the core to the shell is 1:0.1-0.3, and the particle size of the core-shell metal selenide nanoparticle is 3-10 nm;
the core of the core-shell metal oxide particle is metal oxide, the shell is surfactant, the mass ratio of the core to the shell is 1:0.1-0.5, and the particle size of the core-shell metal oxide nanoparticle is 4-10 nm;
and the component B comprises the following components:
0.4 to 4 percent of photoinitiator.
2. The filter coating material of claim 1, wherein the reactive diluent is at least one of benzyl acrylate, ethoxyphenol acrylate, biphenylmethanol acrylate, ortho-phenylphenoxyethyl acrylate, 1, 6-hexanediol diacrylate, pentaerythritol triacrylate, or trimethylolpropane triacrylate;
the defoaming agent is AT least one of T-1000A type defoaming agent, DS100 silicone oil type defoaming agent, AT350 polyether type defoaming agent and D90 acrylic acid polymerization type defoaming agent;
the photoinitiator is a free radical polymerization photoinitiator.
3. The filter coating material of claim 2, wherein the photoinitiator is selected from the group consisting of: 2-hydroxy-2-methyl-1-phenylpropion, 1-hydroxycyclohexylphenyl ketone, 2-dimethyl-1-phenyl-1-propanone, ethyl 2,4, 6-trimethylbenzoyl phenylphosphonate, 2-dimethylamino-2-benzyl-1-butanone, 2-hydroxy-2-methyl-1-propanone, and 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide; more preferably, the photoinitiator is 2-hydroxy-2-methyl-1-phenylpropionic acid.
4. The filter coating material of claim 1, wherein the diisocyanate is selected from toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate, hexamethylene diisocyanate and/or lysine diisocyanate;
the polyester polyol is selected from polycaprolactone diol, polyethylene glycol adipate, phthalic anhydride polyester diol and/or polycarbonate diol;
the hydroxy acrylic ester is selected from hydroxyethyl acrylate, hydroxypropyl acrylate and/or hydroxyethyl methacrylate.
5. The filter coating material of claim 1, wherein the metal selenide is at least one of cadmium selenide, zinc selenide, copper selenide, barium selenide, indium selenide, and zirconium selenide;
the surfactant of the core-shell metal selenide particle is as follows: at least one of lauroyl ampholytic sodium acetate, sodium laurylsulfate, lauroyl glutamic acid and fatty alcohol polyoxyethylene ether.
6. The filter coating material of claim 1, wherein the metal oxide is at least one of cadmium oxide, zinc oxide, copper oxide, cobalt oxide, indium oxide, iron oxide, erbium oxide, manganese oxide, titanium oxide, and barium oxide;
the surfactant of the core-shell metal oxide particles is as follows: at least one of stearic acid, alkyl glucoside, sodium dodecyl benzene sulfonate, fatty glyceride and polysorbate.
7. The filter coating material of any one of claims 1-6, which is a yellow filter coating liquid, wherein the metal selenide is ZnSe and BaSe, and the metal oxide is TiO 2 ；ZnSe、BaSe、TiO 2 The mass ratio of the three components is (2-3) to 1 to (1-2).
8. The filter coating material of any one of claims 1-6, which is a green filter coating liquid, wherein the metal selenide is CuSe and the metal oxide is MnO 2 The method comprises the steps of carrying out a first treatment on the surface of the CuSe and MnO 2 The mass ratio of (3) to (7) is 1.
9. The filter coating material according to any one of claims 1 to 6, which is a cyan-yellow filter coating liquid, wherein the metal selenide is ZnSe, and wherein the goldThe oxide is TiO 2 And MnO 2 ；ZnSe、TiO 2 、MnO 2 The mass ratio of the three components is (1-2) to 1 to (1-2).
10. The filter coating material according to any one of claims 1 to 6, which is a blue-green filter coating liquid, wherein the metal selenide is InSe, and the oxide is MnO 2 The method comprises the steps of carrying out a first treatment on the surface of the InSe and MnO 2 The mass ratio of (1-2) to 1.
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