CN109852207B - Dynamic optical coating with changed refractive index and preparation method and use method thereof - Google Patents
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Abstract
The invention belongs to the technical field of optical coatings, and discloses a dynamic optical coating with a changed refractive index, and a preparation method and a use method thereof. The method comprises the following steps: dissolving high molecular resin in a mixed solvent to prepare a high molecular solution; and (3) inserting the substrate into the polymer solution by using a solution pulling method, then pulling the substrate to be above the liquid level, and placing the substrate in an environment with set humidity and temperature to volatilize the solvent so as to obtain the substrate coated with the polymer coating. The invention adopts a solution pulling method to prepare the optical coating, controls optical interference by adjusting the average refractive index and the thickness of the polymer coating, thereby constructing the optical coating with dynamically adjustable reflection spectrum, and when response solvent is dipped and coated on the surface of the coating, the coating generates optical interference and presents rainbow color. After the response solvent evaporated, the coating returned to colorless transparency, and the solvent driven process was reversible. The method has simple process, strong operability and quick color response, and is expected to bring new breakthrough in the application field of optical coatings.
Description
Technical Field
The invention belongs to the technical field of optical coatings, and particularly relates to a dynamic optical coating with a changed refractive index, and a preparation method and a use method thereof.
Background
The structural color generated in nature is mainly caused by thin film interference, multilayer film interference, grating diffraction, light scattering and other reasons, such as opals, scaly wings of butterflies, beetle coleoptera, fish scales, peacock feathers, shells, pearls and the like. The principle of the thin film interference is that complex interference effect occurs when light propagates in an ultrathin multilayer thin film structure to form a specific reflection spectrum, and then different colors are presented. The optical coating is composed of single layer or multiple layers of different materials, and it mainly utilizes optical interference effect and inherent optical characteristics of materials to give different optical functions to the coating, and makes the coating output specific spectrum by controlling the film thickness and selecting different materials. The main methods include vacuum evaporation, cathode sputtering, chemical vapor deposition, ion plating, and conventional optical material coating. Schuler et al (Solar Energy materials 2004,84(1-4): 241-. Roddaro et al (Nano Letter,2007,7(9): 2707-. Mikhail A. Kats et al (Applied Physics Letters,2013,103(10): 101104; Applied Physics Letters,2014,105(13): 131108; Optics and Photonics News,2014,25(1):40-47) break the bottleneck of the traditional low extinction coefficient dielectric material, and realize the color control of the germanium optical coating of the strong absorption material. Therefore, the optical coating is widely researched at home and abroad, but the static optical coating is mainly prepared by some traditional methods, so that the further application of the optical coating in the field of the world is greatly limited. The dynamic optical coating is formed by applying response materials to an optical coating structure to construct the optical coating structure with dynamically adjustable reflection spectrum, and is mainly realized by methods of conversion of amorphous and crystalline states of phase-change materials, periodic change of dielectric constant of photonic crystal hydrogel, change of environmental medium and the like. Chinese patent 201110311787.X discloses a preparation method of bionic temperature control response type intelligent composite optical glass based on nano-scale phase change, which controls the light transmittance of the material by phase separation of reversible nano at critical temperature to prepare a temperature control dynamic reversible optical material. The chinese patent 201610381823.2 cross-links the cholesteric liquid crystal cellulose nanocrystals with the temperature responsive polymer to prepare the humidity responsive photonic crystal composite material. Chinese patent 108641582a reports a method for preparing a temperature-responsive optical reflective coating, which mainly uses the polymerization reaction between acrylate liquid crystal and amine to generate a main-chain cholesteric liquid crystal polymer, and the main-chain cholesteric liquid crystal polymer is coated on a substrate to form the optical reflective coating. The dynamic optical coating based on the change of the environmental medium is still in the preliminary research stage, so the design of the optical coating formula, the analysis of the medium response mechanism, the application of the coating functionalization and the like need to be enhanced, and an optical coating which can obtain the controllable color through a simple method needs to be designed and developed.
Disclosure of Invention
In order to overcome the above-mentioned drawbacks and deficiencies of the prior art, it is a primary object of the present invention to provide a method for producing a dynamic optical coating with a modified refractive index. The preparation method has the advantages of simple process, low cost and strong operability.
Another object of the present invention is to provide a dynamic optical coating with altered refractive index prepared by the above method.
It is a further object of the present invention to provide a method of using the above-described refractive index changing dynamic optical coating. In particular, methods for controlling the color of optical coatings by modulating optical interference in response to a solvent.
The purpose of the invention is realized by the following scheme:
a method of making a refractive index changing dynamic optical coating comprising the steps of: dissolving high molecular resin in a mixed solvent to prepare a high molecular solution; and (3) inserting the substrate into the polymer solution by using a solution pulling method, then pulling the substrate to be above the liquid level, and placing the substrate in an environment with set humidity and temperature to volatilize the solvent so as to obtain the substrate coated with the polymer coating.
In the method of the present invention, the humidity may be 30% to 95%, preferably 50% to 80%.
In the method, the temperature can be 0-150 ℃, and preferably 30-100 ℃.
In the method, the concentration of the polymer resin in the mixed solvent can be 1 g/L-100 g/L; preferably 5g/L to 50 g/L; more preferably 10g/L to 25 g/L.
In the method of the present invention, the polymer resin may be at least one of polyethylene, polypropylene, polystyrene, polylactic acid, polyvinyl chloride, acrylonitrile-butadiene-styrene copolymer, polyurethane, polysulfone, polyamide, polybutylene adipate-terephthalate, polymethyl methacrylate, styrene-butadiene-styrene block copolymer, styrene-isoprene-styrene block copolymer, and other conventional polymer resins.
In order to better implement the method of the present invention, the polymer resin preferably includes at least one of polylactic acid, polystyrene, styrene-butadiene-styrene block copolymer, polymethyl methacrylate, and polybutylene adipate terephthalate.
In the method of the present invention, the average refractive index of the polymer resin is close to or equal to the refractive index of the base material. Specifically, the refractive index of the polymer coating is measured by a refractometer according to the refractive index of the base material, and the components and the formula of the polymer resin are determined.
In the method, the mixed solvent comprises at least two of N, N-dimethylformamide, dimethyl sulfoxide, dichloromethane, dioxane, trichloromethane, tetrahydrofuran, ethyl acetate, dioxane, isopropanol, cyclohexane, acetone, ethanol and water. The mixed solvent is preferably at least two of chloroform, dichloromethane, ethanol and water.
In the method of the present invention, the base material may be a common transparent material, and may include a common glass sheet, a quartz sheet, a silicon wafer, a polyester substrate, a polyimide substrate, a polysulfone resin substrate, a polycarbonate substrate, a polyethylene substrate, a polypropylene substrate, a polyvinyl chloride substrate, a polyurethane substrate, a rubber substrate, or the like.
In the method of the present invention, the substrate is inserted into the polymer solution and then pulled up to a level higher than the liquid surface, and preferably inserted and pulled up at the same speed, and preferably inserted vertically. Preferably immediately after said insertion. The speed can be 100-800 mm/min; preferably 100-500 mm/min.
In the method, the prepared coating is a colorless transparent coating. The thickness of the coating may be 10nm to 2 μm. Preferably 50nm to 1 μm, more preferably 100nm to 800 nm. The method can control the thickness of the coating by controlling the concentration of the polymer solution and the speed of insertion and pulling.
The invention also provides the dynamic optical coating with the changed refractive index prepared by the method.
The invention also provides a use method of the dynamic optical coating with the changed refractive index. The coating is dip-coated with a response solvent, and the coating has rainbow color; after the response solvent evaporated, the coating returned to colorless transparency.
The response solvent may include at least one of tetrahydrofuran, acetone, ethanol, water, isopropanol and ethyl acetate, preferably at least one of ethanol, acetone and water.
The average refractive index of the polymer coating after dip coating is changed, and rainbow color is presented; after the response solvent is volatilized, the coating returns to be colorless and transparent, and the solvent-driven change process is reversible.
The average refractive index is the composite refractive index of the polymer coating and the response solvent.
The optical coating is prepared by adopting a solution pulling method, and the optical interference is controlled by adjusting the average refractive index and the thickness of the polymer coating, so that the optical coating with dynamically adjustable reflection spectrum is constructed, when the average refractive index of the coating is close to that of the substrate, the optical interference is weaker, and the coating is colorless and transparent; when the response solvent is coated on the surface of the coating in a dip mode, the solvent and the film are interacted to swell or shrink, so that the thickness and the average refractive index of the film are changed, the coating is subjected to optical interference, and the coating is iridescent. After the response solvent evaporated, the coating returned to colorless transparency, and the solvent driven process was reversible. The preparation method of the dynamic optical coating has the advantages of simple process, strong operability and quick color response, and is expected to bring new breakthrough in the application field of the optical coating.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the dynamic optical coating with the changed refractive index changes the thickness and the average refractive index of a film by utilizing the swelling and shrinking effects of a solvent on a high molecular resin in the using process, and the process of the solvent-driven dynamic optical coating is reversible.
(2) The preparation method disclosed by the invention is simple in process, strong in operability and fast in color response, and is expected to bring a new breakthrough in the application field of optical coatings.
Drawings
FIG. 1 is a schematic diagram of the preparation method of the present invention.
FIG. 2 is a graph of the color effect exhibited by the film of example 1.
FIG. 3 is a graph of the color effect exhibited by the film of example 2.
FIG. 4 is a graph of the color effect exhibited by the film of example 3.
FIG. 5 is a color effect exhibited by the film of example 4.
FIG. 6 is a color effect exhibited by the film of example 6.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated. Unless otherwise indicated, reagents and materials used in the following examples are commercially available. A schematic diagram of the preparation process of the present invention is shown in FIG. 1.
Example 1
Dissolving 3 parts by mass of high molecular resin polyethylene, 3 parts by mass of polypropylene, 4 parts by mass of polystyrene and 15 parts by mass of polylactic acid in a mixed solvent of 200 parts by mass of N, N-dimethylformamide, 200 parts by mass of dimethyl sulfoxide, 400 parts by mass of dichloromethane, 100 parts by mass of ethyl acetate, 50 parts by mass of dioxane and 50 parts by mass of water to prepare a high molecular solution with the mass volume concentration of 25g/L, vertically inserting a common glass sheet into the solution at a certain speed (the speed is respectively 100 mm/min, 200 mm/min, 300 mm/min, 400 mm/min and 500 mm/min) by adopting a pulling device, immediately vertically pulling the common glass sheet to a position above the liquid level at the same speed, coating the surface of the common glass sheet with a high molecular coating, placing the common glass sheet in an environment with the humidity of 50% and the temperature of 90 ℃, until the solution is completely volatilized, the coating is colorless and transparent. The average refractive index of the polymer coating was 1.5 as measured by an Abbe refractometer. The thickness of the coating was measured by a step profiler and was 125nm, 200nm, 350nm, 410nm, 500nm in this order. The polymer coating is dip-coated with acetone, the average refractive index of the polymer coating after dip-coating is changed, the coating presents rainbow color (as shown in figure 2), the coating is colorless and transparent after the solvent is volatilized, and the dynamic response process is reversible.
Example 2
Dissolving 30 parts by mass of high molecular resin polylactic acid, 10 parts by mass of polyvinyl chloride, 5 parts by mass of acrylonitrile-butadiene-styrene copolymer and 5 parts by mass of polyurethane in a mixed solvent of 650 parts by mass of chloroform, 300 parts by mass of tetrahydrofuran, 10 parts by mass of acetone, 20 parts by mass of isopropanol and 20 parts by mass of cyclohexane to prepare a high molecular solution with the mass volume concentration of 50g/L, vertically inserting a polyethylene substrate into the solution at a certain speed (the speed is respectively 500 mm/min, 550 mm/min, 600 mm/min, 650 mm/min and 800 mm/min) by adopting a lifting device, immediately vertically lifting the polyethylene substrate to a position above the liquid level at the same speed so as to coat the surface of the polyethylene substrate with a high molecular coating, placing the polyethylene substrate in an environment with the humidity of 30% and the temperature of 150 ℃ until the solution is completely volatilized, the coating was colorless and transparent. The average refractive index of the polymer coating was measured by abbe refractometer to be 1.51. The coating thickness was measured by a step meter and was 650nm, 720nm, 800nm, 1 μm, 1.5 μm in this order. The polymer coating is dip-coated with tetrahydrofuran, the average refractive index of the polymer coating after dip-coating is changed, the coating presents rainbow color (as shown in figure 3), the coating is colorless and transparent after the solvent is volatilized, and the dynamic response process is reversible.
Example 3
1 part by mass of high polymer resin polysulfone, 0.5 part by mass of polyamide, 0.5 part by mass of polybutylene adipate terephthalate, 7.5 parts by mass of polymethyl methacrylate and 0.5 part by mass of styrene-butadiene-styrene block copolymer are dissolved in a mixed solvent of 500 parts by mass of dichloromethane, 200 parts by mass of trichloromethane, 250 parts by mass of ethanol and 50 parts by mass of water to prepare a high polymer solution with the mass volume concentration of 10g/L, a pulling device is adopted to vertically insert a polyimide substrate into the solution at a certain speed (the speed is respectively 200 mm/min, 220 mm/min, 240 mm/min, 260 mm/min and 280 mm/min), the polyimide substrate is immediately and vertically pulled to be above the liquid level at the same speed, so that the surface of the polyimide substrate is coated with a high polymer coating, and the polyimide substrate is placed at the humidity of 80%, And (4) the temperature is 45 ℃ until the solution is completely volatilized, and the coating is colorless and transparent. The average refractive index of the polymer coating was 1.48 as measured by an Abbe refractometer. The thickness of the coating was measured by a step profiler and was 300nm, 350nm, 380nm, 420nm, 450nm in this order. The polymer coating is dip-coated with ethanol, the average refractive index of the polymer coating after dip-coating is changed, the coating presents rainbow color (as shown in figure 4), the coating is colorless and transparent after the solvent is volatilized, and the dynamic response process is reversible.
Example 4
70 parts by mass of high molecular resin polymethyl methacrylate, 30 parts by mass of styrene-isoprene-styrene block copolymer and polystyrene are dissolved in 600 parts by mass of dichloromethane, 300 parts by mass of trichloromethane, 50 parts by mass of cyclohexane and 50 parts by mass of ethyl acetate to prepare a high molecular solution with the mass volume concentration of 100g/L, a quartz plate is vertically inserted into the solution at the speed of 500 mm/min by adopting a lifting device, the quartz plate is immediately lifted above the liquid level at the same speed, so that the surface of the quartz plate is coated with a high molecular coating, and the quartz plate is placed in an environment with the humidity of 45% and the temperature of 60 ℃ until the solution is completely volatilized, and the coating is colorless and transparent. The average refractive index of the polymer coating was 1.45 as measured by an Abbe refractometer. The coating thickness was measured by a step meter to be 450 nm. The polymer coating is dip-coated with isopropanol, the average refractive index of the dip-coated polymer coating is changed, the coating presents rainbow colors of yellow, purple and blue from left to right (as shown in figure 5), after the solvent is volatilized, the coating is colorless and transparent, and the dynamic response process is reversible.
Example 5
Dissolving 15 parts by mass of high polymer resin polylactic acid in 950 parts by mass of dichloromethane and 50 parts by mass of water to prepare a high polymer solution with the mass volume concentration of 15g/L, vertically inserting a common glass sheet into the solution at the speed of 400 mm/min by adopting a lifting device, immediately vertically lifting the quartz sheet to a position above the liquid level at the same speed, coating the surface of the quartz sheet with a high polymer coating, and placing the quartz sheet in an environment with the humidity of 70% and the temperature of 0 ℃ until the solution is completely volatilized, wherein the coating is colorless and transparent. The average refractive index of the polymer coating was 1.45 as measured by an Abbe refractometer. The thickness of the coating was 740nm as measured by a step profiler, and the surface of the coating was relatively rough. The polymer coating is dipped in water, the average refractive index of the polymer coating after dip coating is changed, the coating presents rainbow color, the coating is colorless and transparent after the solvent is volatilized, and the dynamic response process is reversible.
Example 6
Dissolving 15 parts by mass of high molecular resin polylactic acid, 10 parts by mass of polymethyl methacrylate and 5g parts by mass of polybutylene adipate terephthalate in a mixed solvent of 300 parts by mass of dichloromethane, 300 parts by mass of trichloromethane, 300 parts by mass of ethyl acetate and 100 parts by mass of water to prepare a high molecular solution with the mass volume concentration of 30g/L, vertically inserting a polyvinyl chloride substrate into the solution at the speed of 100 mm/min by adopting a lifting device, immediately vertically lifting the polyvinyl chloride substrate to a position above the liquid level at the same speed, coating a high molecular coating on the surface of the polyvinyl chloride substrate, and placing the polyvinyl chloride substrate in an environment with the humidity of 35% and the temperature of 80 ℃ until the solution is completely volatilized, wherein the coating is colorless and transparent. The average refractive index of the polymer coating was measured by abbe refractometer to be 1.54. The coating thickness was measured by a step meter to be 1.2 μm. The polymer coating is dipped in water, the average refractive index of the polymer coating after dip coating is changed, the coating presents rainbow colors with different colors from left to right (as shown in figure 6), after the solvent is volatilized, the coating is colorless and transparent, and the dynamic response process is reversible.
Comparative example 1
Dissolving 15 parts by mass of high polymer resin polylactic acid, 10 parts by mass of polymethyl methacrylate and 5 parts by mass of poly (butylene adipate terephthalate) in a mixed solvent of 300 parts by mass of dichloromethane, 200 parts by mass of trichloromethane, 300 parts by mass of ethyl acetate and 100 parts by mass of water to prepare a high polymer solution with the mass volume concentration of 200g/L, vertically inserting a polyvinyl chloride substrate into the solution at the speed of 1000 mm/min by adopting a lifting device, immediately vertically lifting the polyvinyl chloride substrate to be above the liquid level at the same speed, coating the surface of the polyvinyl chloride substrate with a high polymer coating, and placing the polyvinyl chloride substrate in an environment with the humidity of 35% and the temperature of 80 ℃ until the solution is completely volatilized, wherein the coating is colorless and transparent. The average refractive index of the polymer coating was measured by abbe refractometer to be 1.54. The coating thickness was measured by a step meter to be 2.5 μm. The polymer coating is dipped and coated with water, and the coating is still colorless and transparent.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. A method for producing a dynamic optical coating with a modified refractive index, comprising the steps of: dissolving high molecular resin in a mixed solvent to prepare a high molecular solution; inserting the substrate into the polymer solution at a certain speed by using a solution pulling method, pulling the substrate to be above the liquid level at the same speed, and placing the substrate in an environment with set humidity and temperature to volatilize the solvent so as to obtain the substrate coated with the polymer coating;
the high polymer resin is at least one of polyethylene, polypropylene, polystyrene, polylactic acid, polyvinyl chloride, acrylonitrile-butadiene-styrene copolymer, polyurethane, polysulfone, polyamide, polybutylene adipate-terephthalate, styrene-butadiene-styrene block copolymer and styrene-isoprene-styrene block copolymer;
the mixed solvent comprises at least two of N, N-dimethylformamide, dimethyl sulfoxide, dichloromethane, dioxane, trichloromethane, tetrahydrofuran, ethyl acetate, dioxane, isopropanol, cyclohexane, acetone, ethanol and water;
the average refractive index of the polymer resin is close to or equal to the refractive index of the base material.
2. A method of producing a dynamic optical coating with a modified refractive index according to claim 1, characterized in that: the humidity is 30% -95%; the temperature is 0-150 ℃.
3. A method of producing a dynamic optical coating with a modified refractive index according to claim 1, characterized in that: the speed is 100-800 mm/min.
4. A method of producing a dynamic optical coating with a modified refractive index according to claim 1, characterized in that: the concentration of the polymer resin in the mixed solvent is 1 g/L-100 g/L.
5. A method of producing a dynamic optical coating with a modified refractive index according to claim 1, characterized in that: the thickness of the coating is 10 nm-2 mu m.
6. A dynamic optical coating with a modified refractive index, characterized in that it is obtained by the method according to any one of claims 1 to 5.
7. A method of using the refractive index changing dynamic optical coating of claim 6, comprising dip coating the refractive index changing dynamic optical coating of claim 6 in a response solvent, the coating exhibiting a rainbow color; after the response solvent evaporated, the coating returned to colorless transparency.
8. The method of using a dynamic optical coating with refractive index modification according to claim 7, wherein: the response solvent comprises at least one of tetrahydrofuran, acetone, ethanol, water, isopropanol and ethyl acetate.
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