CN110770557B - Visual heat accumulation indicator based on photonic crystal structure and preparation and application thereof - Google Patents
Visual heat accumulation indicator based on photonic crystal structure and preparation and application thereof Download PDFInfo
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- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K11/00—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
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Abstract
The invention relates to a visual heat accumulation indicator based on a photonic crystal structure, and preparation and application thereof. The indicator includes: the composite layer A comprises a substrate A, and at least one surface of the substrate A is provided with a photonic crystal layer; the composite layer B comprises a substrate B, and at least one surface of the substrate B is provided with a viscoelastic polymer. When the surface of the composite layer A, to which the photonic crystal material is attached, is attached to the surface of the composite layer B, to which the viscoelastic polymer is attached, the indicator enters a working state. The invention reflects the heat accumulation process experienced after the reaction starts by utilizing the weakening degree of the photonic crystal structure color, and has great significance for monitoring the heat accumulation process of objects needing to be stored and transported at low temperature.
Description
Technical Field
The invention relates to a visual heat accumulation indicator, in particular to a visual heat accumulation indicator based on a photonic crystal structure, and preparation and application thereof.
Background
Photonic Crystal (Photonic Crystal) was independently proposed by S.John and E.Yablonovith in 1987, and is an artificial microstructure formed by periodically arranging media with different dielectric constants. From a material structure perspective, photonic crystals are a class of artificially designed and manufactured crystals with periodic dielectric structures on the optical scale. The special periodic structure of the Photonic crystal ensures that the Photonic crystal has a forbidden effect on photons with specific wavelength or wave Band to form a Photonic Band Gap, which is similar to an electron energy Band in a semiconductor and is called as a Photonic Band Gap (PBG for short). Like semiconductor materials, the periodic arrangement of dielectric constants creates a certain "potential field" that when the dielectric constants of the two media differ sufficiently, light will interfere and diffract at the interface of the media, creating a photonic band gap where light with energy falling at the band gap will not propagate and will be reflected off in a specular fashion, thus forming a structural color. The reflection reflectivity is high, the spectrum is single, the formed structure is bright and pure in color, and the color cannot be reproduced by using conventional chemical pigments through color mixing.
The structural color of a photonic crystal is directly related to the periodic structure of the material in the optical dimension, and if the structure is destroyed, the structural color decreases until it subsides. If a material medium is selected, the refractive index of the material medium is similar to that of the photonic crystal material, and the material medium is filled in the gaps of the periodic structure of the photonic crystal material, the dielectric constant difference of the photonic crystal medium interface can be reduced, and the interference and diffraction of light at the medium interface can be reduced to weaken the structural color. Further, if the selected filling medium can react with or dissolve the photonic crystal material, so that the two materials are fused together, the photonic crystal structure is further destroyed, the structural color is further weakened, until the two materials are thoroughly fused together, the photonic crystal structure is thoroughly destroyed, and the structural color is also thoroughly disappeared.
It is now known that the degree of color attenuation of a photonic crystal structure correlates with the degree to which the photonic crystal structure is destroyed. The applicant has found that by correlating the extent of such a reaction which causes damage to the photonic crystal structure with the temperature of the reaction and the time of the reaction, the heat accumulation process experienced after the start of the reaction can be reflected by the degree of color weakening of the photonic crystal structure. The visual heat accumulation indicator based on the photonic crystal structure prepared by the principle can indicate the accumulated heat exposure time of an object attached to the visual heat accumulation indicator, and has great significance for monitoring the heat accumulation history of the object needing to be stored and transported at low temperature.
Disclosure of Invention
The invention aims to provide a visual heat accumulation indicator based on a photonic crystal structure, and a preparation method and application thereof.
To achieve one of the objects of the present invention, the present invention provides a visual heat accumulation indicator based on a photonic crystal structure, comprising: a composite layer A and a composite layer B,
the composite layer A comprises a substrate A, wherein at least one surface of the substrate A is provided with a photonic crystal layer;
the composite layer B comprises a substrate B, and at least one surface of the substrate B is provided with a viscoelastic polymer.
When the surface of the composite layer A, to which the photonic crystal layer is attached, is attached to the surface of the composite layer B, to which the viscoelastic polymer is attached, the indicator enters a working state.
The working principle of the indicator is as follows: after the surface of the composite layer A, to which the photonic crystal layer is attached, is attached to the surface of the composite layer B, to which the viscoelastic polymer is attached, the viscoelastic polymer enters into a gap of the photonic crystal material, the refractive index difference between the photonic crystal material and the viscoelastic polymer is reduced, and the structural color is weakened; further, as time goes by, the photonic crystal material is dissolved and fused under the action of the viscoelastic polymer, the refractive index difference between the photonic crystal material and the viscoelastic polymer is further reduced, the structural color is further weakened until the structure of the photonic crystal material is completely destroyed, the photonic crystal material and the viscoelastic polymer are mixed into a single homogeneous material, and the structural color completely disappears. The degree to which the two materials interpenetrate and fuse is related to the reaction temperature and reaction time. The higher the temperature and the longer the time, the greater the degree of structural failure of the photonic crystal material, and the more severe the structural color resolved by its structure, until the photonic crystal material is completely destroyed, the structural color will also completely resolve. Based on this principle, the thermal history experienced by the indicator can be indicated by a macroscopic structural color fading process.
The photonic crystal layer has a photonic band gap structure.
Preferably, the photonic crystal material comprises monodisperse nano-microspheres in close-packed form periodically closely arranged; more preferably, the monodisperse nanoparticle is in the form of a close packed hexagonal close packing.
The raw materials of the monodisperse nano-microsphere are selected from but not limited to: polystyrene, polyacrylate, polymethacrylate, polyacrylic acid, silicon dioxide, aluminum oxide, titanium dioxide, zirconium oxide, ferroferric oxide, polyimide, silicone resin and phenolic resin.
In one embodiment of the present invention, the monodisperse nanoparticle is polystyrene as the starting material.
The refractive index of the monodisperse nano microsphere is 1.0-2.5 (such as 1.0, 1.5, 2.0 and 2.5).
The monodisperse nanoparticle has a Polydispersity (PDI) of less than 5% (e.g., less than 5%, 2%, 1%, 0.5%).
Preferably, the monodisperse nanoparticle has a polydispersity index (PDI) of less than 0.5%.
The particle size of the monodisperse nano microsphere is 80-1100nm (such as 80, 100, 120, 200, 300, 400, 800, 1000, 1100 nm).
Preferably, the monodisperse nanoparticle has a particle size of 120-400nm.
In one embodiment of the invention, the monodisperse nanoparticle size is 215nm.
The forbidden band wavelength of the photonic crystal material is infrared light, visible light or ultraviolet light with the wavelength of 200-2000 nm.
Preferably, the photonic crystal material has a forbidden band wavelength of visible light of 450-640 nm.
The thickness of the photonic crystal layer is 1-50 μm (specifically, 1, 2, 5, 8, 10, 20, 40, 50 μm).
In one embodiment of the invention, the photonic crystal layer has a thickness of 10 μm.
The viscoelastic polymer is selected from, but is not limited to: polyisoprene, atactic polypropylene, polybutadiene, polyisobutylene, silane, vinyl acetate, acrylate methacrylate and styrene.
In one embodiment of the invention, the viscoelastic polymer is a butyl acrylate-styrene-methyl methacrylate terpolymer.
Specifically, in the butyl acrylate-styrene-methyl methacrylate terpolymer, the content of the structural units of butyl acrylate, styrene and methyl methacrylate is 15-25% (such as 15%, 16%, 18%, 20%, 22%, 24%, 25%), 30-40% (such as 30%, 32%, 34%, 35%, 36%, 38%, 40%) and 40-50% (such as 40%, 42%, 44%, 45%, 46%, 48% and 50%) respectively.
In one embodiment of the present invention, the butyl acrylate-styrene-methyl methacrylate terpolymer may have a content of about 20%, 35% and 45% of the butyl acrylate, styrene and methyl methacrylate structural units, respectively.
The viscoelastic polymer has a refractive index of 1.2 to 1.8 (specifically, 1.2, 1.4, 1.6, 1.8).
The viscoelastic polymer has a thickness of 1-50 μm (specifically, 1, 2, 5, 8, 10, 20, 40, 50 μm).
The viscoelastic polymer has a molecular weight of 500000-5000000 (specifically, for example, 500000, 1000000, 1500000, 2000000, 2500000, 3000000, 3500000, 4000000, 4500000, 5000000).
In one embodiment of the invention, the viscoelastic polymer has a thickness of 10 μm.
The starting materials for substrates a and B are independently selected from, but are not limited to: plastic, paper, leather, metal, wood, and ceramic.
Further, the substrate a is transparent.
Further, the substrate B is transparent.
In one embodiment of the present invention, the substrate a is plastic, such as PET plastic.
In one embodiment of the present invention, the substrate B is plastic, such as PET plastic.
Further, a barrier layer C is provided between the composite layer a and the composite layer B.
Working principle: the barrier layer C is used for preventing the composite layer A from reacting with the composite layer B immediately and achieving the purpose of long-term storage of the composite layer A and the composite layer B under the conventional condition. The reaction between composite layer a and composite layer B can be activated by removing the barrier layer C when needed for recording the heat accumulation history.
The barrier layer C is a release film, such as a PET release film, which exhibits low or no chemical permeability to the composite layers a and B, and contains no or little amount of the penetrable composite layer, and when a barrier layer C is disposed between the composite layers a and B, no significant optical change occurs between the composite layers a and B.
Further, the above-mentioned indicator may further comprise an adhesive layer for adhering the indicator to an object to which the indicator is applied, which may be coated on one surface of the indicator using an adhesive agent conventional in the art.
In order to achieve the second object of the present invention, the present invention provides a method for preparing the above-mentioned visual heat accumulation indicator based on photonic crystal structure, comprising the steps of:
1) Coating a photonic crystal material on the substrate A, and drying to obtain a composite layer A;
2) Coating the viscoelastic polymer on the substrate B, and drying to obtain the composite layer B.
Further, the preparation method further comprises the following steps: and a barrier layer C is arranged between the composite layer A and the composite layer B.
To achieve the third object of the present invention, a final aspect of the present invention provides a method of monitoring the thermal history of an object (e.g., an object to be cryogenically stored and/or transported) comprising the step of attaching (e.g., affixing) a visual thermal accumulation indicator of the present invention to the object or to a package of the object. If the vaccine is transported in the cold chain, the visual heat accumulation indicator is stuck on the outer package of the vaccine, and the working state is achieved after the barrier layer C is removed. The fluidity of the composite layer B can be adjusted according to the temperature requirements of different transported objects, so that the requirements can be met.
The invention has the beneficial effects that:
existing products that can implement techniques for visually indicating heat accumulation history can be collectively referred to as time temperature patches (TTI), and are mainly divided into three categories: diffusion TTI, mainly Tempdot in the United kingdom TM The method comprises the steps of carrying out a first treatment on the surface of the PolymerizationReactive VVM mainly used in the United states TM The method comprises the steps of carrying out a first treatment on the surface of the Enzymatic reaction type, mainly referred to as German OnVu TM 。
Compared with the prior art, the invention has the following characteristics:
1) The indication effect provided by the invention is weakening of the color of the photonic crystal structure until the color disappears, the effect is obvious, the visual indication is easy to identify by naked eyes, the indication effect is simple, visual indication is realized, and the indication result is simple, reliable and strong in visual.
2) The indication effects of different heat accumulation stages are all based on the structural colors of the photonic crystal structure, the color spectrum is single, the formed structural colors are bright and pure, the conventional chemical pigments cannot be used for reproduction through color matching, the possibility of counterfeiting and falsifying the real heat accumulation process is eliminated, and the result is non-tamperable.
3) The invention has low cost and is easy to industrialize.
4) The product of the invention has simple structure and is easy to store and transport.
Detailed Description
The invention will be further described with reference to specific embodiments, and advantages and features of the invention will become apparent from the description. These examples are merely exemplary and do not limit the scope of the invention in any way. It will be understood by those skilled in the art that various changes and substitutions of details and forms of the technical solution of the present invention may be made without departing from the spirit and scope of the present invention, but these changes and substitutions fall within the scope of the present invention.
Example 1
(1) Preparing monodisperse nano microspheres:
the monodisperse nano microsphere with the diameter of 215nm is prepared by an emulsion polymerization method, the solid content is 10 percent, and the specific preparation method comprises the following steps:
a) 0.58g of sodium dodecyl sulfate is weighed and dissolved in 90mL of deionized water, and the mixture is stirred in a 250mL three-neck flask at 300r/min, and nitrogen is introduced to bubble for 30min;
b) After heating to 85 ℃ in water bath and stabilizing, adding 5g of styrene;
c) After 15min, 0.1g of potassium persulfate was added, and the mixture was reacted at 85℃for 5 hours under stirring and nitrogen protection, wherein the particle size of the obtained monodisperse nanoparticle was 215nm, and the polydispersity index was DPI=0.02.
Wherein the styrene may be replaced by methyl methacrylate or acrylic acid.
(2) Preparing a composite layer A:
a) Coating the prepared monodisperse nano-microspheres on black PET, drying at 75 ℃, and self-assembling the monodisperse nano-microspheres on the black PET to form photonic crystal materials which are periodically arranged in a close-packed mode; the thickness of the photonic crystal material coating is 10 microns, and the photonic crystal material coating presents bright green structural color;
b) Namely, the composite layer A is prepared;
(3) preparation of viscoelastic polymers:
the butyl acrylate-styrene-methyl methacrylate ternary polymerization viscoelastic polymer is prepared by a solution polymerization method, and the specific preparation method comprises the following steps:
adding an emulsifier (sodium dodecyl sulfate SDS/OP-10 compound), water, part of styrene, butyl acrylate, methyl methacrylate and an initiator into a 500mL four-neck flask, stirring at 300r/min, introducing nitrogen to bubble for 30min, heating to 60 ℃, dropwise adding the rest of monomers (after 10min, dropwise adding the rest of the initiator in 1 h), heating to 75 ℃ in batches, reacting for 3h or so, heating to 90 ℃ after no obvious reflux, preserving heat, reacting for 1h, and cooling to 40 ℃ to obtain the viscoelastic polymer. The content ratio of the butyl acrylate, the styrene and the methyl methacrylate structural units in the polymer is about 20:35:45.
(4) Preparing a composite layer B:
a) Coating the prepared viscoelastic polymer on transparent PET, wherein the thickness of the viscoelastic polymer coating is 10 micrometers;
b) Namely, the composite layer B is prepared;
(5) starting the working state:
the surface of the composite layer A, to which the photonic crystal material is attached, is attached to the surface of the composite layer B, to which the viscoelastic polymer is attached, and then the two surfaces start to react, so that the structural color gradually subsides.
In the present embodiment of the present invention, in the present embodiment,
the composite layer A, B conjugate was exposed to a temperature environment of 0 ℃ and had a structural color complete fade time of 473 hours.
The composite layer A, B conjugate was exposed to a temperature environment of 10 ℃ and had a structural color complete fade time of 274 hours.
The composite layer A, B conjugate was exposed to a temperature environment of 20 ℃ and the structural color was completely resolved for 46 hours.
The composite layer A, B conjugate was exposed to a temperature environment of 30 ℃ and the structural color was completely resolved for 11 hours.
The visual heat accumulation indicator of the embodiment can be used for various foods which need refrigeration or have certain requirements on temperature, such as yoghurt, cake, fresh milk and the like, of life, and can be used for conveniently monitoring the temperature time accumulation of the foods so as to judge whether the foods are fresh or not.
Example 2
(1) Preparing monodisperse nano microspheres:
the monodisperse nano microsphere with the diameter of 215nm is prepared by an emulsion polymerization method, the solid content is 10 percent, and the specific preparation method comprises the following steps:
a) 0.58g of sodium dodecyl sulfate is weighed and dissolved in 90mL of deionized water, and the mixture is stirred in a 250mL three-neck flask at 300r/min, and nitrogen is introduced to bubble for 30min;
b) After heating to 85 ℃ in water bath and stabilizing, adding 5g of styrene;
c) After 15min, 0.1g of potassium persulfate was added, and the mixture was reacted at 85℃for 5 hours under stirring and nitrogen protection, wherein the particle size of the obtained monodisperse nanoparticle was 215nm, and the polydispersity index was DPI=0.02.
Wherein the styrene may be replaced by methyl methacrylate or acrylic acid.
(2) Preparing a composite layer A:
a) Coating the prepared monodisperse nano-microspheres on PET, drying at 75 ℃, and self-assembling the monodisperse nano-microspheres on PET to form photonic crystal materials which are periodically arranged in a close-packed form; the thickness of the photonic crystal material coating is 10 microns, and the photonic crystal material coating presents bright green structural color;
b) Namely, the composite layer A is prepared;
(3) preparation of viscoelastic polymers:
3 different viscoelastic materials of butyl acrylate-styrene-methyl methacrylate ternary polymerization viscoelastic polymers which respectively become mobile phases at 10, 20 and 30 ℃ are prepared by adjusting the mass ratio of three monomers of styrene, butyl acrylate and methyl methacrylate through a solution polymerization method. The preparation method refers to the corresponding procedure of example 1.
(4) Preparing a composite layer B:
a) Uniformly coating the prepared 3 viscoelastic polymers on different area positions of the transparent PET film, wherein the thickness of the viscoelastic polymer coating is 10 micrometers;
b) Namely, the composite layer B is prepared;
(5) starting the working state:
the surface of the composite layer A, to which the photonic crystal material is attached, is attached to the surface of the composite layer B, to which the viscoelastic polymer is attached, and then the two surfaces start to react, so that the structural color gradually subsides.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is to be construed as including any modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
The foregoing embodiments and methods described herein may vary based on the capabilities, experience, and preferences of those skilled in the art. The listing of the steps of a method in a certain order does not constitute any limitation on the order of the steps of the method.
Claims (13)
1. A heat accumulation indicator, comprising: a composite layer A and a composite layer B, wherein,
the composite layer A comprises a substrate A, at least one surface of the substrate A is provided with a photonic crystal layer, the photonic crystal layer comprises a photonic crystal material, and the photonic crystal material is constructed by monodisperse nano microspheres which are periodically and tightly arranged in a hexagonal close-packed mode; the monodisperse nano microsphere is prepared from the following raw materials: one or more of polystyrene, polyacrylate, polymethacrylate, polyacrylic acid, silicon dioxide, aluminum oxide, titanium dioxide, zirconium oxide, ferroferric oxide, polyimide, silicone resin and phenolic resin;
the composite layer B comprises a substrate B, and at least one surface of the substrate B is provided with a viscoelastic polymer;
the viscoelastic polymer is a butyl acrylate-styrene-methyl methacrylate terpolymer, wherein the contents of structural units of butyl acrylate, styrene and methyl methacrylate are respectively 15-25%, 30-40% and 40-50%;
a barrier layer C is arranged between the composite layer A and the composite layer B;
the operating temperature of the heat accumulation indicator is 0-30 ℃.
2. The heat accumulation indicator of claim 1, wherein the butyl acrylate structural unit is present in an amount of 15%, 16%, 18%, 20%, 22%, 24% or 25%; the content of the styrene structural unit is 30%, 32%, 34%, 35%, 36%, 38% or 40%; the methyl methacrylate structural units are 40%, 42%, 44%, 45%, 46%, 48% or 50%.
3. The heat accumulation indicator of claim 1, wherein the monodisperse nanoparticle has a refractive index of 1.0 to 2.5; and/or the viscoelastic polymer has a refractive index of 1.2-1.8.
4. The heat accumulation indicator of claim 1, wherein the monodisperse nanoparticle has a polydispersity of less than 5%; and/or, the particle size of the monodisperse nano microsphere is 80-1100nm.
5. The heat accumulation indicator of claim 1, wherein the monodisperse nanoparticle has a polydispersity of less than 0.5%; and/or, the particle size of the monodisperse nano microsphere is 120-400nm.
6. The heat accumulation indicator of claim 1, wherein the photonic crystal layer has a thickness of 1-50 μm; and/or the viscoelastic polymer has a thickness of 1-50 μm.
7. The heat accumulation indicator of any one of claims 1-6, wherein the starting materials for substrates a and B are independently selected from the group consisting of: plastic, paper, leather, metal, wood, and ceramic.
8. The heat accumulation indicator of claim 7, wherein the substrate a and/or substrate B is transparent.
9. The heat accumulation indicator of claim 1, wherein the substrate a and/or substrate B is PET plastic.
10. The heat accumulation indicator of claim 1, wherein the barrier layer C is a PET release film.
11. A method of making a heat accumulation indicator as claimed in any one of claims 1 to 10 which includes the steps of:
coating a photonic crystal material on the substrate A, and drying to obtain a composite layer A; the method comprises the steps of,
coating a viscoelastic polymer on a substrate B, and drying to obtain a composite layer B, wherein the viscoelastic polymer is a butyl acrylate-styrene-methyl methacrylate terpolymer, and the contents of structural units of butyl acrylate, styrene and methyl methacrylate are respectively 15-25%, 30-40% and 40-50%;
and a step of arranging a barrier layer C between the composite layer A and the composite layer B.
12. The method of producing a heat accumulation indicator according to claim 11, wherein the content of the butyl acrylate structural unit is 15%, 16%, 18%, 20%, 22%, 24% or 25%; the content of the styrene structural unit is 30%, 32%, 34%, 35%, 36%, 38% or 40%; the methyl methacrylate structural units are 40%, 42%, 44%, 45%, 46%, 48% or 50%.
13. A method of monitoring the heat accumulation history of an object comprising the step of attaching a heat accumulation indicator according to any one of claims 1 to 10 to the object or to a package of the object.
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| PCT/CN2019/101315 WO2021031063A1 (en) | 2019-08-19 | 2019-08-19 | Photonic crystal structure-based visualized heat accumulation indicator, manufacturing of same, and applications thereof |
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| CN101023146A (en) * | 2004-09-09 | 2007-08-22 | 蒂萨股份公司 | Method for producing an adhesive strip comprising a thermally cross-linked acrylate hot-melt adhesive layer |
| WO2012100338A1 (en) * | 2011-01-25 | 2012-08-02 | Opalux Incorporated | Photonic crystal device with infiltrating component |
| CN105949379A (en) * | 2016-05-18 | 2016-09-21 | 珠海光驭科技有限公司 | Nanoparticle, surface optical material and preparation method of surface optical material |
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| WO2021031063A1 (en) | 2021-02-25 |
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