CN105949379B - A kind of preparation method of nanoparticle and surface optical material and surface optical material - Google Patents
A kind of preparation method of nanoparticle and surface optical material and surface optical material Download PDFInfo
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- CN105949379B CN105949379B CN201610329842.0A CN201610329842A CN105949379B CN 105949379 B CN105949379 B CN 105949379B CN 201610329842 A CN201610329842 A CN 201610329842A CN 105949379 B CN105949379 B CN 105949379B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/043—Drying and spraying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/20—After-treatment of capsule walls, e.g. hardening
- B01J13/22—Coating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/002—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of materials engineered to provide properties not available in nature, e.g. metamaterials
- G02B1/005—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of materials engineered to provide properties not available in nature, e.g. metamaterials made of photonic crystals or photonic band gap materials
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/12—Reflex reflectors
- G02B5/126—Reflex reflectors including curved refracting surface
- G02B5/128—Reflex reflectors including curved refracting surface transparent spheres being embedded in matrix
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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Abstract
The present invention relates to the preparation methods of a kind of nanoparticle and surface optical material and surface optical material.A kind of nanoparticle, the nanoparticle are nucleocapsid, it is characterised in that：The core material of the nanoparticle includes organic or inorganic material, and the Shell Materials of the nanoparticle include elastomeric polymer materials, and the size of the nanoparticle is 100 1000 nanometers.The entirely different preparation process and micro-sphere structure of materials'use described herein, it ensure that excellent strain colour change function and monochromaticjty, considerably increase the speed of production of material, 10 times or more of the output increased of unit interval, while conducive to producing thinner optical thin film.
Description
Technical field
The invention belongs to optical material technical field, it is related to a kind of nanoparticle and surface optical material and surface optical
The preparation method of material.
Background technology
Current coloured decoration, packaging material can be divided into pigment colour and schemochrome two major classes, pigment according to color theory
The material of color includes the material containing extinction or light-reflecting property dyestuff, and schemochrome material is realized using material internal nanostructure
Certain color is obtained to the reflection, refraction and diffraction of light.The material of pigment colour is low to the angular selectivity of light, generally not
It is uniform with angle colorations；The characteristic that the material of schemochrome depends on structure can have not the angle of incident light and the angle of observation
Color is corresponding, and it includes laser film, multi-layer co-extruded molding colorful film etc. to represent material.
Occurred the optical material of the three-dimensional structure reflection light constituted using nanoparticle in other patents or document,
These technologies are substantially is self-assembled into thin layer by inorganic or organic nano microballoon in liquid phase environment, then by it is dry,
Other dielectric material final moldings are penetrated into sintering in gap.However, penetrating into medium in the case of that is not elastomer institute
Prepare that thin layer is hard crisp frangible not to have strain metachrosis；It is combined with medium because of microballoon in the case where penetrating into medium and being elastomer
Power is weaker to cause film to be difficult to straining greatly（30%）It is lower still to keep good strain discoloration.Meanwhile liquid phase assembling is micro-
Structure, which is difficult to avoid that, there are a large amount of faults of construction, and monochromaticjty, brightness and the size of material is made to be a greater impact.Coating transfer radium
It is to realize optical characteristics by imprinting one or more layers micro-structure on polymeric film substrate to penetrate thin film technique, in different angle
Color preference it is poor, film do not have substantially stretch colour change function, be generally below 5% using range of strain.Multiple polymers co-extrusion
Colorful thin film technique is to be layered co-extrusion by extruder by a variety of different polymer then to extend into plural layers realization optics
Characteristic, principle are multilayered interference film, and structure is one-dimentional structure, and it is poor that film stretches colour change function.As patent CN1430551 is public
A kind of multilayer co-extruded ionomeric decorative surfacing in column is opened, including：A) the first coextrusion polymeric layer being made of substantially ionomer；
And b) at least one and the first coextrusion Polymer layer contact coextrusion the second polymer layer, selected from ionomer, from poly-
Object-polyethylene blend and ionomer-polyamide blend.The patent is not directed to the technology of nanoparticle.
Invention content
For overcome the deficiencies in the prior art, a kind of nanoparticle of present invention offer and surface optical material and surface light
The preparation method of material is learned, the entirely different preparation process and micro-sphere structure of materials'use described herein ensure that excellent
Good strain colour change function and monochromaticjty, considerably increase the speed of production of material, 10 times of the output increased of unit interval with
On, while conducive to the thinner optical thin film of production.
The present invention provides the following technical solutions：
A kind of nanoparticle, the nanoparticle are nucleocapsid, the core material of the nanoparticle include it is organic or
The Shell Materials of inorganic material, the nanoparticle include polymer elastomer material, and the size of the nanoparticle is 100-
1000 nanometers.
The size of nanoparticle largely determine materials optical reflection wave band, the wavelength reflected if size is big compared with
Long, the optical wavelength reflected if size is small is partially short；Core layer and shell centainly keep the difference of a refractive index, and shell is follow-up
It is required to deform and melt in process to be filled into the gap of microballoon, needs rational viscoplasticity；Core layer is according to need
To ensure certain rigidity in process.
The optical material of the present invention is since internal nanostructure characteristic causes color constantly to change in different angle, meeting simultaneously
In stress, electric field, temperature, the lower variation that strain occurs and leads to nanostructure lattice variations thus reflected light wave band occurs, in turn
The variation of material appearance color, range of strain is caused there are lasting graduated colors within the scope of strain 0-120%.
Preferably, the core material includes polystyrene, silica, ferroso-ferric oxide, poly-methyl methacrylate
Ester（PMMA）, polyethyl acrylate（PEA）, tin indium oxide（ITO）, arsenic trioxide（ATO）, gold and one kind in silver or several
Kind.
The core material that the present invention selects is at low cost, and synthesis is simple, and method is ripe, strong with the binding ability of other materials,
Refractive index is relatively high.
In any of the above-described scheme preferably, the Shell Materials include polyethyl acrylate, dimethyl silicone polymer
（PDMS）, two fat of polyacrylic acid second, polymethyl methacrylate（PMMA）, polyurethane, polystyrene, oligosaccharide glycol propylene
Sour methyl esters（oligo(ethylene glycol)‐methacrylate）Chemical formula is H2C=C(CH3)CO(OCH2CH2)nO
(CH3), one or more of acrylic compounds and rubber.
Shell Materials elasticity it is excessively high if be easy to keep material too hard, caking property is bad, it is difficult to allow arrangement of microspheres at regular
Lattice structure, viscosity is too low to make material excessively soft, it is difficult to working process and use.Wherein polyethyl acrylate is viscoelastic state
Polymer, while there is suitable elasticity and viscosity.
In any of the above-described scheme preferably, further include transition zone between the core and the shell.
It is attached by transition zone between shell and core.
In any of the above-described scheme preferably, the buffer layer material includes polyethyl acrylate and polymethylacrylic acid
One or more of methyl esters.
In any of the above-described scheme preferably, the core includes accounting for the nucleocapsid mass fraction 20%-40%
Crosslinking agent and core material, the shell include Shell Materials and the Tg adjustings for accounting for the nucleocapsid mass fraction 30%-60%
Agent, the transition zone include accounting for the nucleocapsid mass fraction 5%-20% buffer layer materials.
In any of the above-described scheme preferably, the crosslinking agent accounts for the crosslinking agent and the core material gross mass
1%-15%。
In any of the above-described scheme preferably, the crosslinking agent accounts for the crosslinking agent and the core material gross mass
10%。
In any of the above-described scheme preferably, the mass fraction that the Tg conditioning agents account for the Shell Materials is 0-50%.
In any of the above-described scheme preferably, the mass fraction that the Tg conditioning agents account for the Shell Materials is 0-15%.
In any of the above-described scheme preferably, the core includes accounting for the nucleocapsid mass fraction 20%-40%
Crosslinking agent and polystyrene.
In any of the above-described scheme preferably, the core includes accounting for the friendship of the nucleocapsid mass fraction 32.5%
Join agent and polystyrene.
In any of the above-described scheme preferably, the crosslinking agent accounts for the crosslinking agent and the polystyrene gross mass
1%-15%。
In any of the above-described scheme preferably, the crosslinking agent accounts for the crosslinking agent and the polystyrene gross mass
10%。
In any of the above-described scheme preferably, the crosslinking agent is divinylbenzene（DVB）Or two propylene of 1,3 butylene glycol
Acid esters（BDDA）.
In any of the above-described scheme preferably, the core further includes emulsifier.
In any of the above-described scheme preferably, the emulsifier is Dowfax2A1.
In any of the above-described scheme preferably, the core further includes dispersant.
In any of the above-described scheme preferably, the dispersant is dodecyl sodium sulfate（SDS）.
Emulsifier and dispersant must be added to, and be related to the size for the seed to be formed and the control of growth.SDS is used
Amount number determine the size and number of the polystyrene seed preliminarily formed, to determine final nucleocapsid indirectly
The size of nanoparticle, SDS excessively can cause seed amount excessive, and average-size is smaller, and finally formed nanoparticle is less than
It is expected that size；SDS is excessively few then opposite.
In any of the above-described scheme preferably, the shell includes accounting for the nucleocapsid mass fraction 30%-60%
Polyethyl acrylate and Tg conditioning agents.
In any of the above-described scheme preferably, the shell includes accounting for gathering for the nucleocapsid mass fraction 56.3%
Ethyl acrylate and Tg conditioning agents.
In any of the above-described scheme preferably, the mass fraction that the Tg conditioning agents account for the polyethyl acrylate is 0-
50%。
In any of the above-described scheme preferably, the mass fraction that the Tg conditioning agents account for the polyethyl acrylate is 0-
15%。
In any of the above-described scheme preferably, the Tg conditioning agents are Isobutyl methacrylate（IBMA）.
In any of the above-described scheme preferably, the transition zone includes accounting for the nucleocapsid mass fraction 5%-20% third
Olefin(e) acid ethyl ester and allyl methacrylate.
In any of the above-described scheme preferably, the transition zone includes accounting for the nucleocapsid mass fraction 11.2% the third
Olefin(e) acid ethyl ester and allyl methacrylate.
Ethyl acrylate is the main component monomer of shell, and polymerization is mainly together with allyl methacrylate herein
A transition zone is formed, the transition zone of this ingredient more effective can must connect the polyacrylic acid of the polystyrene and shell of core
Ethyl ester（PEA）.
In any of the above-described scheme preferably, the size dispersity of same nanoparticle is generally below 5%.
Sphere monodisperse, obtained optical material optical property is better, and it is poorer to disperse poorer optical property, 5% time
It is best to learn performance.
In any of the above-described scheme preferably, the nanoparticle is prepared by the method for emulsion polymerization.
The present invention also provides a kind of surface optical material, material includes the nanoparticle of nucleocapsid, the nanoparticle
For above-mentioned nanoparticle.
In any of the above-described scheme preferably, the nanoparticle is formed in three dimensions dense accumulation permutation and combination and is advised
The then mixing of lattice structure, random structure or rule and random structure.
In any of the above-described scheme preferably, dry after prepared by the nanoparticle, the nanoparticle after drying is adding
Added with the sticky mixture with certain fluidity is formed after solvent or specific monomer, it is coated on basement membrane, it is solid by UV light
Change forms elastic film.
In any of the above-described scheme preferably, the organic solvent or specific monomer include 1,3-BDO diacrylate
Ester（BDDA）Or ethyl alcohol.
In any of the above-described scheme preferably, the wavelength of the UV photocurings is 200nm-350nm.
In any of the above-described scheme preferably, the surface optical material improves optics using roll-in and subsequent technique
Performance.
In any of the above-described scheme preferably, the subsequent technique includes concussion shearing micro-structure Regularization technique.
The present invention also provides the preparation methods of the surface optical material, including following steps：
（1）The preparation of the nanoparticle：
（1.1）The preparation of core：Core material and crosslinking agent are mixed at 60-90 DEG C；
（1.2）The preparation of transition zone：Buffer layer material is added again, reaction temperature is 60-90 DEG C；
（1.3）The preparation of shell：Shell Materials and Tg conditioning agents are added again, reaction temperature is 60-90 DEG C, is then broken
Nanoparticle is obtained after breast, drying；
（2）The nanoparticle is processed into surface optical material:
（2.1）By step（1）The nanoparticle of synthesis forms sticky steady after addition organic solvent or specific monomer
Fixed mixture；
（2.2）On the mixture coating basement membrane, protective film is covered on basement membrane；
（2.3）The basement membrane coated is put into UV solidification cases, is taken out after 200-350nm solidifications；
（2.4）Keep its upper and lower surface smooth to get to the surface optical basement membrane microstress roller extruding after solidification
Material.
In any of the above-described scheme preferably, step（1.1）Described in core material and crosslinking agent be added in two portions.
It is in order to form the required seed emulsion of emulsion polymerization, required for being formed greatly that DVB and styrene are added for the first time
Can further add styrene and DVB after small seed makes seed grow up to form the polystyrene sphere for needing size.
In any of the above-described scheme preferably, step（1.1）Middle addition dispersant, main initiator, co initiator and
One or more of emulsifier.
In any of the above-described scheme preferably, the dispersant is dodecyl sodium sulfate.
In any of the above-described scheme preferably, the main initiator is Na2S2O8。
In any of the above-described scheme preferably, the co initiator is Na2S2O5。
In any of the above-described scheme preferably, the emulsifier is Dowfax2A1.
In any of the above-described scheme preferably, step（1.2）Middle addition dispersant.
In any of the above-described scheme preferably, step（1.2）Described in dispersant be dodecyl sodium sulfate.
In any of the above-described scheme preferably, step（1.3）Middle addition dispersant and adjustable refractive index material.
In any of the above-described scheme preferably, step（1.3）Described in dispersant be dodecyl sodium sulfate.
In any of the above-described scheme preferably, step（1.3）Described in adjustable refractive index material be 2,2,2-
trifluoroethyl acrylate （TFMA）.
In any of the above-described scheme preferably, step（1.3）In be additionally added thermal cross-linking agent.
In any of the above-described scheme preferably, step（1.3）Described in thermal cross-linking agent be
hydroxyethylmethacrylate（HEMA）.
In any of the above-described scheme preferably, step（2.1）Middle addition UV cross-linked evocating agents.
In any of the above-described scheme preferably, step（2.1）Described in UV cross-linked evocating agents be Benzophenone.
In any of the above-described scheme preferably, step（2.2）The basement membrane is PET basement membranes.
Surface optical material of the present invention is for packaging material, electronic equipment appearance material, automobile appearance material, dress ornament
Material, sporting goods material, building and ornament materials, currency security strip material, brand material or pattern anti-fake material.
From core by different material preparations, viscoelastic shell exists the nanoparticle shell of surface optical material of the present invention
Continuous phase medium is formed in subsequent technique in softer filler to the gap of ball and ball, depends on the height of microballoon and medium refraction index
The structure of comparison, film can be to be formally or trans-, as shown in Figure 1.
Surface optical material of the present invention constantly changes with the become larger color of material of incident angle, as shown in Figure 2.
It is an object of the invention to prepare nanoparticle assembling by novel optical material preparation technology fast and high quality
Three-D photon crystal thin polymer film, laser film and multilayer interference film material preparation process relatively currently on the market are more
Simply, changeable colors along with angle quality higher, color is easy regulation and control, and has excellent ess-strain colour change function, relative to all solid state
Rolling forming process faster, improves into adaptability of the production to low viscosity raw material, is suitable for the system of more light basis weight material at production speed
Standby, making material include temperature, stress, voltage etc. to environmental stimuli by flexibly changing component has higher corresponding color shifting properties.
The novelty of the present invention is only limited using the targeted material of the technology for preparing photon crystal material similar to coating processes in the past
In the colloidal solution of extremely low viscosity, it is not suitable for the material therefor of the present invention of hyperviscosity system, in addition prepared optics material
Material does not have elasticity, and brittleness is high.The present invention combines coating process and solid-state rolling forming process for material property
Advantage, ensure that the high quality optical performance of material is suitable for while greatly improving production efficiency includes but not limited to fill
The various aspects purposes such as decorations, product packaging surfacing, anti-fake material, sensor indicator, energy saving solar film, photoprotection.
The material of the application has the characteristic sensitive to angle of incidence of light and viewing angle, itself does not contain special suction
Light or reflective dyestuff, optical property is realized by itself nanostructure, this structure and realizes color effect on this basis
Optical principle and other materials have bigger difference；Technical principle used in herein described material is the polymerization by nucleocapsid
Object nanoparticle three dimensions dense accumulation permutation and combination formed certain regular lattice structure, disordered structure or rule with not
Incident ray is selectively reflected specific wave band and angle by the mixing of regular texture by Bragg diffraction principle.This Shen
Please described in the entirely different preparation process and micro-sphere structure of materials'use, ensure that excellent strain colour change function and monochrome
Property.Compared to all solid state roll forming, the addition of coating processes considerably increases the speed of production of material, the yield of unit interval
10 times or more are improved, while conducive to the thinner optical thin film of production.
Description of the drawings
Fig. 1 is the one excellent of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
It selects the material of embodiment to coat and is light-cured into membrane process；
Fig. 2 is Fig. 1 of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
The formal film of the surface optical material of illustrated embodiment and the light of reflective film are into outgoing direction；
Fig. 3 is Fig. 1 of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
The surface optical material of illustrated embodiment is with angle discoloration schematic diagram；
Fig. 4 is Fig. 1 of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
The surface optical material of illustrated embodiment is with angle color change mirror-reflection spectrum example；
Fig. 5 is the use schematic diagram of the embodiment 2 of a kind of nanoparticle of the present invention and surface optical material；
Fig. 6 is the one excellent of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
Select 3.1 application examples of the surface optical material of embodiment；
Fig. 7 is the one excellent of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
Select 3.2 application examples of the surface optical material of embodiment；
Fig. 8 is the one excellent of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
Select 3.2 application examples of the surface optical material of embodiment；
Fig. 9 is the one excellent of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
Select 3.3 application examples of the surface optical material of embodiment；
Figure 10 is the one of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
3.4 application examples of the surface optical material of preferred embodiment；
Figure 11 is the one of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
3.5 application examples of the surface optical material of preferred embodiment；
Figure 12 is the one of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
3.5 application examples of the surface optical material of preferred embodiment；
Figure 13 is the one of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
3.6 application examples of the surface optical material of preferred embodiment；
Figure 14 is the one of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
3.6 application examples of the surface optical material of preferred embodiment；
Figure 15 is the one of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
3.6 application examples of the surface optical material of preferred embodiment；
Figure 16 is the one of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
3.7 application examples of the surface optical material of preferred embodiment；
Figure 17 is the one of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
3.8 application examples of the surface optical material of preferred embodiment；
Figure 18 is the one of the preparation method of a kind of nanoparticle of the present invention and surface optical material and surface optical material
3.8 application examples of the surface optical material of preferred embodiment.
Specific implementation mode
In order to further appreciate that the technical characteristic of the present invention, the present invention is explained in detail with reference to specific embodiment
It states.Embodiment only has illustrative effect to the present invention, without the effect of any restrictions, those skilled in the art
The modification for any unsubstantiality made on the basis of the present invention should all belong to the scope of protection of the present invention.
Embodiment 1：
A kind of surface optical material, material include 320nm sized core-shell structure nano microballoons, and preparation method includes following
Step：
（1）The preparation of the nanoparticle：
Core：Match blender using 10 liters of reaction kettles, argon gas protection is heated to 75 degrees Celsius, premixes 2.6 grams of SDS, and 2800
Gram deionized water, 36 grams of styrene monomers, 4 grams of DVB enter reaction kettle, reaction kettle mixing speed 250rpm, wherein being substituted using DVB
BDDA makes the polystyrene of polymerization have higher refractive index as crosslinking agent, improves optical reflection ratio.Then it is added 0.72 gram
Na2S2O5And 5.18 grams of Na2S2O8.2.3 grams of SDS, 4 grams of NaOH are added with 10ml speed per minute after 20 minutes, 2.2 grams
Dowfax2A1,900 grams of deionized waters, 700 grams of styrene monomers, 70 grams of DVB.
Transition zone：The mixed solution of 0.25 gram of SPS and 5 gram of deionized water composition is added after 30 minutes, after 15 minutes
0.5 gram of SDS, 2.1 grams of Dowfax2A1,320g deionized waters, 250 grams of ethylacrylate are added with speed per minute 14ml
（EA）Monomer and 30 grams of allyl methacrylate（ALMA）Monomer.
Shell：4 grams of SDS are added with 18ml speed per minute after twenty minutes, 2 grams of NaOH, 1600 grams of deionized waters, 1000
Gram butyl acrylate (BA) monomer, 350 grams of i-butyl methacrylate（IBMA）, 42 grams
hydroxyethylmethacrylate（HEMA）And 100 gram 2,2,2-trifluoroethyl acrylate (TFMA)
Shell refractive index is reduced, increases nucleocapsid refractive index contrast and improves optical property.
Completion of dropwise addition carries out demulsification filtering and is dried to obtain nanoparticle agglomerate precursor after 1 hour.
（2）The nanoparticle is processed into surface optical material:
By the butanediol acrylate of obtained nanoparticle and 32% mass fraction（BDDA）And mass fraction
2% Benzophenone is mixed to form sticky stabilized mixture.
In addition the mixture of synthesis is covered using scraper or other tools coated on PET or other basement membranes above
Layer protecting film is put into UV solidification cases, and solidification wavelength is 200-350nm, is taken out after three minutes.Pass through microstress after film
Roll-in is that upper and lower surface is smooth, then so that the queueing discipline of nanoparticle is obtained more preferably by concussion shearing Regularization process
Optical property, as shown in Figure 1.
Fig. 1 is that material coating is light-cured into membrane process：Sticky slurry scraper or other tools are coated uniformly on by a
On PET basement membranes；B affixs surface protection film simultaneously is compacted become the three-decker being close to；C is three one-tenth structures；Film is put after d
Enter in UV curing ovens, the film after being cured is taken out after three minutes；Film is as shown in e and f.
Fig. 2 is that nuclear shell structure nano microballoon prepares composite optical film.Nanoparticle shell is from kernel by different
Material preparation, viscoelastic shell form continuous phase medium in softer filler to the gap of ball and ball in the subsequent process, depend on
It is compared in the height of microballoon and medium refraction index, the structure of film can be formally or trans-.
Fig. 3 is material to change colour schematic diagram with angle, is long wavelength in positive incident and angle of reflection position reflected light, such as red
Color, as incident angle becomes larger, blue shift occurs for reflected light, becomes green and then blue etc. from red.
Fig. 4 be material with angle color change mirror-reflection spectrum example, direction indicated by arrows becomes larger with incident angle
The color of material constantly changes, and wherein the longitudinal axis indicates reflectivity.
The material that the present embodiment obtains, to a certain wavelength specular reflectivity 40% of visible-range, the transmission of the same band
Than being less than 15%, reflection peak and the half-wave width for transmiting paddy are 20-50nm, and the reflection peak of material constantly changes with the variation of angle,
It is highest reflection wavelength when positive incident reflection, blue shift occurs for reflection peak when incidence angle increases.
Embodiment 2：
Completed optical thin-film material prepared by the present invention generally has upper layer and lower layer protective film, takes the circumstances into consideration to take off when in use
The exposure of optical material is directly attached on application target surface as shown in Figure 5 by one surface protective film.
Fig. 5 is that surface optical material concrete application mode is by material（O）Protective film on one side（P）It takes off, then attaches
In the surface substrate Jing Guo cleaning treatment（S）On, the surface roughness of base material is depended on during this can use bonding
Agent can not also use.
Embodiment 3：
Following manner application can be used in surface optical material prepared by embodiment 1：
3.1 packaging materials as shown in FIG. 6.Fig. 6 is that the surface optical material is applied as product packaging material with medicine
For product packing box.After the protective film of this material one side is removed, exposed optical material（O）The height that surface has due to itself
Viscosity, which directly can be pressed or be fitted in, can be attached to product packing box（B）In surfacing such as papery or plastics package
（OB）.
3.2 electromagnetic induction as shown in FIG. 7 and 8.Fig. 7 is using water as the Electrochromic composite material light of flexible electrode material
Learn film applicating example.Film（O）It is attached to one layer of VHB polymeric substrates（V）, have the flexibility that deionized water is done in upper and lower surface
Electrode（W）, the flexible electrode of lower layer is placed in vessel（P）, in extra electric field（V）The light that the lower light source of effect projects is penetrating
The variation of spectral signal is collected after above-mentioned apparatus by spectrometer.
Fig. 8 illustrates for no attaching type application of electrode.Electrochromic composite material film（O）It is embedded in holder coil（R）In,
It is placed on the two poles of the earth of high-tension apparatus（E）Between, voltage（V）Variation causes material strain to change colour.
3.3 electronic equipment appearances as shown in Figure 9.Fig. 9 novel opticals composite materials as by taking iwatch as an example can
Dress the applicating example of electronic equipment appearance.Material is in the form of film or band as wrist strap（B）Or dial plate（R）Or display
Screen（D）Appearance material.
3.4 automobile appearance as shown in Figure 10.Figure 10 is applicating example of the herein described material on automobile appearance.Newly
Type polymeric optical film can be used for vehicle body（B）And vehicle window（W）Film is directed or through viscose and is attached to vehicle by pad pasting
Body or glass surface, outside apply PET or other materials protective layer, and the personalized repacking of vehicle body and vehicle window color may be implemented.
Composite optical film is attached on automobile to be changed with angle different colours.
3.5 mechanically deforms as shown in FIG. 11 and 12.
Figure 11, which is mechanically deform, leads to color-changing composite material applicating example.Undeformed polymer composites optical thin film
（O）There is uniform stretching discoloration property in the case where not there is any additional structure, now the convex stamp with certain pattern
Plate（S）It is pressed on film and realizes pattern transfer.The rough patterning of film surface causes different under identical stress
The strain of position is different, and weaker position should become larger and thicker position should become smaller, different when film is through Tensile
The strain difference of position causes color change inconsistent.Effect same can be by adding certain thickness other one on film
Layer or a few layer films are realized.
Figure 12, which is mechanically deform, leads to electrochromic polymer composite optical material applicating example.Undeformed polymer composite
Expect optical thin film（O）With uniform stretching discoloration property, UV lamp is now utilized（L）Pass through the shade of opening（M）Selectively
The certain characteristic areas of material surface are irradiated, are made using the photocrosslinking agent added in material illuminated partial cross-linked.Cross-linked areas
The Young's modulus of material be much higher than the Young's modulus of uncrosslinked region material, more collection are strained when material is stretched in this way
In in uncrosslinked region, crosslinked areal strain is relatively small.The field color that should become larger changes relatively uncrosslinked area
Domain bigger.Required security pattern can be radiated at material surface in advance by this method, material when not having mechanically deform
Color is uniform, and pattern is stealthy, when material is subjected to mechanically deform since the different pattern of different zones deflection displays.
3.6 pressure sensors as shown in Figure 13,14 and 15.
Figure 13 is color change of the composite optical film after not pressurizeing and pressurizeing, and material heaves two-way drawing after pressurization
It stretches, color is caused to become blue from green, be green when not pressurizeing, be blue after pressurization.
Figure 14 is novel optical composite material as pressure indicator example schematic.Material（O）It is enclosed in balancing gate pit（C）Sense
Answer opening（It is left）, after gas pressurized in balancing gate pit（It is right）, material bulging, which stretches, leads to color change.
Figure 15 is that novel optical composite material makees pressure instruction material schematic diagram applied to football surface.Material（O）Adherency
In football（B）Surface（It is left）, after football inflation（It is right）Material tension-thining leads to color change, low in internal air pressure drop
When this process reverse.
3.7 Application in Building as shown in figure 16.Figure 16 is the application material in architectural appearance（It is left）With it is built-in（It is right）On
Applicating example.Material can be adhered directly to build by way of pad pasting（B）Outer surface glass curtain wall（W）Deng bright and clean table
Face, also building interior door and window（W）, to realize different color demands.
3.8 Application in Anti-counterfeiting as shown in FIG. 17 and 18.
Figure 17 is the application material in currency（C）It is upper to be used as anti-counterfeiting code band（O）Applicating example.For different currency bases
Material, this material can be cut to band and are directly attached on currency base material use as anti-counterfeiting code.
Figure 18 is the application material as trade mark or other purposes pattern anti-fake applicating examples.Except this material is directly pasted
It is attached on base material except use, it can be on material film（OS）It imprints various patterns or one or more layers compound different size is micro-
Material prepared by ball（OP）Different pattern is formed, realizes more complicated antiforge function.
Embodiment 4：
A kind of surface optical material, material include 320nm sized core-shell structure nano microballoons, and preparation method includes following
Step：
（1）The preparation of the nanoparticle：
Core：Match blender using 10 liters of reaction kettles, argon gas protection is heated to 60 degrees Celsius, premixes 2.6 grams of SDS, and 2800
Gram deionized water, 36 grams of styrene monomers, 4 grams of DVB enter reaction kettle, reaction kettle mixing speed 250rpm, wherein being substituted using DVB
BDDA makes the polystyrene of polymerization have higher refractive index as crosslinking agent, improves optical reflection ratio.Then it is added 0.72 gram
Na2S2O5And 5.18 grams of Na2S2O8.2.3 grams of SDS, 4 grams of NaOH are added with 5ml speed per minute after 20 minutes, 2.2 grams
Dowfax2A1,900 grams of deionized waters, 700 grams of styrene monomers, 70 grams of DVB.
Transition zone：The mixed solution of 0.25 gram of SPS and 5 gram of deionized water composition is added after 30 minutes, after 15 minutes
0.5 gram of SDS, 2.1 grams of Dowfax2A1,320g deionized waters, 250 grams of ethylacrylate are added with speed per minute 7ml
（EA）Monomer and 30 grams of allyl methacrylate（ALMA）Monomer.
Shell：4 grams of SDS are added with 9ml speed per minute after twenty minutes, 2 grams of NaOH, 1600 grams of deionized waters, 1000
Gram butyl acrylate (BA) monomer, 350 grams of i-butyl methacrylate（IBMA）, 42 grams
hydroxyethylmethacrylate（HEMA）And 100 gram 2,2,2-trifluoroethyl acrylate (TFMA)
Shell refractive index is reduced, increases nucleocapsid refractive index contrast and improves optical property.
Completion of dropwise addition carries out demulsification filtering and is dried to obtain nanoparticle agglomerate precursor after 1 hour.
（2）The nanoparticle is processed into surface optical material:
By the butanediol acrylate of obtained nanoparticle and 32% mass fraction（BDDA）And mass fraction
2% Benzophenon is mixed to form sticky stabilized mixture.
In addition the mixture of synthesis is covered using scraper or other tools coated on PET or other basement membranes above
Layer protecting film is put into UV solidification cases, and solidification wavelength is 200-350nm, is taken out after three minutes.Pass through microstress after film
Roll-in is that upper and lower surface is smooth, then so that the queueing discipline of nanoparticle is obtained more preferably by concussion shearing Regularization process
Optical property.
Embodiment 5：
A kind of surface optical material, material include 320nm sized core-shell structure nano microballoons, and preparation method includes following
Step：
（1）The preparation of the nanoparticle：
Core：Match blender using 10 liters of reaction kettles, argon gas protection is heated to 90 degrees Celsius, premixes 2.6 grams of SDS, and 2800
Gram deionized water, 36 grams of styrene monomers, 4 grams of DVB enter reaction kettle, reaction kettle mixing speed 250rpm, wherein being substituted using DVB
BDDA makes the polystyrene of polymerization have higher refractive index as crosslinking agent, improves optical reflection ratio.Then it is added 0.72 gram
Na2S2O5And 5.18 grams of Na2S2O8.2.3 grams of SDS, 4 grams of NaOH are added with 15ml speed per minute after 20 minutes, 2.2 grams
Dowfax2A1,900 grams of deionized waters, 700 grams of styrene monomers, 70 grams of DVB.
Transition zone：The mixed solution of 0.25 gram of SPS and 5 gram of deionized water composition is added after 30 minutes, after 15 minutes
0.5 gram of SDS, 2.1 grams of Dowfax2A1,320g deionized waters, 250 grams of ethylacrylate are added with speed per minute 21ml
（EA）Monomer and 30 grams of allyl methacrylate（ALMA）Monomer.
Shell：4 grams of SDS are added with 27ml speed per minute after twenty minutes, 2 grams of NaOH, 1600 grams of deionized waters, 1000
Gram butyl acrylate (BA) monomer, 350 grams of i-butyl methacrylate（IBMA）, 42 grams
hydroxyethylmethacrylate（HEMA）And 100 gram 2,2,2-trifluoroethyl acrylate (TFMA)
Shell refractive index is reduced, increases nucleocapsid refractive index contrast and improves optical property.
Completion of dropwise addition carries out demulsification filtering and is dried to obtain nanoparticle agglomerate precursor after 1 hour.
（2）The nanoparticle is processed into surface optical material:
By the butanediol acrylate of obtained nanoparticle and 32% mass fraction（BDDA）And mass fraction
2% Benzophenon is mixed to form sticky stabilized mixture.
In addition the mixture of synthesis is covered using scraper or other tools coated on PET or other basement membranes above
Layer protecting film is put into UV solidification cases, and solidification wavelength is 200-350nm, is taken out after three minutes.Pass through microstress after film
Roll-in is that upper and lower surface is smooth, then so that the queueing discipline of nanoparticle is obtained more preferably by concussion shearing Regularization process
Optical property.
Claims (52)
1. a kind of surface optical material, material includes the nanoparticle of nucleocapsid, it is characterised in that：The core of the nanoparticle
Core material includes organic material or inorganic material, and the Shell Materials of the nanoparticle include polymer elastomer material, described
The size of nanoparticle is 100-1000 nanometers, the preparation method of the surface optical material, including following steps：
(1) preparation of the nanoparticle：
(1.1) preparation of core：Core material and crosslinking agent are mixed at 60-90 DEG C；
(1.2) preparation of transition zone：Buffer layer material is added again, reaction temperature is 60-90 DEG C；
(1.3) preparation of shell：Shell Materials and Tg conditioning agents are added again, reaction temperature is 60-90 DEG C, is then demulsified, is dry
Nanoparticle is obtained after dry；
(2) nanoparticle is processed into surface optical material：
(2.1) nanoparticle of step (1) synthesis is formed into sticky stabilization after addition organic solvent or specific monomer
Mixture；
(2.2) on the mixture coating basement membrane, protective film is covered on basement membrane；
(2.3) basement membrane coated is put into UV solidification cases, is taken out after 200-350nm solidifications；
(2.4) keep its upper and lower surface smooth to get to the surface optical material basement membrane microstress roller extruding after solidification.
2. surface optical material according to claim 1, it is characterised in that：The core material includes polystyrene, two
In silica, ferroso-ferric oxide, polymethyl methacrylate, polyethyl acrylate, tin indium oxide, arsenic trioxide, gold and silver
One or more.
3. surface optical material according to claim 2, it is characterised in that：The Shell Materials include polyacrylic acid second
Ester, polymethyl methacrylate, polyurethane, polystyrene, oligosaccharide glycol propylene acid methyl esters, is changed dimethyl silicone polymer
Formula is H2C=C (CH3)CO(OCH2CH2)nO(CH3One or more of) and rubber.
4. surface optical material according to claim 3, it is characterised in that：Further include between the core and the shell
Transition zone.
5. surface optical material according to claim 4, it is characterised in that：The buffer layer material includes polyacrylic acid second
One or more of ester and polymethyl methacrylate.
6. surface optical material according to claim 4, it is characterised in that：The core includes accounting for the nucleocapsid matter
The crosslinking agent and core material of score 20%-40% are measured, the shell includes accounting for the nucleocapsid mass fraction 30%-60%
Shell Materials and Tg conditioning agents, the transition zone include account for the nucleocapsid mass fraction 5%-20% buffer layer materials.
7. surface optical material according to claim 6, it is characterised in that：The crosslinking agent accounts for the crosslinking agent and described
The 1%-15% of core material gross mass.
8. surface optical material according to claim 7, it is characterised in that：The crosslinking agent accounts for the crosslinking agent and described
The 10% of core material gross mass.
9. surface optical material according to claim 6, it is characterised in that：The Tg conditioning agents account for the Shell Materials
Mass fraction is 0-50%.
10. surface optical material according to claim 9, it is characterised in that：The Tg conditioning agents account for the Shell Materials
Mass fraction be 0-15%.
11. surface optical material according to claim 4, it is characterised in that：The core includes accounting for the nucleocapsid
The crosslinking agent and polystyrene of mass fraction 20%-40%.
12. surface optical material according to claim 11, it is characterised in that：The core includes accounting for the nucleocapsid
The crosslinking agent and polystyrene of mass fraction 32.5%.
13. surface optical material according to claim 11 or 12, it is characterised in that：The crosslinking agent accounts for the crosslinking agent
With the 1%-15% of the polystyrene gross mass.
14. surface optical material according to claim 13, it is characterised in that：The crosslinking agent accounts for the crosslinking agent and institute
State the 10% of polystyrene gross mass.
15. surface optical material according to claim 11 or 12, it is characterised in that：The crosslinking agent be divinylbenzene or
1,3 butyleneglycol diacrylate.
16. surface optical material according to claim 11, it is characterised in that：The core further includes emulsifier.
17. surface optical material according to claim 16, it is characterised in that：The emulsifier is Dowfax2A1.
18. surface optical material according to claim 11, it is characterised in that：The core further includes dispersant.
19. surface optical material according to claim 18, it is characterised in that：The dispersant is dodecyl sodium sulfonate
Sodium.
20. surface optical material according to claim 11, it is characterised in that：The shell includes accounting for the nucleocapsid
The polyethyl acrylate and Tg conditioning agents of mass fraction 30%-60%.
21. surface optical material according to claim 20, it is characterised in that：The shell includes accounting for the nucleocapsid
The polyethyl acrylate and Tg conditioning agents of mass fraction 56.3%.
22. the surface optical material according to claim 20 or 21, it is characterised in that：The Tg conditioning agents account for described poly- third
The mass fraction of olefin(e) acid ethyl ester is 0-50%.
23. surface optical material according to claim 22, it is characterised in that：The Tg conditioning agents account for the polyacrylic acid
The mass fraction of ethyl ester is 0-15%.
24. the surface optical material according to claim 20 or 21, it is characterised in that：The Tg conditioning agents are metering system
Sour isobutyl ester.
25. surface optical material according to claim 20, it is characterised in that：The transition zone includes accounting for the nucleocapsid knot
Structure mass fraction 5%-20% ethyl acrylates and allyl methacrylate.
26. surface optical material according to claim 25, it is characterised in that：The transition zone includes accounting for the nucleocapsid knot
11.2% ethyl acrylate of structure mass fraction and allyl methacrylate.
27. surface optical material according to claim 1, it is characterised in that：The size dispersity of same nanoparticle
Less than 5%.
28. surface optical material according to claim 1, it is characterised in that：The nanoparticle passes through emulsion polymerization
It is prepared by method.
29. surface optical material according to claim 1, it is characterised in that：The nanoparticle is intensive in three dimensions
Stacked arrangement combines the mixing of formation rule lattice structure, random structure or rule and random structure.
30. surface optical material according to claim 1, it is characterised in that：The nanoparticle is dry after preparing, dry
Nanoparticle afterwards forms the sticky mixture with certain fluidity after addition organic solvent or specific monomer, is coated in base
On film, elastic film is formed by UV photocurings.
31. surface optical material according to claim 30, it is characterised in that：The organic solvent is ethyl alcohol or specific
Monomer is 1,3 butyleneglycol diacrylate.
32. surface optical material according to claim 30, it is characterised in that：The wavelength of the UV photocurings is 200nm-
350nm。
33. surface optical material according to claim 1, it is characterised in that：The surface optical material is using roll-in
And subsequent technique improves optical property.
34. surface optical material according to claim 33, it is characterised in that：The subsequent technique includes that concussion shearing is micro-
Compound with regular structure chemical industry skill.
35. according to the preparation method of any one of the claims 1 to 34 surface optical material, including following steps：
(1) preparation of the nanoparticle：
(1.1) preparation of core：Core material and crosslinking agent are mixed at 60-90 DEG C；
(1.2) preparation of transition zone：Buffer layer material is added again, reaction temperature is 60-90 DEG C；
(1.3) preparation of shell：Shell Materials and Tg conditioning agents are added again, reaction temperature is 60-90 DEG C, is then demulsified, is dry
Nanoparticle is obtained after dry；
(2) nanoparticle is processed into surface optical material:
(2.1) nanoparticle of step (1) synthesis is formed into sticky stabilization after addition organic solvent or specific monomer
Mixture；
(2.2) on the mixture coating basement membrane, protective film is covered on basement membrane；
(2.3) basement membrane coated is put into UV solidification cases, is taken out after 200-350nm solidifications；
(2.4) keep its upper and lower surface smooth to get to the surface optical material basement membrane microstress roller extruding after solidification.
36. according to the preparation method of surface optical material described in claim 35, it is characterised in that：Core described in step (1.1)
Core material and crosslinking agent are added in two portions.
37. according to the preparation method of surface optical material described in claim 35, it is characterised in that：It is added and divides in step (1.1)
One or more of powder, main initiator, co initiator and emulsifier.
38. according to the preparation method of surface optical material described in claim 37, it is characterised in that：The dispersant is dodecane
Base sodium sulfonate.
39. according to the preparation method of surface optical material described in claim 37, it is characterised in that：The main initiator is
Na2S2O8。
40. according to the preparation method of surface optical material described in claim 37, it is characterised in that：The co initiator is
Na2S2O5。
41. according to the preparation method of surface optical material described in claim 37, it is characterised in that：The emulsifier is
Dowfax2A1。
42. according to the preparation method of surface optical material described in claim 35, it is characterised in that：It is added and divides in step (1.2)
Powder.
43. according to the preparation method of surface optical material described in claim 42, it is characterised in that：Divide described in step (1.2)
Powder is dodecyl sodium sulfate.
44. according to the preparation method of surface optical material described in claim 35, it is characterised in that：It is added and divides in step (1.3)
Powder and adjustable refractive index material.
45. according to the preparation method of surface optical material described in claim 44, it is characterised in that：Divide described in step (1.3)
Powder is dodecyl sodium sulfate.
46. according to the preparation method of surface optical material described in claim 45, it is characterised in that：Step is rolled over described in (1.3)
It is 2,2,2- trifluoroethyl acrylate to penetrate rate and adjust material.
47. according to the preparation method of surface optical material described in claim 45, it is characterised in that：Step is additionally added in (1.3)
Thermal cross-linking agent.
48. according to the preparation method of surface optical material described in claim 47, it is characterised in that：It is hot described in step (1.3)
Crosslinking agent is hydroxyethyl methacrylate.
49. according to the preparation method of surface optical material described in claim 35, it is characterised in that：UV is added in step (2.1)
Cross-linked evocating agent.
50. according to the preparation method of surface optical material described in claim 49, it is characterised in that：UV described in step (2.1)
Cross-linked evocating agent is Benzophenone.
51. according to the preparation method of surface optical material described in claim 35, it is characterised in that：Step (2.2) described basement membrane
For PET basement membranes.
52. according to any one of the claims 1 to 34 surface optical material for packaging material, electronic equipment appearance material
Material, automobile appearance material, dress material, sporting goods material, building and ornament materials, currency security strip material, brand material or
Pattern anti-fake material.
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| CN107674457B (en) * | 2017-08-12 | 2020-05-15 | 安徽文峰特种纸业有限公司 | Preparation method of modified silicon dioxide filler for photographic paper ink-absorbing layer coating |
| CN107901519A (en) * | 2017-09-28 | 2018-04-13 | 捷开通讯(深圳)有限公司 | A kind of preparation method of glass substrate, glass substrate and intelligent mobile terminal |
| CN108072927B (en) * | 2017-11-22 | 2020-09-25 | 南通纳科达聚氨酯科技有限公司 | Preparation method and application of anti-blue light film |
| CN108227055B (en) * | 2018-03-14 | 2020-09-25 | 纳琳威纳米科技南通有限公司 | Preparation method and application of visible light reflecting film |
| CN108845380B (en) * | 2018-07-27 | 2020-09-01 | 珠海光驭科技有限公司 | Composite optical material |
| CN109988333B (en) * | 2019-04-04 | 2023-04-07 | 成都爱兴生物科技有限公司 | Polystyrene microsphere |
| WO2021031063A1 (en) * | 2019-08-19 | 2021-02-25 | 苏州科技大学 | Photonic crystal structure-based visualized heat accumulation indicator, manufacturing of same, and applications thereof |
| CN110481107B (en) * | 2019-09-05 | 2024-05-28 | 深圳市摩码克来沃化学科技有限公司 | Dynamic color-changeable film and preparation method thereof |
| CN110908016B (en) * | 2019-10-31 | 2021-06-18 | 珠海光驭科技有限公司 | Composite optical film with photonic crystal structure and preparation method thereof |
| CN110933204A (en) * | 2019-11-22 | 2020-03-27 | Oppo广东移动通信有限公司 | Decoration, cover plate assembly and electronic equipment |
| CN111152210B (en) * | 2020-01-17 | 2021-05-07 | 浙江大学 | Flexible electrohydrodynamic driver |
| CN111363393B (en) * | 2020-03-24 | 2021-05-11 | 珠海光驭科技有限公司 | Coating composition for preparing photonic crystal film, photonic crystal film and preparation method |
| CN111690331B (en) * | 2020-05-07 | 2022-04-12 | 复旦大学 | Transparent heat-insulating anti-ultraviolet film based on photonic quasicrystal material and preparation method thereof |
| CN111923325A (en) * | 2020-07-23 | 2020-11-13 | 东风柳州汽车有限公司 | Integrated surface color-changing structural part and manufacturing method thereof |
| CN113433727B (en) * | 2021-06-18 | 2023-04-07 | 珠海光驭科技有限公司 | Electrochromic optical film and preparation method thereof |
| CN113539392B (en) * | 2021-07-30 | 2022-09-06 | 复旦大学 | FDTD-based structural color microsphere shell preparation method |
| CN115406343A (en) * | 2021-10-28 | 2022-11-29 | 中科韧和科技(山东)有限公司 | Capacitive elastic strain sensor with strain visualization function |
| CN117737886B (en) * | 2024-02-19 | 2024-05-31 | 相变储能(北京)科技有限公司 | Composite phase change fiber and preparation method and application thereof |
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| BR0212478A (en) * | 2001-09-14 | 2004-08-24 | Merck Patent Gmbh | Moldings made of core / shell particles |
| DE10318480A1 (en) * | 2003-04-23 | 2004-11-18 | Itn Nanovation Gmbh | Photonic crystal |
| DE10341198A1 (en) * | 2003-09-04 | 2005-05-19 | Merck Patent Gmbh | Shaped articles with homogeneous, evenly distributed cavities, useful e.g. in electro-optical devices, obtained using core-shell particles having thermoplastic matrix shell and solid core |
| US9561615B2 (en) * | 2011-01-12 | 2017-02-07 | Cambridge Enterprise Limited | Manufacture of composite optical materials |
| CN104029513B (en) * | 2014-06-04 | 2015-12-09 | 绍兴京华激光制品有限公司 | A kind of type compound transparent holographic film production technology |
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