CN105949379A - Nanoparticle, surface optical material and preparation method of surface optical material - Google Patents
Nanoparticle, surface optical material and preparation method of surface optical material Download PDFInfo
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- CN105949379A CN105949379A CN201610329842.0A CN201610329842A CN105949379A CN 105949379 A CN105949379 A CN 105949379A CN 201610329842 A CN201610329842 A CN 201610329842A CN 105949379 A CN105949379 A CN 105949379A
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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
-
- 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
-
- 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
- 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
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
-
- 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
Abstract
The invention relates to a nanoparticle, a surface optical material and a preparation method of the surface optical material. The nanoparticle adopts a core-shell structure and is characterized in that a core material of the nanoparticle comprises an organic or inorganic material, a shell material of the nanoparticle comprises an elastomer polymer material, and the nanoparticle has the size ranging from 100 nanometers to 1,000 nanometers. The material adopts entirely different preparation technologies and nanoparticle structures, the excellent strain discoloration function and monochromaticity are guaranteed, the production speed of the material is greatly increased, the yield in unit time is increased by ten times or above, and meanwhile, production of thinner optical films is facilitated.
Description
Technical field
The invention belongs to optical material technical field, relate to a kind of Nano microsphere and surface optical material and the preparation method of surface optical material.
Background technology
The most coloured decoration, packaging material can be divided into pigment colour and the big class of schemochrome two according to color theory, the material of pigment colour includes containing extinction or the material of light-reflecting property dyestuff, and schemochrome material is to utilize material internal nanostructured to realize the reflection to light, refraction and diffraction to obtain certain color.The material of pigment colour is low to the angular selectivity of light, and general different angles color is homogeneous；The material of schemochrome depends on that the angle of the angle of incident illumination and observation can be had no color corresponding by the characteristic of structure, represents material and includes the colorful thin film etc. of laser film, multi-layer co-extruded molding.
The optical material of the three dimensional structure reflection light utilizing Nano microsphere to constitute occurred in other patents or document, these technology are substantially and are self-assembled into thin layer in liquid phase environment by inorganic or organic nano microsphere, are then passed through being dried, sinter or penetrate in gap other dielectric material final molding.But, prepared thin layer in the case of medium is not elastomer is hard crisp frangible does not possess strain metachrosis penetrating into；Thin film is caused to be difficult at the big strain discoloration straining and still keeping good under (30%) in the case of medium is elastomer because microsphere and medium adhesion are more weak penetrating into.Meanwhile, the micro structure that liquid phase assembles is difficult to avoid that a large amount of faults of construction of appearance, makes the monochromaticity of material, brightness and size be a greater impact.Coating transfer laser film technology is to realize optical characteristics by imprinting one or more layers micro structure on polymeric film substrate, poor at the color preference of different angles, and thin film does not the most stretch colour change function, and use range of strain is generally below 5%.Multiple polymers co-extrusion colorful thin film technique is then to extend into plural layers by multiple different polymer by extruder layering co-extrusion to realize optical characteristics, and principle is multilayered interference film, and structure is one-dimentional structure, and thin film stretching colour change function is poor.Such as patent CN1430551 open hurdle one multilayer co-extruded ionomeric decorative surfacing, comprise: a) the first coextrusion polymeric layer being substantially made up of ionomer；And b) at least one coextrusion the second polymer layer with the first coextrusion Polymer layer contact, selected from ionomer, ionomer-polyethylene blend and ionomer-polyamide blend.This patent is not directed to the technology of Nano microsphere.
Summary of the invention
In order to overcome the deficiencies in the prior art, the present invention provides a kind of Nano microsphere and surface optical material and the preparation method of surface optical material, materials'use described herein diverse preparation technology and micro-sphere structure, ensure that excellent strain colour change function and monochromaticity, considerably increase the speed of production of material, the output increased of unit interval more than 10 times, is beneficial to produce thinner optical thin film simultaneously.
The invention provides following technical scheme:
A kind of Nano microsphere, described Nano microsphere is nucleocapsid structure, and the core material of described Nano microsphere includes that organic or inorganic material, the Shell Materials of described Nano microsphere include that polymer elastomer material, the size of described Nano microsphere are 100-1000 nanometer.
The size of Nano microsphere largely determines the wave band of materials optical reflection, and if size is big, the wavelength of reflection is longer, and if size is little, the optical wavelength of reflection is the shortest；Core layer and shell necessarily keep the difference of a refractive index, and shell is required in deformation and the melted space being filled into microsphere during following process, needs rational viscoelasticity；Core layer ensures certain rigidity as required in the course of processing.
The optical material of the present invention causes color to be continually changing in different angles due to internal nanostructure characteristic, nanostructured lattice variations can be caused in stress, electric field, temperature, lower generation strain simultaneously thus the change of reflecting light section occurs, and then causing the change of material appearance color, range of strain has lasting graduated colors in the range of strain 0-120%.
Preferably, one or more during described core material includes polystyrene, silicon dioxide, ferroso-ferric oxide, polymethyl methacrylate (PMMA), polyethyl acrylate (PEA), tin indium oxide (ITO), arsenic trioxide (ATO), gold and silver.
The core material low cost that the present invention selects, synthesis is simple, and method is ripe, and strong with the binding ability of other materials, refractive index is of a relatively high.
In any of the above-described scheme preferably, described Shell Materials includes that polyethyl acrylate, polydimethylsiloxane (PDMS), polyacrylic acid second two fat, polymethyl methacrylate (PMMA), polyurethane, polystyrene, oligosaccharide glycol propylene acid methyl ester (oligo (ethylene glycol) methacrylate) chemical formula are H2C=C(CH3)CO(OCH2CH2)nO(CH3), one or more in acrylic compounds and rubber.
Easily making material too hard if the elasticity of Shell Materials is too high, caking property is bad, is difficult to allow arrangement of microspheres become regular lattice structure, and the lowest meeting of viscosity makes material the softest, it is difficult to processed and use.Wherein polyethyl acrylate is the polymer of viscoelastic state, has the most elastic and viscosity simultaneously.
In any of the above-described scheme preferably, transition zone is also included between described core and described shell.
It is attached by transition zone between shell and core.
In any of the above-described scheme preferably, one or more during described buffer layer material includes polyethyl acrylate and polymethyl methacrylate.
In any of the above-described scheme preferably, described core includes cross-linking agent and the core material accounting for described nucleocapsid structure mass fraction 20%-40%, described shell includes Shell Materials and the Tg regulator accounting for described nucleocapsid structure mass fraction 30%-60%, and described transition zone includes accounting for described nucleocapsid structure mass fraction 5%-20% buffer layer material.
In any of the above-described scheme preferably, described cross-linking agent accounts for described cross-linking agent and the 1%-15% of described core material gross mass.
In any of the above-described scheme preferably, described cross-linking agent accounts for described cross-linking agent and the 10% of described core material gross mass.
In any of the above-described scheme preferably, described Tg regulator accounts for the mass fraction of described Shell Materials is 0-50%.
In any of the above-described scheme preferably, described Tg regulator accounts for the mass fraction of described Shell Materials is 0-15%.
In any of the above-described scheme preferably, described core includes cross-linking agent and the polystyrene accounting for described nucleocapsid structure mass fraction 20%-40%.
In any of the above-described scheme preferably, described core includes cross-linking agent and the polystyrene accounting for described nucleocapsid structure mass fraction 32.5%.
In any of the above-described scheme preferably, described cross-linking agent accounts for described cross-linking agent and the 1%-15% of described polystyrene gross mass.
In any of the above-described scheme preferably, described cross-linking agent accounts for described cross-linking agent and the 10% of described polystyrene gross mass.
In any of the above-described scheme preferably, described cross-linking agent is divinylbenzene (DVB) or 1,3 butylene glycol diacrylate (BDDA).
In any of the above-described scheme preferably, described core also includes emulsifying agent.
In any of the above-described scheme preferably, described emulsifying agent is Dowfax2A1.
In any of the above-described scheme preferably, described core also includes dispersant.
In any of the above-described scheme preferably, described dispersant is dodecyl sodium sulfate (SDS).
Emulsifying agent and dispersant must be added to, and are related to size and the control of growth of the seed of formation.The number of SDS usage amount determines the size and number of the polystyrene seed preliminarily formed, thus indirectly determine the size of final nuclear shell structure nano microsphere, SDS too much can cause seed amount too much, and average-size is less, and the Nano microsphere ultimately formed is less than anticipated size；SDS crosses the most contrary.
In any of the above-described scheme preferably, described shell includes polyethyl acrylate and the Tg regulator accounting for described nucleocapsid structure mass fraction 30%-60%.
In any of the above-described scheme preferably, described shell includes polyethyl acrylate and the Tg regulator accounting for described nucleocapsid structure mass fraction 56.3%.
In any of the above-described scheme preferably, described Tg regulator accounts for the mass fraction of described polyethyl acrylate is 0-50%.
In any of the above-described scheme preferably, described Tg regulator accounts for the mass fraction of described polyethyl acrylate is 0-15%.
In any of the above-described scheme preferably, described Tg regulator is isobutyl methacrylate (IBMA).
In any of the above-described scheme preferably, described transition zone includes accounting for described nucleocapsid structure mass fraction 5%-20% ethyl acrylate and allyl methacrylate.
In any of the above-described scheme preferably, described transition zone includes accounting for described nucleocapsid structure mass fraction 11.2% ethyl acrylate and allyl methacrylate.
Ethyl acrylate is the main component monomer of shell, is here polymerized mainly one transition zone of formation together with allyl methacrylate, and the transition zone of this composition can the more effective polystyrene that must connect core and the polyethyl acrylate (PEA) of shell.
In any of the above-described scheme preferably, the size dispersity of same Nano microsphere is generally below 5%.
Spheroid single dispersing, the optical material optical property obtained is the best, disperses the poorest optical property the poorest, and when 5%, optical property is best.
In any of the above-described scheme preferably, prepared by the method that described Nano microsphere is polymerized by emulsion.
The present invention also provides for a kind of surface optical material, and material includes that the Nano microsphere of nucleocapsid structure, described Nano microsphere are above-mentioned Nano microsphere.
In any of the above-described scheme preferably, described Nano microsphere is in the mixing of three dimensions dense accumulation permutation and combination formation rule lattice structure, random structure or rule with random structure.
In any of the above-described scheme preferably, being dried after the preparation of described Nano microsphere, dried Nano microsphere forms thickness after adding organic solvent or specific monomer and has the mixture of certain fluidity, is coated on basement membrane, forms elastic film by UV photocuring.
In any of the above-described scheme preferably, described organic solvent or specific monomer include 1,3 butylene glycol diacrylate (BDDA) or ethanol.
In any of the above-described scheme preferably, the wavelength of described UV photocuring is 200nm-350nm.
In any of the above-described scheme preferably, described surface optical material improves optical property through roll-in and subsequent technique again.
In any of the above-described scheme preferably, described subsequent technique includes that micro structure Regularization technique is sheared in concussion.
The present invention also provides for the preparation method of described surface optical material, including following steps:
(1) preparation of described Nano microsphere:
(1.1) preparation of core: by core material and cross-linking agent 60-90 DEG C of mixing；
(1.2) preparation of transition zone: being added by buffer layer material, reaction temperature is 60-90 DEG C again；
(1.3) preparation of shell: Shell Materials and Tg regulator being added, reaction temperature is 60-90 DEG C again, then breakdown of emulsion, dried Nano microsphere；
(2) described Nano microsphere is processed into surface optical material:
(2.1) described Nano microsphere step (1) synthesized forms the mixture that thickness is stable after adding organic solvent or specific monomer；
(2.2), on described mixture coating basement membrane, basement membrane is coated with protecting film；
(2.3) basement membrane coated is put in UV solidification case, take out after 200-350nm solidification；
(2.4) make its upper and lower surface smooth basement membrane microstress roller extruding after solidification, i.e. obtain described surface optical material.
In any of the above-described scheme preferably, described in step (1.1), core material and cross-linking agent add the most at twice.
Add for the first time DVB and styrene is to form the seed emulsion required for emulsion polymerization, can add styrene after forming the seed of required size further and DVB makes seed grow up to form the polystyrene sphere needing size.
In any of the above-described scheme preferably, step (1.1) adds one or more in dispersant, main initiator, co initiator and emulsifying agent.
In any of the above-described scheme preferably, described dispersant is dodecyl sodium sulfate.
In any of the above-described scheme preferably, described main initiator is Na2S2O8。
In any of the above-described scheme preferably, described co initiator is Na2S2O5。
In any of the above-described scheme preferably, described emulsifying agent is Dowfax2A1.
In any of the above-described scheme preferably, step (1.2) adds dispersant.
In any of the above-described scheme preferably, described in step (1.2), dispersant is dodecyl sodium sulfate.
In any of the above-described scheme preferably, step (1.3) adds dispersant and adjustable refractive index material.
In any of the above-described scheme preferably, described in step (1.3), dispersant is dodecyl sodium sulfate.
In any of the above-described scheme preferably, described in step (1.3), adjustable refractive index material is 2,2,2-trifluoroethyl
Acrylate (TFMA).
In any of the above-described scheme preferably, step (1.3) is additionally added thermal cross-linking agent.
In any of the above-described scheme preferably, described in step (1.3), thermal cross-linking agent is hydroxyethylmethacrylate(HEMA).
In any of the above-described scheme preferably, step (2.1) adds UV cross-linked evocating agent.
In any of the above-described scheme preferably, described in step (2.1), UV cross-linked evocating agent is Benzophenone.
In any of the above-described scheme preferably, step (2.2) described basement membrane is PET basement membrane.
Surface optical material of the present invention is for packaging material, electronic equipment appearance material, automobile appearance material, dress material, sporting goods material, building and ornament materials, currency security strip material, brand material or pattern anti-fake material.
The Nano microsphere shell of surface optical material of the present invention is prepared by different materials from core, viscoelastic shell softer filler in subsequent technique forms continuous phase medium in the gap of ball and ball, depend on the height contrast of microsphere and medium refraction index, the structure of thin film can be formally can also be for trans, as shown in Figure 1.
The color that surface optical material of the present invention becomes big material along with incident angle is continually changing, as shown in Figure 2.
It is an object of the invention to prepare, by novel optical material preparation technology fast and high quality, the three-D photon crystal thin polymer film that Nano microsphere assembles, laser film and multilayer interference film material preparation process the most in the market are simpler, changeable colors along with angle quality is higher, color easily regulates and controls, and have excellent ess-strain colour change function, become to produce speed faster relative to all solid state rolling forming process, improve into the product adaptability to low viscosity raw material, it is applicable to the preparation of more light basis weight material, make material stimulate to external world by change component flexibly and include temperature, stress, voltage etc. have higher corresponding color shifting properties.The novelty of the present invention is, the material using similar coating processes to prepare the technology of photon crystal material targeted in the past is only limitted to the most low viscous colloid solution, not being suitable for the material therefor of the present invention of hyperviscosity system, additionally prepared optical material does not possess elasticity, and fragility is high.The present invention is directed to material behavior and combine coating process and the advantage of solid-state rolling forming process, while being greatly improved production efficiency, ensure that the high quality optical performance of material is applicable to include but not limited to each side purposes such as decoration, product surface of package material, anti-fake material, sensor indicator, energy-conservation solar film, photoprotection.
The material of the application has the characteristic sensitive to light angle and viewing angle, itself do not contain special extinction or reflective dyestuff, optical property relies on self nanostructured to realize, this structure and realize the optical principle of color effect on this basis and have bigger difference with other materials；Know-why used by herein described material is that incident ray is reflected specific wave band and angle through Bragg diffraction principle by mixing selectively that form certain regular lattice structure, disordered structure or rule and irregular structure in three dimensions dense accumulation permutation and combination by the polymer nano-microspheres of nucleocapsid structure.Materials'use described herein diverse preparation technology and micro-sphere structure, it is ensured that excellent strain colour change function and monochromaticity.Compared to all solid state roll forming, the addition of coating processes considerably increases the speed of production of material, the output increased of unit interval more than 10 times, is beneficial to produce thinner optical thin film simultaneously.
Accompanying drawing explanation
Fig. 1 is that the material coating of a preferred embodiment of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material is light-cured into membrane process；
Fig. 2 is the formal thin film light turnover direction with reflective film of the described surface optical material of the embodiment illustrated in fig. 1 of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material；
Fig. 3 is that the described surface optical material of the embodiment illustrated in fig. 1 of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material is with angle variable color schematic diagram；
Fig. 4 is that the described surface optical material of the embodiment illustrated in fig. 1 of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material changes direct reflection spectrum example with angle color；
Fig. 5 is the use schematic diagram of the embodiment 2 of a kind of Nano microsphere of the present invention and surface optical material；
Fig. 6 is 3.1 application examples of the surface optical material of a preferred embodiment of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material；
Fig. 7 is 3.2 application examples of the surface optical material of a preferred embodiment of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material；
Fig. 8 is 3.2 application examples of the surface optical material of a preferred embodiment of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material；
Fig. 9 is 3.3 application examples of the surface optical material of a preferred embodiment of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material；
Figure 10 is 3.4 application examples of the surface optical material of a preferred embodiment of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material；
Figure 11 is 3.5 application examples of the surface optical material of a preferred embodiment of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material；
Figure 12 is 3.5 application examples of the surface optical material of a preferred embodiment of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material；
Figure 13 is 3.6 application examples of the surface optical material of a preferred embodiment of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material；
Figure 14 is 3.6 application examples of the surface optical material of a preferred embodiment of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material；
Figure 15 is 3.6 application examples of the surface optical material of a preferred embodiment of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material；
Figure 16 is 3.7 application examples of the surface optical material of a preferred embodiment of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material；
Figure 17 is 3.8 application examples of the surface optical material of a preferred embodiment of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material；
Figure 18 is 3.8 application examples of the surface optical material of a preferred embodiment of the preparation method of a kind of Nano microsphere of the present invention and surface optical material and surface optical material.
Detailed description of the invention
In order to further appreciate that the technical characteristic of the present invention, below in conjunction with specific embodiment, the present invention is set forth in.Embodiment only has exemplary effect to the present invention, and does not have any restrictive effect, and the amendment of any unsubstantiality that those skilled in the art makes on the basis of the present invention all should belong to protection scope of the present invention.
Embodiment
1
:
A kind of surface optical material, material includes 320nm sized core-shell structure nano microsphere, and preparation method includes following steps:
(1) preparation of described Nano microsphere:
Core: use 10 liters of reactors to join agitator; argon shield; it is heated to 75 degrees Celsius; premix 2.6 grams of SDS, 2800 grams of deionized waters, 36 grams of styrene monomers; 4 grams of DVB enter reactor; reactor mixing speed 250rpm, wherein uses DVB to substitute BDDA and makes the polystyrene of polymerization have higher refractive index as cross-linking agent, improve optical reflection ratio.It is subsequently adding 0.72 gram of Na2S2O5And 5.18 grams of Na2S2O8.2.3 grams of SDS, 4 grams of NaOH, 2.2 grams of Dowfax2A1,900 grams of deionized waters, 700 grams of styrene monomers, 70 grams of DVB are added with 10ml speed per minute after 20 minutes.
Transition zone: add 0.25 gram of SPS and the mixed solution of 5 grams of deionized water compositions after 30 minutes, 0.5 gram of SDS is added with speed per minute for 14ml after 15 minutes, 2.1 grams of Dowfax2A1,320g deionized water, 250 grams of ethylacrylate(EA) monomer and 30 grams of allyl methacrylate(ALMA) monomer.
Shell: add 4 grams of SDS, 2 grams of NaOH, 1600 grams of deionized waters, 1000 grams of butyl acrylate (BA) monomers, 350 grams of i-butyl with speed per minute for 18ml after 20 minutes
Methacrylate(IBMA), 42 grams of hydroxyethylmethacrylate(HEMA), and 100 gram 2,2,2-trifluoroethyl
Acrylate (TFMA) reduces shell refractive index, increases nucleocapsid refractive index contrast and improves optical property.
Completion of dropwise addition carries out breakdown of emulsion filtration and is dried to obtain Nano microsphere agglomerate precursor after 1 hour.
(2) described Nano microsphere is processed into surface optical material:
By the butanediol acrylate(BDDA of the Nano microsphere obtained and 32% mass fraction) and the Benzophenone mix and blend formation thickness stabilized mixture of mass fraction 2%.
Using scraper or other instruments to be coated on PET or other basement membranes in the mixture of synthesis, cover other layer protecting film above, put in UV solidification case, solidification wavelength is 200-350nm, takes out after three minutes.It is that upper and lower surface is smooth through microstress roll-in after thin film, is then passed through shaking cutting rule integralization process and makes the queueing discipline of Nano microsphere obtain more preferably optical property, as shown in Figure 1.
Fig. 1 is that material coating is light-cured into membrane process: a and slurry scraper or other instruments of thickness is coated uniformly on PET basement membrane；B affix surface protection film also is compacted become the three-decker being close to；C is three one-tenth structures；Thin film is put in UV curing oven after d, after three minutes, take out the thin film after being solidified；Thin film is as shown in e and f.
Fig. 2 is that composite optical thin film prepared by nuclear shell structure nano microsphere.Nano microsphere shell is prepared by different materials from kernel, viscoelastic shell softer filler in subsequent technique forms continuous phase medium in the gap of ball and ball, depending on the height contrast of microsphere and medium refraction index, the structure of thin film can be formally can also be for trans.
Fig. 3 is material with angle variable color schematic diagram, and incident in front and angle of reflection position reflection light is long wavelength, such as red, along with incident angle becomes big, reflects light generation blue shift, redness become green then blue etc..
Fig. 4 is that material changes direct reflection spectrum example with angle color, and the color that direction indicated by arrows becomes big material along with incident angle is continually changing, and wherein the longitudinal axis represents reflectance.
The material that the present embodiment obtains, a certain wavelength specular reflectivity 40% to visible-range, the transmittance of the same band is less than 15%, the a width of 20-50nm of half-wave of reflection peak and transmission paddy, the reflection peak of material is continually changing with the change of angle, it is the highest reflection wavelength when front incidence reflection, reflection peak generation blue shift when that angle of incidence increasing.
Embodiment
2
:
Completed optical thin-film material prepared by the present invention typically has upper and lower two-layer protecting film, takes the circumstances into consideration when in use to take a surface protective film off, by the exposure of optical material directly against being combined on application target surface as shown in Figure 5.
Fig. 5 be the concrete application mode of surface optical material be by material (O) one side protecting film (P) take off; then it is attached on the surface substrate (S) that cleaning processes, during this, depends on that the surface roughness of base material can use binding agent not use.
Embodiment
3
:
The surface optical material of embodiment 1 preparation can be applied in the following ways:
3.1 packaging material as shown in Figure 6.Fig. 6 is that described surface optical material is applied as a example by medicine packing box as product packaging material.After being removed by the protecting film of this material one side, the high viscosity that optical material (O) surface of exposure has due to self can directly can be attached in product packing box (B) surfacing such as papery or plastics package (OB) in pressing or be fitted in.
3.2 electromagnetic induction as shown in FIG. 7 and 8.Fig. 7 is the Electrochromic composite material optical thin film applicating example with water as flexible electrode material.Thin film (O) is attached to one layer of VHB polymeric substrates (V), the flexible electrode (W) that deionized water does is had at upper and lower surface, the flexible electrode of lower floor is placed in vessel (P), and under extra electric field (V) acts on, the light of light source injection is collected the change of spectral signal after penetrating said apparatus by spectrogrph.
Fig. 8 is to illustrate without attaching type application of electrode.Electrochromic composite material thin film (O) is embedded in support coil (R), is placed between the two poles of the earth (E) of high pressure equipment, and voltage (V) change causes material strain variable color.
3.3 electronic equipment outward appearances as shown in Figure 9.Fig. 9. novel optical composite is as the applicating example of the wearable electronic outward appearance as a example by iwatch.Material is using the form of thin film or band as wrist strap (B) or dial plate (R) or display screen (D) appearance material.
3.4 automobile appearances as shown in Figure 10.Figure 10 is herein described material applicating example on automobile appearance.New polymers optical thin film may be used for vehicle body (B) and vehicle window (W) pad pasting, thin film directs or through viscose and is attached to vehicle body or glass surface, and outside applies PET or other materials protective layer, it is possible to achieve vehicle body and the personalized repacking of vehicle window color.Composite optical thin film is attached on automobile change with angle different colours.
3.5 mechanically deforms as shown in FIG. 11 and 12.
Figure 11 is that mechanically deform causes color-changing composite material applicating example.Undeformed polymer composites optical thin film (O) has homogeneous stretching variable color character in the case of not having any additional structure, and the existing convex die plate (S) with certain pattern is pressed on thin film and realizes pattern transfer.The rough patterning of film surface causes the strain difference of diverse location under identical stress, and weaker position strains position thick greatly and relatively and should diminish, and thin film is through Tensile when, the strain difference of diverse location causes color change inconsistent.Effect same can be by additional on thin film certain thickness other one layer or the realization of a few layer film.
Figure 12 is that mechanically deform causes electrochromic polymer composite optical material applicating example.Undeformed polymer composites optical thin film (O) has homogeneous stretching variable color character, now utilize UV lamp (L) to irradiate some characteristic area of material surface selectively by the shade (M) of opening, utilize the photocrosslinking agent added in material to make illuminated partial cross-linked.The Young's modulus of the material of cross-linked areas is much higher than the Young's modulus of uncrosslinked region material, and so when material is stretched, strain is focusing more on uncrosslinked region, and the areal strain cross-linked is relatively small.The region straining big field color change the most uncrosslinked is bigger.Required security pattern can be radiated at material surface in advance by this method, when not having mechanically deform, material color is homogeneous, and pattern is stealthy, displays due to the different pattern of zones of different deflection when material stands mechanically deform.
3.6 such as Figure 13, the pressure transducer shown in 14 and 15.
Figure 13 is the color change after not pressurizeing and pressurizeing of the composite optical thin film, and after pressurization, biaxial tension heaved by material, causes color to be become blue from green, for green when not pressurizeing, is blue after pressurization.
Figure 14 is that novel optical composite is as pressure indicator example schematic.Material (O) is enclosed in pressure chamber (C) sensing opening part (left), and to (right) after gas pressurized in pressure chamber, the stretching of material tympanites causes color to change.
Figure 15 be novel optical composite be applied to football surface do pressure instruction material schematic diagram.Material (O) sticks to football (B) surface (left), and after football inflation, (right) material tension-thining causes color to change, and air pressure inside reduces when, this process reverses.
3.7 Application in Building as shown in figure 16.Figure 16 is the application material applicating example in architectural appearance (left) and built-in (right).By the way of pad pasting, material can be adhered directly to build the smooth finish surface of (B) outer surface glass curtain wall (W) etc., and 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 applicating example as false proof band (O) on currency (C).For different currency base materials, this material can be cut to band directly against being attached on currency base material use as false proof bar.
Figure 18 is that the application material is as trade mark or other purposes pattern anti-fake applicating examples.In addition to by this material directly against being attached on base material use, (OS) various pattern can be imprinted or be combined material (OP) formation different pattern prepared by one or more layers different size microsphere on material film, it is achieved more complicated antiforge function.
Embodiment
4
:
A kind of surface optical material, material includes 320nm sized core-shell structure nano microsphere, and preparation method includes following steps:
(1) preparation of described Nano microsphere:
Core: use 10 liters of reactors to join agitator; argon shield; it is heated to 60 degrees Celsius; premix 2.6 grams of SDS, 2800 grams of deionized waters, 36 grams of styrene monomers; 4 grams of DVB enter reactor; reactor mixing speed 250rpm, wherein uses DVB to substitute BDDA and makes the polystyrene of polymerization have higher refractive index as cross-linking agent, improve optical reflection ratio.It is subsequently adding 0.72 gram of Na2S2O5And 5.18 grams of Na2S2O8.2.3 grams of SDS, 4 grams of NaOH, 2.2 grams of Dowfax2A1,900 grams of deionized waters, 700 grams of styrene monomers, 70 grams of DVB are added with 5ml speed per minute after 20 minutes.
Transition zone: add 0.25 gram of SPS and the mixed solution of 5 grams of deionized water compositions after 30 minutes, 0.5 gram of SDS is added with speed per minute for 7ml after 15 minutes, 2.1 grams of Dowfax2A1,320g deionized water, 250 grams of ethylacrylate(EA) monomer and 30 grams of allyl methacrylate(ALMA) monomer.
Shell: add 4 grams of SDS, 2 grams of NaOH, 1600 grams of deionized waters, 1000 grams of butyl acrylate (BA) monomers, 350 grams of i-butyl with speed per minute for 9ml after 20 minutes
Methacrylate(IBMA), 42 grams of hydroxyethylmethacrylate(HEMA), and 100 gram 2,2,2-trifluoroethyl
Acrylate (TFMA) reduces shell refractive index, increases nucleocapsid refractive index contrast and improves optical property.
Completion of dropwise addition carries out breakdown of emulsion filtration and is dried to obtain Nano microsphere agglomerate precursor after 1 hour.
(2) described Nano microsphere is processed into surface optical material:
By the butanediol acrylate(BDDA of the Nano microsphere obtained and 32% mass fraction) and the Benzophenon mix and blend formation thickness stabilized mixture of mass fraction 2%.
Using scraper or other instruments to be coated on PET or other basement membranes in the mixture of synthesis, cover other layer protecting film above, put in UV solidification case, solidification wavelength is 200-350nm, takes out after three minutes.It is that upper and lower surface is smooth through microstress roll-in after thin film, is then passed through shaking cutting rule integralization process and makes the queueing discipline of Nano microsphere obtain more preferably optical property.
Embodiment
5
:
A kind of surface optical material, material includes 320nm sized core-shell structure nano microsphere, and preparation method includes following steps:
(1) preparation of described Nano microsphere:
Core: use 10 liters of reactors to join agitator; argon shield; it is heated to 90 degrees Celsius; premix 2.6 grams of SDS, 2800 grams of deionized waters, 36 grams of styrene monomers; 4 grams of DVB enter reactor; reactor mixing speed 250rpm, wherein uses DVB to substitute BDDA and makes the polystyrene of polymerization have higher refractive index as cross-linking agent, improve optical reflection ratio.It is subsequently adding 0.72 gram of Na2S2O5And 5.18 grams of Na2S2O8.2.3 grams of SDS, 4 grams of NaOH, 2.2 grams of Dowfax2A1,900 grams of deionized waters, 700 grams of styrene monomers, 70 grams of DVB are added with 15ml speed per minute after 20 minutes.
Transition zone: add 0.25 gram of SPS and the mixed solution of 5 grams of deionized water compositions after 30 minutes, 0.5 gram of SDS is added with speed per minute for 21ml after 15 minutes, 2.1 grams of Dowfax2A1,320g deionized water, 250 grams of ethylacrylate(EA) monomer and 30 grams of allyl methacrylate(ALMA) monomer.
Shell: add 4 grams of SDS, 2 grams of NaOH, 1600 grams of deionized waters, 1000 grams of butyl acrylate (BA) monomers, 350 grams of i-butyl with speed per minute for 27ml after 20 minutes
Methacrylate(IBMA), 42 grams of hydroxyethylmethacrylate(HEMA), and 100 gram 2,2,2-trifluoroethyl
Acrylate (TFMA) reduces shell refractive index, increases nucleocapsid refractive index contrast and improves optical property.
Completion of dropwise addition carries out breakdown of emulsion filtration and is dried to obtain Nano microsphere agglomerate precursor after 1 hour.
(2) described Nano microsphere is processed into surface optical material:
By the butanediol acrylate(BDDA of the Nano microsphere obtained and 32% mass fraction) and the Benzophenon mix and blend formation thickness stabilized mixture of mass fraction 2%.
Using scraper or other instruments to be coated on PET or other basement membranes in the mixture of synthesis, cover other layer protecting film above, put in UV solidification case, solidification wavelength is 200-350nm, takes out after three minutes.It is that upper and lower surface is smooth through microstress roll-in after thin film, is then passed through shaking cutting rule integralization process and makes the queueing discipline of Nano microsphere obtain more preferably optical property.
Claims (10)
1. a Nano microsphere, described Nano microsphere is nucleocapsid structure, it is characterized in that: the core material of described Nano microsphere includes that organic material or inorganic material, the Shell Materials of described Nano microsphere include that polymer elastomer material, the size of described Nano microsphere are 100-1000 nanometer.
Nano microsphere the most according to claim 1, it is characterised in that: described core material includes one or more in polystyrene, silicon dioxide, ferroso-ferric oxide, polymethyl methacrylate, polyethyl acrylate, tin indium oxide, arsenic trioxide, gold and silver.
Nano microsphere the most according to claim 2, it is characterised in that: described Shell Materials includes that polyethyl acrylate, polydimethylsiloxane, polyacrylic acid second two fat, polymethyl methacrylate, polyurethane, polystyrene, oligosaccharide glycol propylene acid methyl ester (oligo (ethylene glycol) methacrylate) chemical formula are H2C=C(CH3)CO(OCH2CH2)nO(CH3), one or more in acrylic compounds and rubber.
Nano microsphere the most according to claim 3, it is characterised in that: also include transition zone between described core and described shell.
Nano microsphere the most according to claim 4, it is characterised in that: described buffer layer material includes one or more in polyethyl acrylate and polymethyl methacrylate.
Nano microsphere the most according to claim 4, it is characterized in that: described core includes accounting for cross-linking agent and the core material of described nucleocapsid structure mass fraction 20%-40%, described shell includes Shell Materials and the Tg regulator accounting for described nucleocapsid structure mass fraction 30%-60%, and described transition zone includes accounting for described nucleocapsid structure mass fraction 5%-20% buffer layer material.
Nano microsphere the most according to claim 6, it is characterised in that: described cross-linking agent accounts for described cross-linking agent and the 1%-15% of described core material gross mass.
8. a surface optical material, material includes the Nano microsphere of nucleocapsid structure, it is characterised in that: described Nano microsphere is arbitrary described Nano microsphere in claim 1 to 7.
The preparation method of surface optical material the most according to claim 8, including following steps:
(1) preparation of described Nano microsphere:
(1.1) preparation of core: by core material and cross-linking agent 60-90 DEG C of mixing；
(1.2) preparation of transition zone: being added by buffer layer material, reaction temperature is 60-90 DEG C again；
(1.3) preparation of shell: Shell Materials and Tg regulator being added, reaction temperature is 60-90 DEG C again, then breakdown of emulsion, dried Nano microsphere；
(2) described Nano microsphere is processed into surface optical material:
(2.1) described Nano microsphere step (1) synthesized forms the mixture that thickness is stable after adding organic solvent or specific monomer；
(2.2), on described mixture coating basement membrane, basement membrane is coated with protecting film；
(2.3) basement membrane coated is put in UV solidification case, take out after 200-350nm solidification；
(2.4) make its upper and lower surface smooth basement membrane microstress roller extruding after solidification, i.e. obtain described surface optical material.
The most according to claim 8, surface optical material is for packaging material, electronic equipment appearance 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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