CN103484099B - Color material under regulation and control of electric field, and preparation method of material - Google Patents
Color material under regulation and control of electric field, and preparation method of material Download PDFInfo
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Abstract
The invention discloses a color material under the regulation and the control of an electric field. The color material comprises a medium and a colloidal crystal material uniformly dispersed in the medium, wherein the medium is propylene carbonate or water; the colloidal crystal material is titanium oxide-coated silicon oxide colloidal SiO2/TiO2 nanoparticles; the volume ratio of the colloidal crystal material to the medium is (1-8): (90-95). The prepared color material is a novel off-color material under the regulation and the control of the electric field, and increases the types of color materials under the regulation and the control of electric fields; the colloidal SiO2/TiO2 nanoparticles are synthetized by the one-step method, and the method is simple and effective; through regulating the added amount of a titanium source, different coated thicknesses of titanium oxide can be realized; the prepared color material is high in color display brightness, has obvious color changes under the action of a very small electric field, and is high in respond speed.
Description
Technical field
The present invention relates to the preparation field of the passive display material of colloidal crystal, particularly relate to lower colour development material of a kind of electric field regulation and control and preparation method thereof.
Background technology
Along with the development of photoelectron technology, more and more higher to the requirement of information displaying, according to the study, people's vision when various sensory organ obtains information from the external world accounts for more than 60%, nowadays much information is all provided by technique of display, therefore proposes more and more higher requirement to technique of display and display device, and display device is as the window of human-computer exchange, there is multiple display category, active display and passive type display can be divided into from light-source angle.Passive display is because being easy under its high light read, comfortableness good (close to paper), (character that not consume energy etc. when keeping image constant receives extensive concern in less energy-consumption, its representative products is Amazon Kindle, but its full-color display performance difference (brightness is inadequate), response speed is slow, does not have development prospect.Current research mainly concentrates on how to realize the passive display of full color, as being that the photon ink technology developed by the isolated company Opalux in University of Toronto adopts the nano particle of precise intervals to form interference to color for realizing commercial photon ink technology before the year two thousand twenty, single pixel can produce any color
Self-assembled structures is the basic reason producing specific light transport phenomena.The colloidal crystal of occurring in nature has opal and blue flash butterfly etc., and the principle that they present riot of color color is that Bragg interferes, so by regulating lattice constant, the indices of diffraction, lattice defects etc. can change the color presented, and the change of these internal factors can be realized, as temperature by outside stimulus again, chemical environment, pressure, magnetic field, electric field etc., Application Areas in view of our research object is display, so are feasible methods by electromagnetic field regulation and control.
As publication number be CN102304263A patent document discloses a kind of photonic crystal paper, comprising: matrix, described matrix is polyacrylamide gel; Be solidificated in the photon crystal material in described matrix, described photon crystal material is the coated Z 250 colloid nano particle of the carbon of superparamagnetism.This invention additionally provides a kind of preparation method of photonic crystal paper.This patent realizes colour developing by the self-assembly of magnetic field regulation and control magnetic particle.
(the TiO such as Xing Ting
2/ SiO
2the preparation of composite particles and the assembling of colloidal crystal thereof, East China Normal University, 2006 postgraduate's master thesis) disclose with monodispersed silica dioxide granule for core, take ethanol as solvent, prepare coated uniform TiO by the hydrolysis of presoma tetrabutyl titanate (TBOT)
2/ SiO
2composite particles, studies various reaction conditions if the concentration of TBOT, the concentration of water, the size of core and coated number of times are for the impact of covered effect by the various characterization method such as scanning electron microscope and micro-electrophoresis apparatus; And the single dispersing TiO disclosed in above-mentioned preparation
2/ SiO
2on the basis of composite particles, utilize gravity settling and vertical sedimentation method to carry out self-assembly to composite particles, obtain three-dimensional colloidal crystal.Adopt the structure of scanning electron microscope to colloidal crystal to characterize, and measure the optical property of colloidal crystal with visible spectrophotometer.With single dispersing TiO
2/ SiO
2composite particles is scattered in dehydrated alcohol, and the ordered 3 D structure of the colloidal crystal obtained after spontaneous evaporation is fixed, and can only form a kind of schemochrome corresponding with this structure, cannot realize the regulation and control to Show Color to incident light after interfering.
Summary of the invention
The invention provides lower colour development material of a kind of electric field regulation and control and preparation method thereof, the silicon oxide colloidal state nanoparticle of titanium-oxide-coated is obtained by single stage method, be scattered in again in medium, preparation method is easy, energy consumption is low, the colour brightness of making the colour development material display of arriving is high, under very little electric field action, just there is obvious colour-change, and fast response time.
The invention discloses the lower colour development material of a kind of electric field regulation and control, comprise medium and dispersed colloidal crystal material in the medium, described medium is propylene carbonate or water; Described colloidal crystal material is the silicon oxide colloidal state nanoparticle of titanium-oxide-coated, is designated as SiO
2/ TiO
2; The volume ratio of described colloidal crystal material and medium is (1 ~ 8): (90 ~ 95).
Described colloidal crystal homogenize material for medium with propylene carbonate or water, with the silicon oxide colloidal state nanoparticle of titanium-oxide-coated for colloidal crystal material, is scattered in after in described medium, then is injected in cell box by the lower colour development material of electric field regulation and control.Colour development material initial injection enters in cell box to present white, and when applying voltage to cell box, dispersion colloidal crystal particle in media as well can form a fixed structure at the move under influence of electric field, interferes the corresponding schemochrome of rear formation to incident light.Keep electric field constant, color relation does not have obvious change; When electric field increases gradually, the spacing between particle changes, thus demonstrates the blueness from shallow to dark.
As preferably, the silicon oxide nanoparticle SiO of described titanium-oxide-coated
2/ TiO
2particle diameter is 50nm ~ 250nm, TiO
2shell thickness is 2nm ~ 50nm; Further preferably, described titanium oxide shell thickness is 20nm ~ 50nm.
As preferably, described colloidal solid is the silicon oxide nanoparticle SiO of the titanium-oxide-coated of modifier modification
2/ TiO
2; Described properties-correcting agent is polyvinyl alcohol, hypromellose equipotential resistance type properties-correcting agent, because this kind of properties-correcting agent can increase the steric hindrance between particle, the distance between particle is increased.
The silicon oxide colloidal state nanoparticle of titanium-oxide-coated can improve its color developing by modification, steric hindrance type properties-correcting agent can increase the steric hindrance between particle, and the distance between particle is increased, and spectrum will red shift, by the adjustment of electric field, the colour developing of full spectrum from redness to blueness namely can be realized.
The invention also discloses the preparation method of the lower colour development material of a kind of electric field regulation and control, comprise the following steps:
A) be (140 ~ 150) by volume ratio: (2 ~ 5): (4 ~ 8): the ethanol of (2 ~ 7), water, ammoniacal liquor, tetraethoxy mixing, at room temperature ~ 50 DEG C after reaction 1 ~ 10h, add 20 ~ 50ml ethanol, at 30 DEG C ~ 70 DEG C, adjust ph is 10 ~ 11, stir the alcoholic solution simultaneously dripping titanium source, be added dropwise to complete rear Keep agitation 1h ~ 5h, leave standstill 2 ~ 5h, through being separated, washing, dry and after milled processed, obtaining the silicon oxide colloidal state nanoparticle of titanium-oxide-coated;
Described alcoholic solution is methyl alcohol, ethanol or ethylene glycol, titanium source is isopropyl titanate, tetrabutyl titanate, titanium tetrachloride or titanyl sulfate, the volume ratio of titanium source and alcoholic solution is (1 ~ 7): (30 ~ 50), and the volume ratio in titanium source and silicon source is (0.5 ~ 10): (5 ~ 9);
B) by SiO
2/ TiO
2nanoparticle with 5% ~ 20% of medium volume dispersion in media as well, obtains described colour development material.
As preferably, the volume ratio in described titanium source and silicon source is (1 ~ 8): (5 ~ 9), and can be obtained the coating layer of the titanium oxide of different thickness by the add-on regulating and controlling titanium source, along with the increase of coating thickness, the intensity of spectrum can increase, and color range increases.
As preferably, the SiO that step a) is obtained
2/ TiO
2nanoparticle 0.1g is scattered in 10mL ~ 30ml water, adds 0.01g ~ 0.05g properties-correcting agent, fully stirs 5 ~ 10h, obtains the SiO of modification
2/ TiO
2nanoparticle; Again by the SiO of modification
2/ TiO
2nanoparticle with 5% ~ 20% of medium volume dispersion in media as well, obtains described colour development material.
Compared with prior art, the present invention has following outstanding advantages:
With the SiO of nucleocapsid structure
2/ TiO
2for colloidal crystal material, be a kind of new electric field regulation and control chromic materials with propylene carbonate or water for the colour development material that medium forms, add the kind of electric field regulation and control colour development material, by one-step synthesis method SiO
2/ TiO
2colloidal nanoparticles, method is simply effective, can realize the coated of the titanium oxide of different thickness by the add-on regulating and controlling titanium source; The colour brightness of obtained colour development material display is high, under very little electric field action, just have obvious colour-change, and fast response time.
With modification SiO
2/ TiO
2for the colour development material of colloidal crystal material and medium composition can realize the colour developing of full spectrum from redness to blueness, expand the range of application of this colour development material further.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture that embodiment 1 obtains the silicon oxide nanoparticle of titanium-oxide-coated;
Fig. 2 is the reflection wavelength spectrogram that embodiment 1 obtains colour development material;
Fig. 3 is the reflection wavelength spectrogram that embodiment 4 obtains colour development material;
Fig. 4 is the transmission electron microscope picture that embodiment 6 obtains the silicon oxide nanoparticle of titanium-oxide-coated;
Fig. 5 is the reflection wavelength spectrogram that embodiment 6 obtains colour development material.
Embodiment
Embodiment 1
By 8ml, 28% ammonia soln, 147ml ethanol, 5ml water adds in 500ml there-necked flask, stir 22min with the speed of 400r/min at 50 DEG C after, drip 7.2ml tetraethoxy with peristaltic pump, after reaction 4h, add 38ml ethanol again, at 50 DEG C, adjust ph is 10 ~ 11, continues to stir 10min.From there-necked flask, take out 105ml solution, stay 100ml solution, drip the ethanolic soln of isopropyl titanate with peristaltic pump, wherein ethanol 50ml, isopropyl titanate 1ml, drip off after 1h is stirred in rear continuation and stop stirring, leave standstill 2h, centrifugation is carried out to reacted product, obtains SiO
2/ TiO
2, wash respectively once with distilled water and ethanol and dry at 50 DEG C ~ 80 DEG C, grind stand-by.
Carry out transmission electron microscope observing to the silicon oxide nanoparticle of described titanium-oxide-coated, result is see Fig. 1, and as shown in Figure 1, success is about the titanium oxide of 7nm in the coated a layer thickness of silicon oxide surface.
Get 0.0648g, the silicon oxide nanoparticle of the thick titanium-oxide-coated of 7nm is scattered in 0.5ml carbonic allyl ester solution to be measured.
Test process is as follows: with syringe, above-mentioned solution is injected the cell box prepared, cell box is made up of two panels ito glass, and centre separates with the insulating film of 200 micron thickness, and applied field is 0V ~ 5V, connect power supply added electric field, the reflection wavelength of observation cell box and colour-change.Result is the reflection wavelength spectrogram that the embodiment of the present invention obtains colour development material see Fig. 2, Fig. 2, can see that collection of illustrative plates has obvious peak position to move, the corresponding corresponding color of different peak position, color by light blue to dark blue.
Embodiment 2
By the silicon oxide nanoparticle 0.096g of the thick titanium-oxide-coated of 7nm of preparation in embodiment 1, be scattered in 0.5mL propylene carbonate to be measured, test process with example 1, similar in the form of the collection of illustrative plates obtained and embodiment 1, but reflection peak intensity entirety increases to some extent.
Embodiment 3
The silicon oxide nanoparticle 0.0648g of the thick titanium-oxide-coated of 7nm of preparation in embodiment 1 is scattered in 0.5mL water to be measured, test process is with example 1, the collection of illustrative plates reflection strength obtained obviously increases to 30%, and voltage is added to the process of 5v from 0v, and peak position moves to 480nm from 420nm.
Embodiment 4
The silicon oxide nanoparticle 0.1g of the thick titanium-oxide-coated of 7nm of preparation in embodiment 1 is scattered in 10mL water, add 0.01g polyvinyl alcohol, fully stir centrifuge washing after 6 hours, obtain modified nanoparticle, wash respectively once with distilled water and ethanol and dry at 50 DEG C, grind stand-by.
The silicon oxide nanoparticle getting the titanium-oxide-coated of the above-mentioned modification of 0.0648g is scattered in 0.5ml carbonic allyl ester solution to be measured, test process with example 1, the reflection wavelength spectrogram obtained as Fig. 3, compared with Fig. 2, Dependent Red Shift, spectrum covers whole visible region.
Embodiment 5
The silicon oxide nanoparticle 0.1g of the thick titanium-oxide-coated of 7nm of preparation in embodiment 1 is scattered in 10mL water, add 0.01g hypromellose, abundant stirring centrifuge washing after 6 hours, obtain modified nanoparticle, wash respectively once with distilled water and ethanol and dry at 50 DEG C, grind stand-by.
The silicon oxide nanoparticle getting the titanium-oxide-coated of the above-mentioned modification of 0.0648g is scattered in 0.5ml carbonic allyl ester solution to be measured, test process with example 1, the reflection wavelength spectrogram obtained and Fig. 3 similar.
Embodiment 6
By 8ml, 28% ammonia soln, 147ml ethanol, 5ml water adds in 500ml there-necked flask, after stirring 22min, drips 7.2ml tetraethoxy with peristaltic pump at 50 DEG C with the speed of 400r/min, adds 38ml ethanol again after reaction 4h, continues to stir 10min.From there-necked flask, take out 105ml solution, stay 100ml solution, drip the ethanolic soln of isopropyl titanate with peristaltic pump, wherein ethanol 50ml, isopropyl titanate 2ml, drip off after 1h is stirred in rear continuation and stop stirring, leave standstill 2h, centrifugation is carried out to reacted product, obtains SiO
2/ TiO
2, wash respectively once with distilled water and ethanol and dry at 50 DEG C, grind stand-by.
Carry out transmission electron microscope observing to the silicon oxide nanoparticle of described titanium-oxide-coated, see Fig. 4, as shown in Figure 4, success is about the titanium oxide of 20nm in the coated a layer thickness of silicon oxide surface.
Get 0.0648g, the silicon oxide nanoparticle of the titanium-oxide-coated that 20nm is thick is scattered in 0.5ml carbonic allyl ester solution to be measured, test process is with example 1, result is see Fig. 5, Fig. 5 is the reflection wavelength spectrogram that the present embodiment obtains colour development material, can see that collection of illustrative plates has obvious peak position to move, compared with example 1, intensity increases to some extent.
Claims (5)
1. the lower colour development material of electric field regulation and control, is characterized in that, comprise medium and dispersed colloidal crystal material in media as well,
Described medium is propylene carbonate or water;
Described colloidal crystal material is the silicon oxide colloidal state nanoparticle of titanium-oxide-coated;
The volume ratio of described colloidal crystal material and medium is (1 ~ 8): (90 ~ 95);
The preparation method of the lower colour development material of described electric field regulation and control, comprises the following steps:
A) be (140 ~ 150) by volume ratio: (2 ~ 5): (4 ~ 8): the ethanol of (2 ~ 8), water, ammoniacal liquor, tetraethoxy mixing, at room temperature ~ 50 DEG C after reaction 1 ~ 10h, add 20 ~ 50mL ethanol, at 30 DEG C ~ 70 DEG C, adjust ph is 10 ~ 11, stir the alcoholic solution simultaneously dripping titanium source, be added dropwise to complete rear Keep agitation 1h ~ 5h, leave standstill 2 ~ 5h, through being separated, washing, dry and after milled processed, obtaining the silicon oxide colloidal state nanoparticle of titanium-oxide-coated;
Described alcoholic solution is methyl alcohol, ethanol or ethylene glycol, titanium source is isopropyl titanate, tetrabutyl titanate, titanium tetrachloride or titanyl sulfate, the volume ratio of titanium source and alcoholic solution is (1 ~ 7): (30 ~ 50), and the volume ratio in titanium source and silicon source is (0.5 ~ 10): (5 ~ 9);
B) by the silicon oxide colloidal state nanoparticle of titanium-oxide-coated with 5% ~ 20% of medium volume dispersion in media as well, described colour development material is obtained.
2. the lower colour development material of electric field regulation and control according to claim 1, it is characterized in that, described colloidal crystal material is the silicon oxide nanoparticle of the titanium-oxide-coated of modifier modification;
Described properties-correcting agent is polyvinyl alcohol or hypromellose.
3. the lower colour development material of electric field regulation and control according to claim 1 and 2, it is characterized in that, the particle diameter of the silicon oxide colloidal state nanoparticle of described titanium-oxide-coated is 50nm ~ 250nm, and titanium oxide shell thickness is 2nm ~ 50nm.
4. the lower colour development material of electric field regulation and control according to claim 3, it is characterized in that, described titanium oxide shell thickness is 20nm ~ 50nm.
5. the lower colour development material of electric field regulation and control according to claim 1, it is characterized in that, the silicon oxide colloidal state nanoparticle 0.1g of titanium-oxide-coated step a) obtained is scattered in 10mL ~ 30mL water, add 0.01g ~ 0.05g properties-correcting agent, abundant stirring 5 ~ 10h, obtains the silicon oxide colloidal state nanoparticle of the titanium-oxide-coated of modification; Again by the silicon oxide colloidal state nanoparticle of the titanium-oxide-coated of modification with 5% ~ 20% of medium volume dispersion in media as well, described colour development material is obtained.
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| US20160000942A1 (en) * | 2013-01-04 | 2016-01-07 | Industry-Academic Cooperation Foundation, Yonsei University | Mri contrast agent including t1 contrast material coated on surface of nanoparticle support |
| US9507183B2 (en) | 2014-03-24 | 2016-11-29 | Adidas Ag | Apparatus for manipulating color changing materials in articles of wear |
| US11828929B2 (en) | 2014-03-24 | 2023-11-28 | Adidas Ag | Color changing materials arranged in slow particle coloration materials |
| US9701071B2 (en) | 2014-03-24 | 2017-07-11 | Adidas Ag | Method of manipulating encapsulation of color changing materials |
| US10698197B2 (en) | 2014-03-24 | 2020-06-30 | Adidas Ag | Color changing materials arranged in slow particle coloration materials |
| US9213192B2 (en) | 2014-03-24 | 2015-12-15 | Adidas Ag | System and method for manipulating color changing materials |
| US9482785B2 (en) | 2014-03-24 | 2016-11-01 | Adidas Ag | Method of applying and using color changing materials in articles of wear |
| CN106423000A (en) * | 2016-09-28 | 2017-02-22 | 武汉纺织大学 | Preparation method for core-shell TiO2-SiO2 microsphere self-assembled structural color film |
| CN111176003B (en) * | 2020-02-07 | 2022-12-06 | 武汉华星光电半导体显示技术有限公司 | Color developing material and display panel thereof |
| CN113625498A (en) * | 2021-08-13 | 2021-11-09 | 上海应用技术大学 | Preparation method of electric field controllable silicon dioxide colloid self-assembly structure color-changing device |
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