CN102314039B - Composition of black and white electrophoretic display liquid for electrophoretic display and preparation method thereof - Google Patents
Composition of black and white electrophoretic display liquid for electrophoretic display and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a composition of black and white electrophoretic display liquid for electrophoretic display and a preparation method thereof; the black and white electrophoretic display liquid respectively adopts carbon black and titanium dioxide nanoparticles as black and white electrophoretic particles; the concentration of the particles in the black and white electrophoretic display liquid is respectively 3 percent to 20 percent and 10 percent to 50 percent, and the mass ratio of the black and white electrophoretic display liquid is 1:15 to 1:30; the dispersion media are Isopar series, the dispersing agents are fluorinated surfactant and polymer dispersant, and the used amount of the dispersing agents is 3 percent to 40 percent of the used amount of the electrophoretic particles. The preparation method of the black and white electrophoretic display liquid comprises the steps that: first, the black and white particles, the polymer dispersant and the dispersion media are respectively ball milled to prepare the black and white electrophoretic display liquid, are mixed by a certain ratio, and are added with the fluorinated surfactant, so that the black and white electrophoretic display liquid is prepared. The electrophoretic display liquid is prepared into a micro-cup device, the spacing of two polar plates is 0.1mm, 15V forward and backward alternating voltage is applied, the response of the electrophoretic display liquid is good, the contrast is above 23:1 and the highest contrast is 38:1, the black display response time is 831ms, and the white display response time is 1123ms.
Description
Technical field
The present invention relates to composition for the black-white electrophoresis display liquid of electrophoresis showed and preparation method thereof, be particularly related to take titanium dioxide nano-particle as white electrophoretic particles, the carbon black nano particle is black electrophoretic particles, Isopar is dispersion medium, fluorochemical surfactant and polymkeric substance are spreading agent, the two aobvious electrophoresis disclosing solutions of the black and white that is formed by electrophoresis particle, dispersion medium and spreading agent.
Technical background
Display technique mainly contains: cathode-ray tube display, liquid crystal display, thin-film electroluminescence (TFEL) flat pannel display and electrophoresis showed etc.Electrophoresis showed is at 20 century 70s, is at first proposed by MAT, is utilize coloured charged particle to move under electric field and develop the color.Electrophoresis showed attracts wide attention with high reflectance, super low-power consumption, convenient frivolous, inexpensive environmental protection and the flexible advantage that shows.The principle of work of electrophoretic display technology is to utilize the principle of electrophoresis, is clipped in two interelectrode charge specieses and moves under the effect of electric field, makes two kinds of different colors of charge species Alternation Display of motion.
Electrophoresis disclosing solution is the core of electrophoretic display device (EPD).Electrophoresis disclosing solution is a nonaqueous colloid system, the stable suspending liquid that is made of various ingredients such as pigment particles, dispersion medium and spreading agents.The composition of electrophoresis disclosing solution and character are determining display performance and stability and the life-spans such as contrast, reflectivity and response time of electrophoretic display device, EDD to a great extent.Obtain high-performance electrophoresis and show that liquid is to improve the most basic and effective method of display performance.So, for the research of electrophoresis disclosing solution with improve and never interrupt in three more than ten years and enjoy attention.
The selection of electrophoresis particle is the committed step that the preparation high-performance electrophoresis shows liquid, and the range of choice of electrophoresis particle is very extensive, can be any charged or easily obtain the particle of electric charge.Generally should possess following condition: (1) in order to reduce and subtract less granular coagulation or floating, its density should with the approaching of dispersion medium; (2) particle should have low solubility, unsoluble-unexpansive and chemical stability in organic solvent; (3) particle should have good optical property, has high refractive index, high scattering coefficient and low absorption coefficient; (4) particle size should be as far as possible little, to increase the stability of disperse system; (5) the easy adsorption charge of particle surface or modification.Inorganic pigment granules commonly used has titania, monox, chrome yellow, ultramarine, carbon black, manganese violet, iron oxide red and cadmium red etc.; Organic pigment particle has red, toluidine red, phthalocyanine blue and quinacridone etc.The electrophoresis particle that the present invention adopts is titanium dioxide nano-particle and carbon black nano particle.Titania as a kind of inorganic Chinese white because its excellent optical property, stable chemical property and studied persons cheap and easy to get generally adopt.Titania has high refractive index (2.76-2.55) and superpower covering power, and this means higher reflectivity and contrast for the reflection-type electrophoresis showed, is used as colour developing particle or background color particle and is widely used.And carbon black is high to the Optical Absorption rate due to its surface as a kind of inorganic black pigment particle, can form high-contrast with white particle, and solubleness is low in organic solvent, without swelling, its surface is adsorption charge easily, easily modification, and it is cheap, and available kind extensively is used.
The effect of dispersion medium is dispersed color particle and dissolving dye, charge control agent and stabilizing agent.Generally should possess following condition: (1) is stable in the temperature range of broadness, thereby should have higher boiling point and lower fusing point; (2) should be good insulativity organic solvent, namely have lower specific inductive capacity, higher resistivity and lower water-soluble; (3) have good optics and electrochemical stability; (4) good mobility of particle, namely the dynamics viscosity is low; (5) refractive index of dispersion medium and particle and density are complementary, to increase stability of system; (6) should have low toxicity, namely show good Environmental compatibility.Operable organic solvent comprises epoxy compound, aromatic hydrocarbons, halogenated hydrocarbons, aliphatic hydrocarbon and siloxane etc.Early stage researcher adopts olive wet goods vegetable oil as dispersion medium, and is unstable and cost is higher due to its chemical composition, is not used now.Halogenated hydrocarbons density is larger, can be composite with color density less aliphatic hydrocarbon or aromatic hydrocarbons, and the density of regulating dispersion medium by regulating compound proportion is complementary in the hope of reaching with particle density.But because the halogenated hydrocarbons part is volatile, and environmental protection not, its application is restricted.And the isoparaffin that the present invention adopts (Isopar series) is cheap and easy to get due to its stable chemical property, and not volatile, has good compatibility to can be used as new dispersion medium with environment and substitutes at present the most frequently used halogenated hydrocarbons.
Spreading agent commonly used is divided into traditional spreading agent and hyper-dispersant two classes.
The tradition spreading agent is adsorbed on particle surface by having hydrophilic polar group and the organism that the non-polar group with hydrophobic nature forms, and the surface free energy of particle is obviously reduced, and increases the dispersion stabilization of electrophoresis particle.Spreading agent as some high score subclasses: polyacrylic acid, styrene-methacrylic acid-alkyl acrylate copolymer, styrene-maleic acid copolymer, vinyl acetate-maleate copolymer etc., can obviously improve the dispersiveness of electrophoresis particle, but in these spreading agents, contained electric charge with TiO 2 particles or the effective combination in carbon black particle surface is less, therefore the electrophoresis liquid response time for preparing is longer, can not satisfy the requirement of e-book.
Hyper-dispersant is the multi-functional wetting dispersing agent of the special polymer-type of a class, its action principle and traditional spreading agent are similar, difference is that hyper-dispersant contains a plurality of anchoring groups, particle dispersion effect for low polarity is more obvious, but due to the deliquescent difference of various hyper-dispersants in dispersion medium (Isopar series), and with the difference of selected electrophoresis particle matching, not all hyper-dispersant is all applicable, as SUP7001, SUP7002 etc.
What the dispersion medium multiselect of present existing black-white electrophoresis display liquid was used is the zellon relatively poor with Environmental compatibility, and the display device contrast of the black-white electrophoresis display liquid preparation take zellon as dispersion medium is higher, and response speed is very fast; And to less with the research of the dispersion medium of the good Isopar series of Environmental compatibility, and the display device of the preparation of the black-white electrophoresis display liquid take Isopar series as dispersion medium or do not respond, the perhaps poor contrast of response, response speed is slow.And the black-white electrophoresis display liquid employing Isopar series of the present invention's preparation is dispersion medium, by adding suitable spreading agent and surfactant, the display device contrast of preparing is high, fast response time, the display effect when having met or exceeded take zellon as dispersion medium.Finally use with the good Isopar series of Environmental compatibility and replaced with the relatively poor zellon of Environmental compatibility having prepared the black-white electrophoresis display liquid of environmental type as spreading agent.
Summary of the invention
The purpose of this invention is to provide a kind of composition of the black-white electrophoresis display liquid for electrophoresis showed and the method for preparation thereof, take Isopar series isoparaffin as dispersion medium, titania and carbon black particle are the two aobvious black-white electrophoresis display liquids of electrophoresis particle preparation, this electrophoresis disclosing solution has dispersiveness and charging property preferably, can be for the preparation of electronic ink display spare.
The succimide class spreading agent that the present invention adopts, this type of spreading agent contains rich electric charge amino group, can increase the quantity of electric charge on electrophoresis particle surface when increasing the particle dispersion stabilization, is conducive to the raising of response speed.CH series auxiliary agent and derivative of fatty acid class hyper-dispersant that the present invention adopts can improve the rheological of electrophoresis liquid when improving the particle dispersion stabilization, be conducive to the improvement of display effect.The present invention adopts the fluorinated surfactant can obviously improve the rheological of electrophoresis liquid, reduce the viscosity of electrophoresis liquid, raising for response speed has positive effect, and the full-fluorine octyl sulfuryl fluoride that adopts, the research in electrophoresis liquid is also seldom as additive application for this class surfactant at present.
Concrete technical scheme is as follows:
The invention provides a kind of composition of the black-white electrophoresis display liquid for electrophoresis showed, comprising:
(1) particle concentration is the titanium dioxide white electrophoresis particle of 10%-50%, and particle concentration is the carbon black black electrophoretic particles of 3%-20%, and in black-white electrophoresis display liquid, the mass ratio of black electrophoresis liquid and white electrophoresis liquid is 1: 15-1: 30.
(2) Isopar series electrophoretic dispersion medium, preferentially select Isopar G, Isopar H, Isopar L and Isopar M.
(3) fluorochemical surfactant and polymkeric substance are spreading agent, fluorochemical surfactant refers to full-fluorine octyl sulfuryl fluoride, its consumption is the 3%-20% of electrophoresis particle consumption, polymer dispersant comprises succimide class spreading agent (T31, T151 and T152), CH series auxiliary agent (CH-5, CH-6 and CH-13) and derivative of fatty acid class hyper-dispersant (A4100 and A4300), and its consumption is respectively 3%-25%, 6%-40% and the 3%-30% of electrophoresis particle consumption.
In white electrophoresis liquid of the present invention, TiO 2 particles concentration is 10%-50%, and in the black electrophoresis liquid, carbon black particle concentration is 3%-20%; If electrophoresis particle concentration is too low, the electrophoresis disclosing solution shape that is translucent, do not reach the contrast of expection; If the electrophoresis particle excessive concentration, the electrophoresis particle arrangement is too tight, and the electrophoresis disclosing solution response is slowly mixed and disorderly, and contrast is low.
The present invention prepares that in black-white electrophoresis display liquid, the mass ratio of black electrophoresis liquid and white electrophoresis liquid is 1: 15-1: 30; If the black electrophoretic particles ratio is excessive, electrophoresis disclosing solution becomes grey black, and white attitude reflectivity is too low; If the black electrophoretic particles ratio is too small, black electrophoretic particles is difficult to hide fully white electrophoretic particles, and the electrophoresis disclosing solution contrast of formation is too low.
The electrophoretic dispersion medium that the present invention adopts is Isopar series isoparaffin, it has higher boiling point and lower fusing point, insulativity is good, lower specific inductive capacity, higher resistivity and lower water-soluble are arranged, good optics and electrochemical stability and good mobility of particle are arranged, and its refractive index and electrophoresis particle are close, and not volatile, nontoxic, fabulous with Environmental compatibility.And in Isopar series due to the difference of fusing point, boiling point, volatile grade, flash-point and viscosity, the preferential dispersion medium of selecting is Isopar G, Isopar H, Isopar L and Isopar M.
and make dispersion medium for Isopar series, titania and carbon black are as the system of electrophoresis particle, by stability and the difference of display comparison degree and response time of being uniformly dispersed, the preferential spreading agent of selecting is succimide class spreading agent (T31, T151 and T152), CH series auxiliary agent (CH-5, CH-6 and CH-13), fluorinated surfactant (full-fluorine octyl sulfuryl fluoride) and derivative of fatty acid class hyper-dispersant (A4100 and A4300), its molecular structure can be divided into two parts, a part is anchoring group, Main Function is that spreading agent adsorbed close and electrophoresis particle is surperficial, prevent that it from coming off, another part is solvent chain, and Main Function is at the certain thickness protective seam of electrophoresis particle surface formation, reduces particle aggregation, improves the dispersion stabilization of electrophoresis particle.
Dispersant dosage of the present invention is the 3%-40% of electrophoresis particle consumption, if consumption is very few, spreading agent and electrophoresis particle Surface Contact are insufficient, and electrophoresis particle can not well be scattered in Isopar, the electrophoresis dispersion poor stability; If dispersant dosage is too much, electrophoresis disclosing solution thickness too, electrophoresis disclosing solution easily condenses and low-response, and contrast is low.
The invention provides a kind of preparation method of the black-white electrophoresis display liquid for electrophoresis showed, comprising:
(1) titanium dioxide white electrophoresis particle, succimide class spreading agent (T31, T151 and T152), CH series auxiliary agent (CH-5, CH-6 and CH-13) and Isopar series dispersion medium are mixed rear ball milling 20h-48h by a certain percentage, obtain white electrophoresis disclosing solution;
(2) carbon black black electrophoretic particles, succimide class spreading agent (T31, T151 and T152), CH series auxiliary agent (CH-5, CH-6 and CH-13) and Isopar series dispersion medium are mixed rear ball milling 20h-48h by a certain percentage, obtain the black electrophoresis disclosing solution;
(3) the black and white electrophoresis disclosing solution with preparation is 1 in mass ratio: 15-1: 30 mix, and add fluorinated surfactant (full-fluorine octyl sulfuryl fluoride) and derivative of fatty acid class hyper-dispersant (A4100 and A4300) and mix.
Electrophoresis disclosing solution of the present invention is put into the sedimentation bottle, place rear observation of a week and show that liquid still keeps stable.Electrophoresis disclosing solution of the present invention is made little cupule spare, and the two-plate spacing is 0.1mm, applies forward and reverse alternate voltages of 15V, the electrophoresis disclosing solution response is good, and contrast is up to 38: 1 more than 23: 1, the aobvious black response time is 831ms, and the whitening response time is 1123ms.
Description of drawings
Fig. 1 is the two eight sections little glass prepared display effect figures of electrophoresis clock display device under electric field of aobvious electrophoresis disclosing solution of the black and white that adopts the present invention's preparation, and wherein (a) is white gravoply, with black engraved characters, is (b) the black matrix wrongly written or mispronounced character.
Embodiment
Example 1
In the ball milling bottle, add CH-5 and the 1.00g TiO of T31,0.10g of Isopar G, the 0.05g of 10mL
2Nano particle or 0.30g carbon black nano particle take 2mm zirconia zirconium pearl as abrasive media, grind 20h under rotating speed 600r/min, preparation white respectively and black electrophoresis disclosing solution.Black-white electrophoresis display liquid was mixed by 1: 30, add full-fluorine octyl sulfuryl fluoride and the 0.03g A4100 of 0.02g, mix and namely obtain black and white particle electrophoresis demonstration liquid.
Electrophoresis disclosing solution of the present invention is put into the sedimentation bottle, place rear observation of a week and show that liquid still keeps stable.Electrophoresis disclosing solution of the present invention is filled in little glass of display device, and the two-plate spacing is 0.1mm, applies forward and reverse alternate voltages of 15V, observes display effect, and contrast is 23.2: 1, and the aobvious black time is 945ms, and the whitening time is 1163ms.
Example 2
In the ball milling bottle, add CH-6 and the 5.00g TiO of T152,0.50g of Isopar H, the 0.20g of 10mL
2Nano particle or 2.00g carbon black nano particle take 2mm zirconia zirconium pearl as abrasive media, grind 24h under rotating speed 600r/min, preparation white respectively and black electrophoresis disclosing solution.Black-white electrophoresis display liquid was mixed by 1: 15, add full-fluorine octyl sulfuryl fluoride and the 0.20g A4100 of 0.06g, mix and namely obtain black and white particle electrophoresis demonstration liquid.
Electrophoresis disclosing solution of the present invention is put into the sedimentation bottle, place rear observation of a week and show that liquid still keeps stable.Electrophoresis disclosing solution of the present invention is filled in little glass of display device, and the two-plate spacing is 0.1mm, applies forward and reverse alternate voltages of 15V, observes display effect, and contrast is 25.1: 1, and the aobvious black time is 1107ms, and the whitening time is 1244ms.
Example 3
In the ball milling bottle, add CH-13 and the 2.00g TiO of T151,0.15g of Isopar L, the 0.10g of 10mL
2Nano particle or 0.40g carbon black nano particle take 2mm zirconia zirconium pearl as abrasive media, grind 28h under rotating speed 600r/min, preparation white respectively and black electrophoresis disclosing solution.Black-white electrophoresis display liquid was mixed by 1: 20, add full-fluorine octyl sulfuryl fluoride and the 0.05g A4100 of 0.03g, mix and namely obtain black and white particle electrophoresis demonstration liquid.
Electrophoresis disclosing solution of the present invention is put into the sedimentation bottle, place rear observation of a week and show that liquid still keeps stable.Electrophoresis disclosing solution of the present invention is filled in little glass of display device, and the two-plate spacing is 0.1mm, applies forward and reverse alternate voltages of 15V, observes display effect, and contrast is 28.3: 1, and the aobvious black time is 1032ms, and the whitening time is 1220ms.
Example 4
In the ball milling bottle, add CH-13 and the 2.00g TiO of T31,0.20g of Isopar G, the 0.08g of 10mL
2Nano particle or 0.50g carbon black nano particle take 2mm zirconia zirconium pearl as abrasive media, grind 32h under rotating speed 600r/min, preparation white respectively and black electrophoresis disclosing solution.Black-white electrophoresis display liquid was mixed by 1: 25, add full-fluorine octyl sulfuryl fluoride and the 0.08g A4300 of 0.02g, mix and namely obtain black and white particle electrophoresis demonstration liquid.
Electrophoresis disclosing solution of the present invention is put into the sedimentation bottle, place rear observation of a week and show that liquid still keeps stable.Electrophoresis disclosing solution of the present invention is filled in little glass of display device, and the two-plate spacing is 0.1mm, applies forward and reverse alternate voltages of 15V, observes display effect, and contrast is 30.6: 1, and the aobvious black time is 827ms, and the whitening time is 1019ms.
Example 5
In the ball milling bottle, add CH-6 and the 4.00g TiO of T152,0.35g of Isopar M, the 0.18g of 10mL
2Nano particle or 1.00g carbon black nano particle take 2mm zirconia zirconium pearl as abrasive media, grind 36h under rotating speed 600r/min, preparation white respectively and black electrophoresis disclosing solution.Black-white electrophoresis display liquid was mixed by 1: 28, add full-fluorine octyl sulfuryl fluoride and the 0.17g A4300 of 0.05g, mix and namely obtain black and white particle electrophoresis demonstration liquid.
Electrophoresis disclosing solution of the present invention is put into the sedimentation bottle, place rear observation of a week and show that liquid still keeps stable.Electrophoresis disclosing solution of the present invention is filled in little glass of display device, and the two-plate spacing is 0.1mm, applies forward and reverse alternate voltages of 15V, observes display effect, and contrast is 33.8: 1, and the aobvious black time is 1531ms, and the whitening time is 2219ms.
Example 6
In the ball milling bottle, add CH-5 and the 3.00g TiO of T151,0.20g of Isopar L, the 0.10g of 10mL
2Nano particle or 0.50g carbon black nano particle take 2mm zirconia zirconium pearl as abrasive media, grind 48h under rotating speed 600r/min, preparation white respectively and black electrophoresis disclosing solution.Black-white electrophoresis display liquid was mixed by 1: 22, add full-fluorine octyl sulfuryl fluoride and the 0.10g A4300 of 0.03g, mix and namely obtain black and white particle electrophoresis demonstration liquid.
Electrophoresis disclosing solution of the present invention is put into the sedimentation bottle, place rear observation of a week and show that liquid still keeps stable.Electrophoresis disclosing solution of the present invention is filled in little glass of display device, and the two-plate spacing is 0.1mm, applies forward and reverse alternate voltages of 15V, observes display effect, and contrast is 37.8: 1, and the aobvious black time is 831ms, and the whitening time is 1123ms.
Claims (3)
1. black-white electrophoresis display liquid that is used for electrophoresis showed, its composition comprises:
(1) black and white electrophoresis particle; White electrophoretic particles is titanium dioxide nano-particle, and particle concentration is 10%-50%, and black electrophoretic particles is the carbon black electrophoresis particle, and particle concentration is 3%-20%, and in black-white electrophoresis display liquid, the mass ratio of black electrophoresis liquid and white electrophoresis liquid is 1:15-1:30;
(2) Isopar series electrophoretic dispersion medium;
(3) spreading agent fluorochemical surfactant and polymer dispersant; Fluorochemical surfactant refers to full-fluorine octyl sulfuryl fluoride, its consumption is the 3%-20% of electrophoresis particle consumption, polymer dispersant comprises succimide class spreading agent, CH series auxiliary agent and derivative of fatty acid class hyper-dispersant, and its consumption is respectively 3%-25%, 6%-40% and the 3%-30% of electrophoresis particle consumption;
Above-mentioned particle percentage composition is the quality percentage composition.
2. the preparation method of the black-white electrophoresis display liquid of the electrophoresis showed of claim 1 is characterized in that comprising the following steps:
(1) titanium dioxide white electrophoresis particle, succimide class spreading agent, CH series auxiliary agent and Isopar series dispersion medium are mixed rear ball milling 20h-48h by a certain percentage, obtain white electrophoresis disclosing solution;
(2) carbon black black electrophoretic particles, succimide class spreading agent, CH series auxiliary agent and Isopar series dispersion medium are mixed rear ball milling 20h-48h, obtain the black electrophoresis disclosing solution;
(3) the black and white electrophoresis disclosing solution with preparation is the 1:15-1:30 mixing in mass ratio, adds fluorinated surfactant and derivative of fatty acid class hyper-dispersant and mixes.
3. according to the preparation method of black-white electrophoresis display liquid claimed in claim 2, it is characterized in that: the spreading agent that adds after black-white electrophoresis display liquid mixes is fluorinated surfactant and derivative of fatty acid class hyper-dispersant.
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| JP2017146457A (en) * | 2016-02-17 | 2017-08-24 | セイコーエプソン株式会社 | Electrophoretic dispersion liquid, electrophoretic sheet, electrophoretic device, and electronic apparatus |
| CN109434094B (en) * | 2018-10-29 | 2021-10-22 | 广州鑫威纳科技有限公司 | Nano metal wire dispersion liquid and preparation and application thereof |
| CN111323983B (en) * | 2020-03-19 | 2021-12-03 | 深圳秋田微电子股份有限公司 | Electrophoresis liquid for improving low-temperature resistance of electronic paper |
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| US6241921B1 (en) * | 1998-05-15 | 2001-06-05 | Massachusetts Institute Of Technology | Heterogeneous display elements and methods for their fabrication |
| CN1704176A (en) * | 2004-06-02 | 2005-12-07 | 精工爱普生株式会社 | Manufacturing method of electrophoretic display sheet material, electrophoretic display sheet material and purposes thereof |
| CN1979319A (en) * | 2005-12-01 | 2007-06-13 | 北京化工大学 | Method for preparing black-white electrophoresis display liquid used for electronic ink |
| CN101794051A (en) * | 2010-02-08 | 2010-08-04 | 天津大学 | Method for preparing microcup electrophoretic display device and method for preparing electrophoretic display solution |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6241921B1 (en) * | 1998-05-15 | 2001-06-05 | Massachusetts Institute Of Technology | Heterogeneous display elements and methods for their fabrication |
| CN1704176A (en) * | 2004-06-02 | 2005-12-07 | 精工爱普生株式会社 | Manufacturing method of electrophoretic display sheet material, electrophoretic display sheet material and purposes thereof |
| CN1979319A (en) * | 2005-12-01 | 2007-06-13 | 北京化工大学 | Method for preparing black-white electrophoresis display liquid used for electronic ink |
| CN101794051A (en) * | 2010-02-08 | 2010-08-04 | 天津大学 | Method for preparing microcup electrophoretic display device and method for preparing electrophoretic display solution |
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