CN102314039A - 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 be used for the composition and preparation method thereof of the black-white electrophoresis display liquid of electrophoresis showed; Be particularly related to the titanium dioxide nano-particle is white electrophoretic particles; The carbon black nano particle is a black electrophoretic particles; Isopar is a dispersion medium, and fluorochemical surfactant and polymkeric substance are spreading agent, the two apparent 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: CRT Displays, liquid crystal display, TFEL FPD and electrophoresis showed etc.Electrophoresis showed is in the seventies in 20th century, is at first proposed by MAT, is to utilize the color band charged under electric field, to move and develop the color.Electrophoresis showed has caused extensive concern 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 under effect of electric field, moves, and makes two kinds of various 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 steady suspension that is made up 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 the 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 in three more than ten years, never interrupt 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 obtain the particle of electric charge easily.Generally should possess following condition: (1) for the coagulation that reduces and reduce particle or floating, and what its density should be with dispersion medium is approaching; (2) particle should have low solubility, unsoluble-unexpansive and chemical stability in organic solvent; (3) particle should have the good optical performance, 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) particle surface is prone to adsorption charge 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 since its excellent optical property, stable chemical property and the person of being studied 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 absorptivity of light owing 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; No swelling, its surface is prone to adsorption charge, is prone to 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 insulation performance property organic solvent, promptly have lower specific inductive capacity, higher resistivity and lower water-soluble; (3) have good optical and electrochemical stability; (4) good mobility of particle, promptly the dynamics viscosity is low; (5) refractive index of dispersion medium and particle and density are complementary, to increase the stability of system; (6) should have low toxicity, promptly 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, because its chemical constitution instability and cost are higher, is not used now.Halogenated hydrocarbons density is bigger, can be composite with color density less aliphatic hydrocarbon or aromatic hydrocarbons, regulate the density of dispersion medium through regulating compound proportion, and be complementary in the hope of reaching with particle density.But because the halogenated hydrocarbons part is volatile, and not enough environmental protection, its application is restricted.And the isoparaffin that the present invention adopts (Isopar series) is cheap and easy to get owing to its stable chemical property, and not volatile, has good compatibility to can be used as new dispersion medium with environment and substitutes the most frequently used halogenated hydrocarbons at present.
Spreading agent commonly used is divided into two types of traditional spreading agent and hyper-dispersants.
The organism that the tradition spreading agent is made up of the polar group of possess hydrophilic property and the non-polar group with hydrophobic nature is adsorbed on the particle surface, and the surface free energy of particle is obviously reduced, and increases the dispersion stabilization of electrophoresis particle.Spreading agent like 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 it is contained less in these spreading agents with the effective electric charge that combines of TiO 2 particles or carbon black particle surface; Therefore the electrophoresis liquid response time for preparing is longer, can not satisfy the requirement of e-book.
Hyper-dispersant is one type of multi-functional wetting dispersing agent of specific polymers type; Its action principle and traditional spreading agent are similar, and difference is that hyper-dispersant contains a plurality of anchoring groups, and be more obvious for the particle dispersion effect of low polarity; But because 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 all is suitable for, like 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, is that the display device contrast of black-white electrophoresis display liquid preparation of dispersion medium is higher with the zellon, and response speed is very fast; And to less with the research of the dispersion medium of the good Isopar of Environmental compatibility series, and with Isopar series be dispersion medium the black-white electrophoresis display liquid preparation display device 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; Through adding suitable spreading agent and surfactant; The display device contrast of preparing is high, and response speed is fast, has met or exceeded the display effect when being dispersion medium with the zellon.Finally use with the good Isopar series of Environmental compatibility replaced with the relatively poor zellon of Environmental compatibility as spreading agent, prepared the black-white electrophoresis display liquid of environmental type.
Summary of the invention
The purpose of this invention is to provide a kind of composition of the black-white electrophoresis display liquid that is used for electrophoresis showed and the method for preparation thereof; With Isopar series isoparaffin is dispersion medium; Titania and carbon black particle are the two black-white electrophoresis display liquids that show of electrophoresis particle preparation; This electrophoresis disclosing solution has dispersiveness and charging property preferably, can be used to prepare 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 when increasing the particle dispersion stabilization, increase electrophoresis particle surface electric charge amount, helps 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, help 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, at present this type surfactant as adjuvant be applied in the electrophoresis liquid research also seldom.
Concrete technical scheme is following:
The invention provides a kind of composition that is used for the black-white electrophoresis display liquid of 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 the mass ratio of black electrophoresis liquid and white electrophoresis liquid is 1 in the black-white electrophoresis display liquid: 15-1: 30.
(2) Isopar series electrophoretic dispersion medium is preferentially selected 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.
TiO 2 particles concentration is 10%-50% in the white electrophoresis liquid of the present invention, and carbon black particle concentration is 3%-20% in the black electrophoresis liquid; If electrophoresis particle concentration is low excessively, then the electrophoresis disclosing solution shape that is translucent does not reach desired contrast; If the electrophoresis particle excessive concentration, then 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 the mass ratio of black electrophoresis liquid and white electrophoresis liquid is 1 in the black-white electrophoresis display liquid: 15-1: 30; If the black electrophoretic particles ratio is excessive, then electrophoresis disclosing solution becomes grey black, and white attitude reflectivity is too low; If the black electrophoretic particles ratio is too small, then black electrophoretic particles is difficult to hide fully white electrophoretic particles, and the electrophoresis disclosing solution contrast of formation is low excessively.
The electrophoretic dispersion medium that the present invention adopts is an Isopar series isoparaffin, and it has higher boiling point and lower fusing point, and insulativity is good; Lower specific inductive capacity, higher resistivity and lower water-soluble are arranged; Good optical 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 because 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 demonstration contrast and the difference of 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), and its molecular structure can be divided into two parts, and a part is an anchoring group; Main effect is with spreading agent adsorbed close and electrophoresis particle surface, prevents that it from coming off; Another part is a solvent chain, and main effect is to form certain thickness protective seam on the electrophoresis particle surface, 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, then spreading agent and electrophoresis particle are surperficial contacts insufficiently, and electrophoresis particle can not well be scattered among the Isopar, the electrophoresis dispersion poor stability; If dispersant dosage is too much, electrophoresis disclosing solution thickness too then, electrophoresis disclosing solution is prone to cohesion and low-response, and contrast is low.
The invention provides a kind of preparation method who is used for the black-white electrophoresis display liquid of 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 back 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 back 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 by 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 week back observation and show that liquid still keeps stable.Electrophoresis disclosing solution of the present invention is processed 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; Showing the 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 spare under electric field of apparent 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, (b) is the black matrix wrongly written or mispronounced character.
Embodiment
Instance 1
In the ball milling bottle, add the Isopar G of 10mL, the T31 of 0.05g, CH-5 and the 1.00g TiO of 0.10g
2Nano particle or 0.30g carbon black nano particle are abrasive media with 2mm zirconia zirconium pearl, under rotating speed 600r/min, grind 20h, 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 promptly obtain black and white particle electrophoresis demonstration liquid.
Electrophoresis disclosing solution of the present invention is put into the sedimentation bottle, place week back observation and show that liquid still keeps stable.Electrophoresis disclosing solution of the present invention is filled in the 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 showing the black time is 945ms, and the whitening time is 1163ms.
Instance 2
In the ball milling bottle, add the Isopar H of 10mL, the T152 of 0.20g, CH-6 and the 5.00g TiO of 0.50g
2Nano particle or 2.00g carbon black nano particle are abrasive media with 2mm zirconia zirconium pearl, under rotating speed 600r/min, grind 24h, 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 promptly obtain black and white particle electrophoresis demonstration liquid.
Electrophoresis disclosing solution of the present invention is put into the sedimentation bottle, place week back observation and show that liquid still keeps stable.Electrophoresis disclosing solution of the present invention is filled in the 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 showing the black time is 1107ms, and the whitening time is 1244ms.
Instance 3
In the ball milling bottle, add the Isopar L of 10mL, the T151 of 0.10g, CH-13 and the 2.00g TiO of 0.15g
2Nano particle or 0.40g carbon black nano particle are abrasive media with 2mm zirconia zirconium pearl, under rotating speed 600r/min, grind 28h, 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 promptly obtain black and white particle electrophoresis demonstration liquid.
Electrophoresis disclosing solution of the present invention is put into the sedimentation bottle, place week back observation and show that liquid still keeps stable.Electrophoresis disclosing solution of the present invention is filled in the 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 showing the black time is 1032ms, and the whitening time is 1220ms.
Instance 4
In the ball milling bottle, add the Isopar G of 10mL, the T31 of 0.08g, CH-13 and the 2.00g TiO of 0.20g
2Nano particle or 0.50g carbon black nano particle are abrasive media with 2mm zirconia zirconium pearl, under rotating speed 600r/min, grind 32h, 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 promptly obtain black and white particle electrophoresis demonstration liquid.
Electrophoresis disclosing solution of the present invention is put into the sedimentation bottle, place week back observation and show that liquid still keeps stable.Electrophoresis disclosing solution of the present invention is filled in the 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 showing the black time is 827ms, and the whitening time is 1019ms.
Instance 5
In the ball milling bottle, add the Isopar M of 10mL, the T152 of 0.18g, CH-6 and the 4.00g TiO of 0.35g
2Nano particle or 1.00g carbon black nano particle are abrasive media with 2mm zirconia zirconium pearl, under rotating speed 600r/min, grind 36h, 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 promptly obtain black and white particle electrophoresis demonstration liquid.
Electrophoresis disclosing solution of the present invention is put into the sedimentation bottle, place week back observation and show that liquid still keeps stable.Electrophoresis disclosing solution of the present invention is filled in the 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 showing the black time is 1531ms, and the whitening time is 2219ms.
Instance 6
In the ball milling bottle, add the Isopar L of 10mL, the T151 of 0.10g, CH-5 and the 3.00g TiO of 0.20g
2Nano particle or 0.50g carbon black nano particle are abrasive media with 2mm zirconia zirconium pearl, under rotating speed 600r/min, grind 48h, 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 promptly obtain black and white particle electrophoresis demonstration liquid.
Electrophoresis disclosing solution of the present invention is put into the sedimentation bottle, place week back observation and show that liquid still keeps stable.Electrophoresis disclosing solution of the present invention is filled in the 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 showing the black time is 831ms, and the whitening time is 1123ms.
Claims (6)
1. black-white electrophoresis display liquid that is used for electrophoresis showed, its composition comprises:
(1) black and white electrophoresis particle;
(2) Isopar series electrophoretic dispersion medium;
(3) spreading agent is with fluorochemical surfactant and polymer dispersant.
2. according to the described demonstration liquid of claim 1; It is characterized in that: white electrophoretic particles is a titanium dioxide nano-particle; Particle concentration is 10%-50%; Black electrophoretic particles is the carbon black electrophoresis particle, and particle concentration is 3%-20%, and the mass ratio of black electrophoresis liquid and white electrophoresis liquid is 1 in the black-white electrophoresis display liquid: 15-1: 30.
3. according to the described demonstration liquid of claim 1, it is characterized in that: electrophoretic dispersion medium is selected Isopar series for use.
4. according to the described demonstration liquid of claim 1; It is characterized in that: spreading agent is with 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 (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.
5. the preparation method of the black-white electrophoresis display liquid of the electrophoresis showed of claim 1 is characterized in that may further comprise the steps:
(1) titanium dioxide white electrophoresis particle, succimide class spreading agent, CH series auxiliary agent and Isopar series dispersion medium are mixed back 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 back ball milling 20h-48h, obtain the black electrophoresis disclosing solution;
(3) the black and white electrophoresis disclosing solution with preparation is 1 by mass ratio: 15-1: 30 mix, and add fluorinated surfactant and derivative of fatty acid class hyper-dispersant and mix.
6. according to the preparation method of the described black-white electrophoresis display liquid of claim 5, it is characterized in that: it is fluorinated surfactant and derivative of fatty acid class hyper-dispersant that black-white electrophoresis display liquid mixes the spreading agent that adds the back, and its addition is 3%-30%.
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CN107092149A (en) * | 2016-02-17 | 2017-08-25 | 精工爱普生株式会社 | Electrophoresis dispersion, electrophoretic sheet, electrophoretic apparatus and electronic equipment |
CN109434094A (en) * | 2018-10-29 | 2019-03-08 | 广州鑫威纳科技有限公司 | Nano metal line dispersion liquid and its preparation and application |
CN111323983A (en) * | 2020-03-19 | 2020-06-23 | 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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Publication number | Priority date | Publication date | Assignee | Title |
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CN107092149A (en) * | 2016-02-17 | 2017-08-25 | 精工爱普生株式会社 | Electrophoresis dispersion, electrophoretic sheet, electrophoretic apparatus and electronic equipment |
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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 |
CN111323983A (en) * | 2020-03-19 | 2020-06-23 | 深圳秋田微电子股份有限公司 | Electrophoresis liquid for improving low-temperature resistance of electronic paper |
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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