CN101333352B - Process for preparing electronic ink by using light complex functional ball of optical subwavelength - Google Patents
Process for preparing electronic ink by using light complex functional ball of optical subwavelength Download PDFInfo
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- CN101333352B CN101333352B CN 200710118122 CN200710118122A CN101333352B CN 101333352 B CN101333352 B CN 101333352B CN 200710118122 CN200710118122 CN 200710118122 CN 200710118122 A CN200710118122 A CN 200710118122A CN 101333352 B CN101333352 B CN 101333352B
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Abstract
The invention relates to a method for preparing electronic ink from light composite function ball at sub-optical wavelength. Mixing dispersant and organic solvent, oscillating with ultrasonic wave, adding light composite function ball at sub-optical wavelength and blending, thus obtaining light composite function ball suspension at sub-optical wavelength with bistability; then adding background dye and mixing, thus obtaining electrophoretic display liquid, namely the electronic ink; or dispersing the light composite function ball at sub-optical wavelength in organic solvent, oscillating with ultrasonic wave, heating to 105-120 DEG C, adding Tissuemat E gradually and blending, thus obtaining light composite function ball suspension at sub-optical wavelength with bistability; then adding background dye and dispersant and mixing, thus obtaining electrophoretic display liquid, namely the electronic ink. Electronic paper display units made from the electronic ink are of good mechanical property, wear resistance, pressure resistance, impact resistance and quick response, and the images produced have clear boundaries, high contrast grade and high resolution.
Description
Technical field
The invention belongs to the electric ink field, particularly a kind of light complex functional ball that adopts optical subwavelength prepares the method for electric ink.
Technical background
The modern displays technology has experienced the triple-substituted development at present, Electronic Paper is as brand-new display device, compare with cathode-ray tube display, liquid-crystal display and the thin-film electroluminescence (TFEL) flat-panel monitor in modern times, have following advantage: one, volume is little, and is lighter, thin than TFT LCD, the STN LCD module of current use.Two, power and energy saving does not need background light source, and image can passively be kept, just power consumption when having only picture to change, and current consumption can reduce more than 90% than LCD.Three, good contrast, big, the readability of visible angle, reflectivity is higher than reflective LCD, and contrast gradient is better than general newspaper.The product of some manufacturer even can reach is xeroxed with paper level (so naked eyes are to the easier identification of its shown word content).Four, recycle the advantage that displaying contents can be brought in constant renewal in as required.Five, soft, good portability, the Electronic Paper watch-dog has pliability or can curl.Therefore, Electronic Paper not only will write down relevant industries to information and bring revolutionary variation, and can hold in e-book, library automation, low consumption and to have wide and profound application prospect aspect indicating meter, large-scale outdoor billboard and the folding display equipment.
The research and development of Electronic Paper have been passed by more than 30 days so far, but along with the emerging of rollable display of making of electronics paper and digital notification board, ultrathin display and Electronic Paper become remarkable focus.The research and development of electronic paper technology mainly concentrate on the research centre of more external large-scale companies, and there are U.S. Gyricon company, Dutch iRex, U.S. E-INK company, Japanese relief printing plate company, U.S. Sipix company and Dutch Philips company in representative famous offshore company of several families.And the research of domestic relevant Electronic Paper is also at the early-stage, and all is to belong to follow-up study.
The preparation method of Electronic Paper has four kinds: screw technology, microcapsulary, minute-pressure mould technology and electric moistening technique of display.Sipix company adopts precision die to extrude little glass of array of regular arrangement in length and breadth on plastic substrate, and each little glass of size is loaded suspension and realized electrophoresis showed about 50～200um in little cup.U.S. MIT and E-Ink company utilize microcapsulary, put into materials such as the suspension that contains dark dye, charged light particles in transparent microcapsule.In the end of the year 2003, Philips company proposes electric moistening technique of display and prepares Electronic Paper.
Microcapsulary is the general demonstration means (U.S. Pat 5961804 and US5930026) of current Electronic Paper research and commerical prod, but there are a lot of not enough (U.S. Pat 6017584) in this method.For example microcapsule are difficult to preparation evenly, the non-constant width of size-grade distribution, and problem such as the aging easily display unit contrast gradient that causes of breaking or the like of cyst wall is low, the life-span is short.Also broad of the distribution of sizes of the inner colour developing electrophoresis particle of filling of microcapsule in addition, and not spherical, therefore surface charge distributes also irregular, be easy to sedimentation, and non-sphere is moved under electric field action and is caused intergranular bridging easily, influence other particulate swimming, so the resolving power of display unit is low.
Summary of the invention
The purpose of this invention is to provide the method that a kind of light complex functional ball that adopts optical subwavelength prepares electric ink, the electric ink response of preparing according to this method rapidly, contrast gradient is high.
The present invention adopts the controlled technology of preparing of nanometer to set size by demand, the scale production size distribution is even, and the optical subwavelength light complex functional ball that specific refractory power is high, it is modified to the electrophoresis particle with bi-stable function, the preparation electric ink, fill it in the little cup of photoetching, be assembled into brand-new electronic paper display device with active driving.The optical subwavelength light complex functional ball that the present invention adopts is electrically charged evenly, and response speed is fast under electric field action, has good bistability.Prepared display device of electronic paper good mechanical property, wear-resisting, withstand voltage, shock-resistant, response is rapid etc., and can control the size of display device as required, cuts out, the image boundary that is obtained is clear, contrast gradient is high, resolving power is high.
The method that the light complex functional ball of employing optical subwavelength of the present invention prepares electric ink comprises the steps:
(1). optical subwavelength light complex functional ball (electrophoresis particle) is modified, obtained having the optical subwavelength light complex functional ball of bi-stable function;
Electric charge is controlled dispersion agent mix with organic solvent, ultra-sonic oscillation add optical subwavelength light complex functional ball (electrophoresis particle), stir, and obtain containing the suspension that is modified to the optical subwavelength light complex functional ball with bi-stable function;
(2). the contain suspension, the background dye that are modified to the optical subwavelength light complex functional ball with bi-stable function that step (1) is obtained are mixed into an electrophoresis disclosing solution, and ultra-sonic oscillation promptly obtain electric ink;
Wherein the optical subwavelength light complex functional ball with bi-stable function in the electric ink accounts for 1～30wt% of electric ink cumulative volume, and background dye accounts for 0.1～5wt%, and electric charge control dispersion agent accounts for 1～20wt%, and all the other are organic solvent;
Or
(1 '). optical subwavelength light complex functional ball (electrophoresis particle) is modified, obtained having the optical subwavelength light complex functional ball of bi-stable function;
Under agitation, optical subwavelength light complex functional ball (electrophoresis particle) is distributed in the organic solvent, ultra-sonic oscillation, be warming up to 105～120 degrees centigrade, slowly add Ployethylene Wax with respect to organic solvent amount 0.1～5wt%, stir, obtain containing the suspension that is modified to optical subwavelength light complex functional ball with bi-stable function;
(2 '). suspension, background dye, electric charge control dispersant that step (1 ') containing of obtaining is modified to the optical subwavelength light complex functional ball with bi-stable function are an electrophoresis disclosing solution, and ultra-sonic oscillation promptly obtain electric ink;
Wherein the optical subwavelength light complex functional ball with bi-stable function in the electric ink accounts for 1～30wt% of electric ink cumulative volume, and background dye accounts for 0.1～5wt%, and electric charge control dispersion agent accounts for 1～20wt%, and all the other are organic solvent and Ployethylene Wax;
The electric ink perfusion that step (2) or step (2 ') are obtained, be packaged in the little cup of the demonstration of adopting the photoetching technique preparation, driving circuit and the little cup that has encapsulated are fit together, finish the assembling (assembling of whole principle device) of little cup and driving circuit, can obtain electronic paper display device.
Described electric charge control dispersion agent is: the byk161 or the byk110 of German Bi Ke chemical company, or the DP-983 of the modest chemical company of Taiwan moral, or monoalkoxytitanates coupling agent (NDZ-101) etc.
Described background dye is solvent green, oil red, nigrosine or solvent blue etc.
Described organic solvent is a zellon.
The optical subwavelength light complex functional ball that the present invention adopts is electrically charged evenly, and response speed is fast under electric field action, has good bistability.Described optical subwavelength lightweight compound ball can be clad structure, hollow structure, meso-hole structure, and its grain size is 150～400 nanometers.
A kind of preferred version, wherein said optical subwavelength light complex functional ball is titanium dioxide ball (preparation method sees the method for making and the spherical particulate preparation method of patent of invention 99123760.9 uniform compound monodispersed nm titanium dioxide of the monodisperse spherical titanium oxide colloid particle that patent of invention 200410009206.7 sizes and pattern are controlled), mesoporous TiO 2 ball (preparation method of the monodisperse spherical mesoporous titanium oxide colloid particle that patent of invention 200610011885.0 sizes and pattern are controlled), zinc oxide and titanium dioxide composite particle (preparation method sees that 200310122438.9 surfaces have spherical zinc oxide and titanium dioxide composite particle and the method for making and the purposes of microgranular texture).
A kind of preferred version, it is that to adopt concentration be the electric charge control dispersion agent of 1～20wt% for optical subwavelength ball with clad structure, hollow structure, meso-hole structure that wherein said optical subwavelength light complex functional ball is modified, perhaps concentration is Ployethylene Wax (PE) coating of 0.1～5wt%, is modified to the electrophoresis particle with bi-stable function.Electric charge control dispersion agent is: byk161, the byk110 of German Bi Ke chemical company, the DP-983 of the modest chemical company of Taiwan moral or monoalkoxytitanates coupling agent (NDZ-101) etc.Utilize the dispersion agent modification as follows: optical subwavelength light complex functional ball ultra-sonic dispersion in organic solvent, is added the electric charge control dispersant with respect to organic solvent amount 1～20wt%.Utilize the process of the cured coating decoration of PE as follows: lightweight function compound ball ultra-sonic dispersion in organic solvent, is warming up to 105～120 degrees centigrade, and slowly adding is cured with respect to the PE of organic solvent amount 0.1～5wt%, stirs 2～3 hours.
Described organic solvent is a zellon.
Little cup is a kind of electrophoresis microchamber that adopts fabrication techniques such as photoetching or minute-pressure mould, because these method controllable size, material property is stable, has overcome the shortcoming of microcapsule effectively; And because the restriction of microchamber makes electrophoretic image show that the turbulent susceptibility reduces greatly to external world, the structure of easier reaching " bistable "; Wall thickness also can be adjusted between little cup, improved greatly withstand voltage, performance such as scrape; Because the consistence of little glass of height makes the electrophoresis liquid of different batches, different zones have identical electrophoretic property, is convenient to the design of pilot circuit.
It is the electrophoresis particle of electric ink that the present invention adopts the optical subwavelength light complex functional ball, and electrically charged even, response speed is fast under electric field action, has good bistability.Utilize the display device of electronic paper good mechanical property of this electric ink preparation, wear-resisting, withstand voltage, shock-resistant, response rapidly, the image boundary that is obtained is clear, contrast gradient, resolving power are high, and can control the size of display device as required, cut out.
Embodiment
The present invention is described further below by specific embodiment.
Embodiment 1
Adopting patent of invention 200410009206.7 " method for making of the monodisperse spherical titanium oxide colloid particle that size and pattern are controlled " preparation particle diameter is that 250nm, relative standard deviation are 9% titanium dioxide ball, further modifies as the core electrophoresis particle with this titanium dioxide ball.With the zellon is dispersion solvent, splash into the byk161 dispersion agent of relative quantity of solvent 3wt%, ultra-sonic oscillation 20～30 minutes, under vigorous stirring, slowly add the titanium dioxide ball of relative quantity of solvent 20wt% in batches, finish the preparation and the modification of optical subwavelength light complex functional ball (electrophoresis particle).The suspension of method for preparing is diluted with zellon, the content of electrophoresis particle accounts for suspension cumulative volume 10wt%, and ultra-sonic oscillation 40 minutes slowly add the oil soluble indigo plant that accounts for suspension cumulative volume 1.5wt% in batches under vigorous stirring, ultra-sonic oscillation 30 minutes obtain electric ink.
Electric ink is filled in the little cup of photocuring, encapsulates.Driving circuit fits together with the microchamber that has encapsulated, finishes the assembling of whole principle device.
Embodiment 2
Adopting patent of invention 99123760.9 " the spherical particulate preparation method of uniform compound monodispersed nm titanium dioxide " preparation particle diameter is that 300nm, relative standard deviation are 7% titanium dioxide ball, further modifies as the core electrophoresis particle with this titanium dioxide ball.With the zellon is dispersion solvent, splashes into the byk110 dispersion agent of relative quantity of solvent 20wt%, ultra-sonic oscillation 20～30 minutes, the slow titanium dioxide ball that in batches adds relative quantity of solvent 20wt% under vigorous stirring.Finish the preparation and the modification of optical subwavelength light complex functional ball (electrophoresis particle).The suspension of method for preparing is diluted with zellon, the content of electrophoresis particle accounts for suspension cumulative volume 1wt%, suspension ultra-sonic oscillation 20 minutes, under vigorous stirring, slowly add the oil soluble indigo plant that accounts for suspension cumulative volume 0.1wt% in batches, ultra-sonic oscillation 30 minutes obtain electric ink.
Electric ink is filled in the little cup of photocuring, encapsulates.Driving circuit fits together with the microchamber that has encapsulated, finishes the assembling of whole principle device.
Embodiment 3
Adopting patent of invention 200610011885.0 " preparation method of the monodisperse spherical mesoporous titanium oxide colloid particle that size and pattern are controlled " preparation particle diameter is that 400nm, relative standard deviation are 10% mesoporous TiO 2 ball, further modifies as the core electrophoresis particle with this mesoporous TiO 2 ball.With the zellon is disperse phase, splashes into the DP-983 dispersion agent of relative quantity of solvent 1wt%, ultra-sonic oscillation 20～30 minutes, the slow mesoporous TiO 2 ball that in batches adds relative quantity of solvent 22wt% under vigorous stirring.Finish the preparation and the modification of optical subwavelength light complex functional ball (electrophoresis particle).The suspension of method for preparing is diluted with zellon, the content of electrophoresis particle accounts for suspension cumulative volume 20wt%, suspension ultra-sonic oscillation 30 minutes, slowly to add the oil soluble that accounts for suspension cumulative volume 0.8wt% under vigorous stirring green in batches, ultra-sonic oscillation 30 minutes obtain electric ink.
Electric ink is filled in the little cup of photocuring, encapsulates.Driving circuit fits together with the microchamber that has encapsulated, finishes the assembling of whole principle device.
Embodiment 4
Employing patent of invention 200610011885.0 " preparation method of the monodisperse spherical mesoporous titanium oxide colloid particle that size and pattern are controlled " preparation 350nm, relative standard deviation are 10% mesoporous TiO 2 ball, further modify as the core electrophoresis particle with this mesoporous TiO 2 ball.With the zellon is dispersion solvent, slowly adds the mesoporous TiO 2 microballoon of relative dispersion solvent amount 15wt% under the vigorous stirring.Ultra-sonic oscillation 30 minutes, be warming up to 105 degrees centigrade, slowly add Ployethylene Wax with respect to quantity of solvent 1wt%, stir after 2 hours, naturally cooling, obtain the mesoporous silica spheres (electrophoresis particle) that the surface coats Ployethylene Wax, finish the preparation and the modification of optical subwavelength light complex functional ball.The above-mentioned zellon suspension ultra-sonic oscillation 40 minutes that will contain the electrophoresis particle of 16wt%, under vigorous stirring, slowly add in batches and account for the nigrosine of suspension cumulative volume 1wt% and the byk161 dispersion agent of 3wt%, ultra-sonic oscillation 30 minutes obtain electric ink.
Electric ink is filled in the little cup of photocuring, encapsulates.Driving circuit fits together with the microchamber that has encapsulated, finishes the assembling of whole principle device.
Embodiment 5
Adopting patent of invention 200310122438.9 " surface has spherical zinc oxide and titanium dioxide composite particle and the method for making and the purposes of microgranular texture " preparation particle diameter is that 240nm, relative standard deviation are 10% zinc oxide and titanium dioxide composite particle, further modifies as the core electrophoresis particle with this composite particles.With the zellon is dispersion solvent, splash into the NDZ-101 dispersion agent of relative dispersion solvent amount 2wt%, ultra-sonic oscillation 30 minutes, under vigorous stirring, slowly add zinc oxide and the titanium dioxide composite particle of relative dispersion solvent amount 12wt% in batches, finish the preparation and the modification of optical subwavelength light complex functional ball (electrophoresis particle).Above-mentioned suspension is diluted with zellon, the content of electrophoresis particle accounts for the 5wt% of suspension cumulative volume, suspension ultra-sonic oscillation 40 minutes, and the slow oil soluble that accounts for suspension cumulative volume 1.1wt% that in batches adds is red under vigorous stirring, ultra-sonic oscillation 30 minutes obtain electric ink.
Electric ink is filled in the little cup of photocuring, encapsulates.Driving circuit fits together with the microchamber that has encapsulated, finishes the assembling of whole principle device.
Embodiment 6
Adopting patent of invention 200610011885.0 " preparation method of the monodisperse spherical mesoporous titanium oxide colloid particle that size and pattern are controlled " preparation particle diameter is that 350nm, relative standard deviation are 10% mesoporous TiO 2 ball, further modifies as the core electrophoresis particle with this mesoporous TiO 2 ball.With the zellon is dispersion solvent, slowly adds under the vigorous stirring with respect to the mesoporous TiO 2 ball that disperses dosage 15wt%, ultra-sonic oscillation 30 minutes, be warmed up to 120 degrees centigrade, slowly add, stir after 3 hours, naturally cooling with respect to dispersion agent 5% Ployethylene Wax.Obtain the mesoporous TiO 2 ball (electrophoresis particle) that the surface coats Ployethylene Wax, finish the preparation and the modification of optical subwavelength light complex functional ball.The zellon suspension ultra-sonic oscillation 30 minutes that will contain the above-mentioned electrophoresis particle of 20w%, under vigorous stirring, slowly add in batches and account for the nigrosine of suspension cumulative volume 1wt% and the byk161 dispersion agent of 3wt%, ultra-sonic oscillation 30 minutes obtain electric ink.
Electric ink is filled in the little cup of photocuring, encapsulates.Driving circuit fits together with the microchamber that has encapsulated, finishes the assembling of whole principle device.
Claims (3)
1. a light complex functional ball that adopts optical subwavelength prepares the method for electric ink, it is characterized in that this method may further comprise the steps:
(1 '). under agitation, the optical subwavelength light complex functional ball is distributed in the organic solvent, ultra-sonic oscillation, be warming up to 105～120 degrees centigrade, slowly add Ployethylene Wax with respect to organic solvent amount 0.1～5wt%, stir, obtain containing the suspension that is modified to optical subwavelength light complex functional ball with bi-stable function;
(2 '). suspension, background dye, electric charge control dispersant that step (1 ') containing of obtaining is modified to the optical subwavelength light complex functional ball with bi-stable function are an electrophoresis disclosing solution, and ultra-sonic oscillation promptly obtain electric ink;
Wherein the optical subwavelength light complex functional ball with bi-stable function in the electric ink accounts for 1～30wt% of electric ink cumulative volume, and background dye accounts for 0.1～5wt%, and electric charge control dispersion agent accounts for 1～20wt%, and all the other are organic solvent and Ployethylene Wax;
Described optical subwavelength light complex functional ball is titanium dioxide ball, mesoporous TiO 2 ball or zinc oxide and titanium dioxide composite particle;
The structure of described titanium dioxide ball, mesoporous TiO 2 ball or zinc oxide and titanium dioxide composite particle is clad structure, hollow structure or meso-hole structure, and its grain size is 150～400 nanometers;
Described electric charge control dispersion agent is the byk 161 or the byk 110 of German Bi Ke chemical company, or the DP-983 of the modest chemical company of Taiwan moral, or the monoalkoxytitanates coupling agent.
2. method according to claim 1 is characterized in that: described organic solvent is a zellon.
3. method according to claim 1 is characterized in that: described background dye is solvent green, oil red, nigrosine or oily molten basket.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102757681A (en) * | 2012-06-21 | 2012-10-31 | 京东方科技集团股份有限公司 | Electronic ink and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102757681A (en) * | 2012-06-21 | 2012-10-31 | 京东方科技集团股份有限公司 | Electronic ink and preparation method thereof |
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