CN102213888A - Preparation method of electrophoretic display solution - Google Patents
Preparation method of electrophoretic display solution Download PDFInfo
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- CN102213888A CN102213888A CN 201110088392 CN201110088392A CN102213888A CN 102213888 A CN102213888 A CN 102213888A CN 201110088392 CN201110088392 CN 201110088392 CN 201110088392 A CN201110088392 A CN 201110088392A CN 102213888 A CN102213888 A CN 102213888A
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Abstract
The invention discloses a preparation method of an electrophoretic display solution. The method comprises the following steps of: adding 5-50 ml of tetrachloroethylene, 0.1-1.0 gram of polyisobutene mono-succinimide series serving as a charge control agent, 0.1-0.5 gram of dehydrated sorbitol tri-oleate series serving as a dispersant and Solspersl7000 serving as a hyper-dispersant, 0.1-1.0 gram of phenolic resin, acrylic ester or polyisobutylene serving as a macromolecule resin stabilizing agent and 3.0-6.0 grams of hollow TiO2 or TiO nanoparticles or carbon black nanoparticles of which the particle sizes are between 50 nanometers and 150 nanometers, into a ball milling bottle; performing ball milling on zirconia balls of 2 millimeters serving as a grinding medium at the speed 500-800 revolutions per minute for 20-30h, wherein a white particle electrophoresis display solution is obtained when the TiO2 particles are white particles, and a black particle electrophoresis display solution is obtained when the TiO or carbon black particles are black particles; and mixing the obtained black and white single-particle electrophoresis display solutions in the mass ratio (10-15):1 of white particles to black particles to obtain black and white double-particle electrophoresis display solutions; and ultrasonically dispersing under the conditions of 100 W and 58 KHz by using an ultrasonic instrument for 30 minutes to obtain the uniformly-dispersed black and white double-particle electrophoresis display solution.
Description
Technical field
The present invention relates to a kind of electrophoresis showed liquid and preparation method thereof.
Background technology
Along with popularizing of development of computer and the Internet, browsing " electronic publication " by media such as computing machines has become a kind of new reading method, but electronic publication can't replace daily newspaper and books.The appearance of Electronic Paper has caused that people pay close attention to greatly.Because it possesses the characteristic of paper and electron device simultaneously, both met people's visual custom, convenient, fast again, but have the characteristics of colorize, Digital Control and multi-sizeization.With respect to traditional paper, the electrophoretic display device (EPD) cost is high slightly, but can combine closely with the digital information technology, can circulate repeatedly and to use, production run does not need to consume big water gaging and timber, when reading and preserving on the paper information, also no longer consuming other energy, is a kind of Green Product.
Electrophoretic display device (EPD) constitutes by two electrode of opposite and with the display medium that is clipped in therebetween, display medium is that one or both charged nano particles are dispersed in the suspending liquid that forms in a kind of insulativity solvent, described devices use electrophoresis under electric field driven charged nano particle to obstructed electrode movement with video data or image.Electrophoretic display device, EDD continues video data and does not consume extra power, unless it receives the electric signal that is used for rewrite operation.Therefore, electrophoretic display device, EDD has the advantage of low energy consumption.
At present, mainly contain two kinds of manufacturing process that prepare little glass, promptly photetching is scribed glass technology and full-automatic at a high speed system cup technology, and is all higher to the requirement of instrument and equipment, and filling and sealing is comparatively complicated.Photetching is scribed a glass technology: be coated with coating one deck radiation curing material on the substrate of conductive film, see through photomask it is carried out selectivity ultraviolet light (or other forms of radiation, as visible light, infrared ray, and electron beam etc.) exposure solidifies, then with the solvent of solubilized radiation curing material will be uncured radiation curing material remove the little cup structure of formation.Full-automatic at a high speed system cup technology: be coated with coating one deck thermosetting substance on the transparency carrier of conductive film, then on the vitrifacation phase transition temperature of thermosetting substance with a punch to its pressure molded cup of rolling, after modes such as cooling or illumination solidify.
Little glass the fluid-tight packing technique of going into has two kinds of one-part form and two-period forms.It is earlier the encapsulated layer material to be scattered in the electrophoresis liquid in advance that one-part form is gone into the fluid-tight packing technique, and layering is floating to the surface rapidly to treat electrophoresis liquid to fill the back, and final curing becomes encapsulating film.It is earlier electrophoresis liquid to be injected little cup that two-period form is gone into the fluid-tight packing technique, the encapsulated layer material is coated on the electrophoresis liquid again, and the encapsulated layer material is through solidifying to form encapsulating film then.
The development of electrophoretic display technology is in the eve of industrialization in the international coverage, though each major company releases state-of-the-art technology and new product frequently, but still is laboratory sample, does not enter large-scale production as yet.Trace it to its cause, except reasons such as through engineering approaches technology imperfection, production cost be high, little glass make and the filling process process of electrophoresis liquid in also have certain difficulty.Therefore, study convenient, simple, practical little glass of manufacture craft and little glass of filling technological method, the test condition of exploring electrophoretic display device, EDD simultaneously has important in being worth to the development of little glass of electrophoretic display technology.
Summary of the invention
The present invention relates to a kind of preparation method and electrophoresis showed liquid and preparation method thereof of little glass of type electrophoretic display device, EDD.It can be avoided because one or more problems that limitation and shortcoming produced of prior art.
Technical scheme of the present invention is as follows:
A kind of electrophoresis showed liquid and preparation method thereof of the present invention, in the ball milling bottle, add zellon 5～50mL, 0.1 charge control agent polyisobutylene mono butonediimide series, 0.1～0.5g spreading agent sorbitan trioleate series and the hyper-dispersant Solspers17000 of～1.0g, 0.1～1.0g macromolecule resin stabilizing agent phenolics, acrylate or polyisobutylene, 3.0～6.0g particle diameter is the hollow TiO of 50～150nm
2, TiO nano particle or carbon black nano particle; With 2mm zirconia zirconium pearl is abrasive media, and ball milling 20～30h under rotating speed 500～800r/min filters suspension with 200 mesh sieve then, and mother liquor is stored in the vial, promptly obtains electrophoresis disclosing solution.
TiO wherein
2When particle is white particles, prepare the white particles electrophoresis disclosing solution; When TiO or carbon black particle are black particles, prepare the black particles electrophoresis disclosing solution.With the black and white single-particle electrophoresis disclosing solution for preparing according to white black track producing particle mass ratio (10～15): 1 ratio mixes and makes the two particle electrophoresises of black and white and show liquid, with ultrasonic instrument ultrasonic dispersion 30min under the condition of 100W, 58KHz, obtain the two particle electrophoresises of finely dispersed black and white and show liquid.
Effect of the present invention provides the manufacture craft of a kind of convenience, simple, practical little glass of electrophoretic display device, EDD, and the method for the display effect of estimating electrophoretic display device, EDD is provided simultaneously.
Description of drawings
The included accompanying drawing of the application is used to provide to further understanding of the present invention, and is included in this instructions and as the part of this instructions, shows embodiments of the present invention and be used to explain principle of the present invention together with the description.
In the accompanying drawings:
Fig. 1 is that little cupule spare is made process flow diagram;
Fig. 2 is the etching effect picture;
Fig. 3 is the little lattice deformation of a nylon photo;
Fig. 4 is the contrast black-and-white display photo of the little lattice of nylon;
Fig. 5 is for showing the change curve of contrast with particle concentration;
Fig. 6 is for showing the change curve of contrast with white black track producing particle mass ratio;
Fig. 7 is for showing the change curve of contrast with electric field intensity;
Fig. 6 is for showing the change curve of contrast with resin concentration;
Fig. 9 is 0.02V/ μ m for electric field intensity, black and white character pattern display photos;
Figure 10 is 0.02V/ μ m for electric field intensity, seven sections black and white digital pattern display photos.
Embodiment
Below in conjunction with accompanying drawing the present invention is done further to discuss in detail.
Figure 1 shows that little cupule spare making process flow diagram, detailed step is as follows:
The first step: the preparation of show electrode
For making pattern or the numeral that device demonstrates to be needed, at first on the ito glass of conduction, etch the literal or the pattern of required demonstration.Chemical method etching conductive glass is adopted in this experiment, and flow process is divided into following two parts:
(1) display pattern scribes
Getting a block size is the glass electrode that is coated with the electroconductive ITO layer of 6 * 6cm, cleans its surface to keep clean and tidy with clear water, dries 30min down for 40 ℃～60 ℃ in baking oven.Dip in a little acetone or alcohol with dustless cloth (multiselect silk class) and clean the ITO conductive layer, after drying up fast with hair-dryer, conductive layer is lain on the dustless desktop up.
Select for use the adhesive tape about thickness 0.5mm entirely to be layered on the ITO conductive layer, it is protected, flatten compacting,, cause leaking erosion easily in the etching process and spot occurs in case bubble enters.(3.5 * 3.5cm) place under the electro-conductive glass, and justified margin is fixing will to be printed on pattern model on the paper then.With Steel Ruler and technology icking tool, pattern is scribed.After pattern has been scribed, dip in a little acetone or alcohol with dustless cloth (multiselect silk class) and clean the pattern of scribing, do not have remaining adhesive tape to guarantee the ITO laminar surface that need etch away pattern model.Repair cutter with technology pattern edge is modified, guarantee the clean and tidy neat of edge.
(2) the chemical etching technology of display pattern
The preparation of etching liquid: measure distilled water and concentrated hydrochloric acid that quality is 50.0g～70.0g, the solid ferric trichloride of 10.0～14.0g joins in the 500mL beaker successively, ultrasonic agitation on ultrasonic instrument, and dissolving is evenly.
The electro-conductive glass of scribing good pattern is lain against in the double dish, and conducting surface is poured chemical etching liquid into up, and a little gets final product to soak the electro-conductive glass upper surface.Behind 30～40 ℃ of etching 9～11min, take out with tweezers and to place 5%～10% sodium hydrate aqueous solution with the surperficial acid solution that neutralizes, take out and use a large amount of distilled water flushings, afterwards with a little acetone or alcohol drip washing, place 50 ℃ of drying in oven then.
The adhesive tape of protection usefulness is taken off, cleaned conductive layer surface, can obtain having the conductive electrode of pattern, in order to making the usefulness of device with ethanol.Fig. 2 is the etching effect picture.
Second step: the making of little cup (the little lattice of nylon)
Selecting diameter for use is that the solid copper facing bloom of 70mm is a compacting tool set, polished surface vis-a-vis, a little silicone oil of coating on the polished surface (preventing the adhesion of nylon wire and mould in pressing process), the big or small nylon wire piece identical with mould of cutting area places in the middle of the mould.Then mould is placed on the hydropress, at room temperature under 0～6.50Mpa pressure, suppress 10min.
Select for use the little lattice of outsourcing nylon as little glass of base material, little lattice specification is long 160～180 μ m, wide 100～130 μ m, high 65～70 μ m.Between the little lattice of nylon is intercommunication, electrophoresis particle can move between little lattice, agglomeration still exists, adopt pressure sintering that the little lattice of nylon are suppressed, it is suppressed into the little lattice of the display unit with limited microchannel, so just avoid the migration of electrophoresis liquid between little lattice, can eliminate the shortcoming of the reunion and the image attenuation of large tracts of land charged corpuscle, also solved the problem that surface tension is big, can is difficult of single micro unit simultaneously.
After compacting is finished, take out the little lattice piece of nylon, clean, dry, adopt the shape of the little lattice of observation by light microscope nylon, with microphotograph analysis hot compression deformation effect with a little tetrachloroethylene solvent.
The key technical indexes of electrophoretic display device, EDD is contrast, response time and the serviceable life etc. of device.The agglomeration of electrophoresis particle is a key influence factor.It is the main method that solves particle aggregation that electrophoresis particle is enclosed in the single small display unit, and microcapsules and little glass of technology are most popular now two kinds of methods with the display unit microminiaturization.
The little lattice piece of the nylon of suppressing under 0Mpa～6.50Mpa pressure is observed suppression degree under metaloscope, can be clear that the deformation phenomenon from microphotograph.Fig. 3 is the little lattice photo of nylon.
The compacting before the little lattice of nylon in length and breadth the separator bar diameter between 65～70 μ m, be increased to after the compacting between 125～150 μ m, produced bigger distortion, a plocoid spot appears in the cross-point of co-ordination, has played the effect that little lattice is divided into complete independent displaying space.
The 3rd step: the making of little glass of type electrophoresis prototype display device
The electrophoresis disclosing solution nucleus is water-insoluble solvent, charge control agent, spreading agent, macromolecule resin stabilizing agent and pigment particles.In the ball milling bottle, add zellon 5～50mL, 0.1 the charge control agent polyisobutylene mono butonediimide series (T151, T152) of～1.0g, 0.1～0.5g spreading agent sorbitan trioleate series (Span series) and hyper-dispersant (Solspers17000), 0.1～1.0g macromolecule resin stabilizing agent phenolics, acrylate or polyisobutylene, 3.0～6.0g particle diameter is the hollow TiO of 50～150nm
2, TiO nano particle or carbon black nano particle; With 2mm zirconia zirconium pearl is abrasive media, and ball milling 20～30h under rotating speed 500～800r/min filters suspension with 200 mesh sieve then, and mother liquor is stored in the vial, promptly obtains electrophoresis disclosing solution.
(1) the heelpiece electrode preparation is chosen the little lattice sheet of nylon of preparation, determines little lattice piece of 3.5 * 3.5cm.((middle of 6 * 6cm) conducting surface evenly is coated with the poly-vinyl alcohol solution that last layer thickness is about 10～15 μ m to 3.5 * 3.5cm) ITO electro-conductive glass making display pattern or pattern-free, the little lattice of the nylon of above-mentioned preparation are sticking thereon, and making it bonding plain with suitable pressure, oven dry 10min are stand-by down at 30～40 ℃.
Select else with the thick mylar of 100 μ m, cut out the square of 5 * 5cm size, the adopting process icking tool is made the demonstration chamber of size a 3.5 * 3.5cm in its middle.Then this is had the mylar that shows the chamber and stick on the above-mentioned ito glass that pastes the little lattice of nylon, and make and show that the chamber just in time comprises the little lattice of nylon and coincide with epoxy resin.So just made hearth electrode.
(2) preparation of display device coating thickness on the mylar in the demonstration of the formation on the hearth electrode that above-mentioned steps is made chamber is the epoxy resin of 1～5 μ m, get the ITO electro-conductive glass of another sheet 6 * 6cm, make the one side along boning along the back of aliging with a side of the mylar that scribbles epoxy resin.The osculum that will stay about 1mm during making on one side of mylar as inlet so that can.
Draw the electrophoresis disclosing solution for preparing with micro syringe, enter,, influence the attractive in appearance and color developing (, need slowly drive out of, and then carry out can) of device if bubble is arranged in case bubble enters from the even can of inlet.After treating that device is filled, with the bonding edge of adhesive (epoxy resin) and inlet to play the effect of air locking.
The circuit control system design and fabrication
Good driving programming writes in the control chip with adopting the C language compilation, selects the AT89S51 series monolithic for use, builds the bread board circuit according to circuit theory then, and the connection jaws of device is linked to each other with bread board output control terminal mouth.
Driving circuit can provide the driving voltage of 20V, and the demonstration time is designed to 5s, and the refresh interval time is 1s for the second time, and wherein dutycycle, frequency etc. are adjustable.Display device thickness is 150 μ m, and the colour developing area is 4.5 * 3.5cm.
Little lattice of making under the hot pressing under 0Mpa～6.50Mpa pressure are shown as micro unit carry out preparation of devices, on the voltage stabilizing electrophoresis apparatus, test, and adopt the black and white reflectivity size of MN-BW type gray scale instrument test period display effect.Fig. 4 is the contrast black-and-white display photo of the little lattice of nylon.At pressure is that the device that the little lattice of nylon suppressed under the 6.50Mpa are prepared shows that the black and white reflectivity is higher, and contrast can reach 15: 1.
The selection of device detection condition
The demonstration contrast of device detection is the ratio of white reflection rate and black reflectivity, and the white reflection rate is big more, and relative contrast also can be bigger.The concentration of overall particle concentration, white black track producing particle mass ratio, electric field intensity, stabilizing agent macromolecule resin is to showing the highly significant that influences of contrast, shows that therefore the display effect that contrast estimates little cupule spare with the variation tendency of the concentration of overall particle concentration, white black track producing particle mass ratio, electric field intensity, stabilizing agent macromolecule resin is most important.
Little lattice type electrophoretic display device, EDD of manufacturing of the present invention and method of evaluating performance thereof are applicable to the electrophoresis disclosing solution of any white, mineral black particle preparation.
Embodiment 1 (electrophoresis disclosing solution preparation)
In the ball milling bottle, add zellon 5mL, 0.1g charge control agent polyisobutylene mono butonediimide series, 0.1g spreading agent sorbitan trioleate series and hyper-dispersant Solspersl7000,0.1g macromolecule resin stabilizing agent phenolics, acrylate or polyisobutylene, 3.0g particle diameter are the hollow TiO of 120nm
2Nano particle; With 2mm zirconia zirconium pearl is abrasive media, and ball milling 20h under rotating speed 500r/min filters suspension with 200 mesh sieve then, and mother liquor is stored in the vial, promptly obtains white electrophoresis disclosing solution.
Embodiment 2 (electrophoresis disclosing solution preparation)
In the ball milling bottle, add zellon 25mL, 0.5g charge control agent polyisobutylene mono butonediimide series, 0.3g spreading agent sorbitan trioleate series and hyper-dispersant Solspersl7000,0.5g macromolecule resin stabilizing agent phenolics, acrylate or polyisobutylene, 4.0g particle diameter are the carbon black nano particle of 70nm; With 2mm zirconia zirconium pearl is abrasive media, and ball milling 25h under rotating speed 700r/min filters suspension with 200 mesh sieve then, and mother liquor is stored in the vial, promptly obtains electrophoresis disclosing solution.
Embodiment 3 (electrophoresis disclosing solution preparation)
In the ball milling bottle, add zellon 50mL, 1.0g charge control agent polyisobutylene mono butonediimide series, 0.5g spreading agent sorbitan trioleate series and hyper-dispersant Solspersl7000,1.0g macromolecule resin stabilizing agent phenolics, acrylate or polyisobutylene, 6.0g particle diameter are the hollow TiO nano particle of 100nm; With 2mm zirconia zirconium pearl is abrasive media, and ball milling 30h under rotating speed 800r/min filters suspension with 200 mesh sieve then, and mother liquor is stored in the vial, promptly obtains electrophoresis disclosing solution.
Embodiment 4 (electrophoresis disclosing solution preparation)
The black and white single-particle electrophoresis disclosing solution for preparing mixed according to 15: 1 ratio of white black track producing particle mass ratio make the two particle electrophoresises of black and white and show liquid, with ultrasonic instrument ultrasonic dispersion 30min under the condition of 100W, 58KHz, obtain the two particle electrophoresises of finely dispersed black and white and show liquid.
Embodiment 5 (little glass of type electrophoretic display device, EDD)
The first step: the preparation of show electrode
(1) display pattern scribes
Getting a block size is the glass electrode that is coated with the electroconductive ITO layer of 6 * 6cm, cleans its surface to keep clean and tidy with clear water, dries 30min down for 50 ℃ in baking oven.Dip in a little acetone or alcohol with dustless cloth (multiselect silk class) and clean the ITO conductive layer, after drying up fast with hair-dryer, conductive layer is lain on the dustless desktop up.
Select for use the adhesive tape about thickness 0.5mm entirely to be layered on the ITO conductive layer, it is protected, flatten compacting,, cause leaking erosion easily in the etching process and spot occurs in case bubble enters.(3.5 * 3.5cm) place under the electro-conductive glass, and justified margin is fixing will to be printed on pattern model on the paper then.With Steel Ruler and technology icking tool, pattern is scribed.After pattern has been scribed, dip in a little acetone or alcohol with dustless cloth (multiselect silk class) and clean the pattern of scribing, do not have remaining adhesive tape to guarantee the ITO laminar surface that need etch away pattern model.Repair cutter with technology pattern edge is modified, guarantee the clean and tidy neat of edge.
(2) the chemical etching technology of display pattern
The preparation of etching liquid: measure distilled water and concentrated hydrochloric acid that quality is 50.0g, the solid ferric trichloride of 10.0g joins in the 500mL beaker successively, ultrasonic agitation on ultrasonic instrument, and dissolving is evenly.
The electro-conductive glass of scribing good pattern is lain against in the double dish, and conducting surface is poured chemical etching liquid into up, and a little gets final product to soak the electro-conductive glass upper surface.Behind 30 ℃ of etching 9min, take out with tweezers and to place 5% sodium hydrate aqueous solution with the surperficial acid solution that neutralizes, take out and use a large amount of distilled water flushings, afterwards with a little acetone or alcohol drip washing, place 50 ℃ of drying in oven then.
The adhesive tape of protection usefulness is taken off, cleaned conductive layer surface, can obtain having the conductive electrode of pattern, in order to making the usefulness of device with ethanol.
Second step: little glass making
Selecting diameter for use is that the solid copper facing bloom of 70mm is a compacting tool set, polished surface vis-a-vis, a little silicone oil of coating on the polished surface (preventing the adhesion of nylon wire and mould in pressing process), the big or small nylon wire piece identical with mould of cutting area places in the middle of the mould.Then mould is placed on the hydropress, at room temperature under 0Mpa pressure, suppress 10min.
Select for use the little lattice of outsourcing nylon as little glass of base material, little lattice specification is long 160 μ m, wide 100 μ m, high 65 μ m.Between the little lattice of nylon is intercommunication, electrophoresis particle can move between little lattice, agglomeration still exists, adopt pressure sintering that the little lattice of nylon are suppressed, it is suppressed into the little lattice of the display unit with limited microchannel, so just avoid the migration of electrophoresis liquid between little lattice, can eliminate the shortcoming of the reunion and the image attenuation of large tracts of land charged corpuscle, also solved the problem that surface tension is big, can is difficult of single micro unit simultaneously.
After compacting is finished, take out the little lattice piece of nylon, clean, dry, adopt the shape of the little lattice of observation by light microscope nylon, with microphotograph analysis hot compression deformation effect with a little tetrachloroethylene solvent.
The 3rd step: the making of little glass of type electrophoresis prototype display device
(1) the heelpiece electrode preparation is chosen the little lattice sheet of nylon of preparation, determines little lattice piece of 3.5 * 3.5cm.((middle of 6 * 6cm) conducting surface evenly is coated with the poly-vinyl alcohol solution that last layer thickness is about 10 μ m to 3.5 * 3.5cm) ITO electro-conductive glass making display pattern or pattern-free, the little lattice of the nylon of above-mentioned preparation are sticking thereon, and making it bonding plain with suitable pressure, oven dry 10min are stand-by down at 30～40 ℃.
Select else with the thick mylar of 100 μ m, cut out the square of 5 * 5cm size, the adopting process icking tool is made the demonstration chamber of size a 3.5 * 3.5cm in its middle.Then this is had the mylar that shows the chamber and stick on the above-mentioned ito glass that pastes the little lattice of nylon, and make and show that the chamber just in time comprises the little lattice of nylon and coincide with epoxy resin.So just made hearth electrode.
(2) preparation of display device coating thickness on the mylar in the demonstration of the formation on the hearth electrode that above-mentioned steps is made chamber is the epoxy resin of 1 μ m, get the ITO electro-conductive glass of another sheet 6 * 6cm, make the one side along boning along the back of aliging with a side of the mylar that scribbles epoxy resin.The osculum that will stay about 1mm during making on one side of mylar as inlet so that can.
Draw the electrophoresis disclosing solution for preparing with micro syringe, enter,, influence the attractive in appearance and color developing (, need slowly drive out of, and then carry out can) of device if bubble is arranged in case bubble enters from the even can of inlet.After treating that device is filled, with the bonding edge of adhesive (epoxy resin) and inlet to play the effect of air locking.
The circuit control system design and fabrication
Good driving programming writes in the control chip with adopting the C language compilation, selects the AT89S51 series monolithic for use, builds the bread board circuit according to circuit theory then, and the connection jaws of device is linked to each other with bread board output control terminal mouth.
Driving circuit can provide the driving voltage of 30V, and the demonstration time is designed to 5s, and the refresh interval time is 1s for the second time, and wherein dutycycle, frequency etc. are adjustable.Display device thickness is 150 μ m, and the colour developing area is 4.5 * 3.5cm.
Embodiment 6 (little glass of type electrophoretic display device, EDD)
The first step: the preparation of show electrode
(1) display pattern scribes
Getting a block size is the glass electrode that is coated with the electroconductive ITO layer of 6 * 6cm, cleans its surface to keep clean and tidy with clear water, dries 30min down for 50 ℃ in baking oven.Dip in a little acetone or alcohol with dustless cloth (multiselect silk class) and clean the ITO conductive layer, after drying up fast with hair-dryer, conductive layer is lain on the dustless desktop up.
Select for use the adhesive tape about thickness 0.5mm entirely to be layered on the ITO conductive layer, it is protected, flatten compacting,, cause leaking erosion easily in the etching process and spot occurs in case bubble enters.(3.5 * 3.5cm) place under the electro-conductive glass, and justified margin is fixing will to be printed on pattern model on the paper then.With Steel Ruler and technology icking tool, pattern is scribed.After pattern has been scribed, dip in a little acetone or alcohol with dustless cloth (multiselect silk class) and clean the pattern of scribing, do not have remaining adhesive tape to guarantee the ITO laminar surface that need etch away pattern model.Repair cutter with technology pattern edge is modified, guarantee the clean and tidy neat of edge.
(2) the chemical etching technology of display pattern
The preparation of etching liquid: measure distilled water and concentrated hydrochloric acid that quality is 60.0g, the solid ferric trichloride of 12.0g joins in the 500mL beaker successively, ultrasonic agitation on ultrasonic instrument, and dissolving is evenly.
The electro-conductive glass of scribing good pattern is lain against in the double dish, and conducting surface is poured chemical etching liquid into up, and a little gets final product to soak the electro-conductive glass upper surface.Behind 35 ℃ of etching 10min, take out with tweezers and to place 10% sodium hydrate aqueous solution with the surperficial acid solution that neutralizes, take out and use a large amount of distilled water flushings, afterwards with a little acetone or alcohol drip washing, place 50 ℃ of drying in oven then.
The adhesive tape of protection usefulness is taken off, cleaned conductive layer surface, can obtain having the conductive electrode of pattern, in order to making the usefulness of device with ethanol.
Second step: little glass making
Selecting diameter for use is that the solid copper facing bloom of 70mm is a compacting tool set, polished surface vis-a-vis, a little silicone oil of coating on the polished surface (preventing the adhesion of nylon wire and mould in pressing process), the big or small nylon wire piece identical with mould of cutting area places in the middle of the mould.Then mould is placed on the hydropress, at room temperature under 3.20Mpa pressure, suppress 10min.
Select for use the little lattice of outsourcing nylon as little glass of base material, little lattice specification is long 170 μ m, wide 150 μ m, high 65 μ m.Between the little lattice of nylon is intercommunication, electrophoresis particle can move between little lattice, agglomeration still exists, adopt pressure sintering that the little lattice of nylon are suppressed, it is suppressed into the little lattice of the display unit with limited microchannel, so just avoid the migration of electrophoresis liquid between little lattice, can eliminate the shortcoming of the reunion and the image attenuation of large tracts of land charged corpuscle, also solved the problem that surface tension is big, can is difficult of single micro unit simultaneously.
After compacting is finished, take out the little lattice piece of nylon, clean, dry, adopt the shape of the little lattice of observation by light microscope nylon, with microphotograph analysis hot compression deformation effect with a little tetrachloroethylene solvent.
The key technical indexes of electrophoretic display device, EDD is contrast, response time and the serviceable life etc. of device.The agglomeration of electrophoresis particle is a key influence factor.It is the main method that solves particle aggregation that electrophoresis particle is enclosed in the single small display unit, and microcapsules and little glass of technology are most popular now two kinds of methods with the display unit microminiaturization.
The 3rd step: the making of little glass of type electrophoresis prototype display device
(1) the heelpiece electrode preparation is chosen the little lattice sheet of nylon of preparation, determines little lattice piece of 3.5 * 3.5cm.((middle of 6 * 6cm) conducting surface evenly is coated with the poly-vinyl alcohol solution that last layer thickness is about 13 μ m to 3.5 * 3.5cm) ITO electro-conductive glass making display pattern or pattern-free, the little lattice of the nylon of above-mentioned preparation are sticking thereon, and making it bonding plain with suitable pressure, oven dry 10min are stand-by down at 30～40 ℃.
Select else with the thick mylar of 100 μ m, cut out the square of 5 * 5cm size, the adopting process icking tool is made the demonstration chamber of size a 3.5 * 3.5cm in its middle.Then this is had the mylar that shows the chamber and stick on the above-mentioned ito glass that pastes the little lattice of nylon, and make and show that the chamber just in time comprises the little lattice of nylon and coincide with epoxy resin.So just made hearth electrode.
(2) preparation of display device coating thickness on the mylar in the demonstration of the formation on the hearth electrode that above-mentioned steps is made chamber is the epoxy resin of 3 μ m, get the ITO electro-conductive glass of another sheet 6 * 6cm, make the one side along boning along the back of aliging with a side of the mylar that scribbles epoxy resin.The osculum that will stay about 1mm during making on one side of mylar as inlet so that can.
Draw the electrophoresis disclosing solution for preparing with micro syringe, enter,, influence the attractive in appearance and color developing (, need slowly drive out of, and then carry out can) of device if bubble is arranged in case bubble enters from the even can of inlet.After treating that device is filled, with the bonding edge of adhesive (epoxy resin) and inlet to play the effect of air locking.
Draw the electrophoresis disclosing solution for preparing with micro syringe, enter,, influence the attractive in appearance and color developing (, need slowly drive out of, and then carry out can) of device if bubble is arranged in case bubble enters from the even can of inlet.After treating that device is filled, with the bonding edge of adhesive (epoxy resin) and inlet to play the effect of air locking.
Embodiment 7 (little glass of type electrophoretic display device, EDD)
The first step: the preparation of show electrode
For making pattern or the numeral that device demonstrates to be needed, at first on the ito glass of conduction, etch the literal or the pattern of required demonstration.Chemical method etching conductive glass is adopted in this experiment, and flow process is divided into following two parts:
(1) display pattern scribes
Getting a block size is the glass electrode that is coated with the electroconductive ITO layer of 6 * 6cm, cleans its surface to keep clean and tidy with clear water, dries 30min down for 50 ℃ in baking oven.Dip in a little acetone or alcohol with dustless cloth (multiselect silk class) and clean the ITO conductive layer, after drying up fast with hair-dryer, conductive layer is lain on the dustless desktop up.
Select for use the adhesive tape about thickness 0.5mm entirely to be layered on the ITO conductive layer, it is protected, flatten compacting,, cause leaking erosion easily in the etching process and spot occurs in case bubble enters.(3.5 * 3.5cm) place under the electro-conductive glass, and justified margin is fixing will to be printed on pattern model on the paper then.With Steel Ruler and technology icking tool, pattern is scribed.After pattern has been scribed, dip in a little acetone or alcohol with dustless cloth (multiselect silk class) and clean the pattern of scribing, do not have remaining adhesive tape to guarantee the ITO laminar surface that need etch away pattern model.Repair cutter with technology pattern edge is modified, guarantee the clean and tidy neat of edge.
(2) the chemical etching technology of display pattern
The preparation of etching liquid: measure distilled water and concentrated hydrochloric acid that quality is 70.0g, the solid ferric trichloride of 14.0g joins in the 500mL beaker successively, ultrasonic agitation on ultrasonic instrument, and dissolving is evenly.
The electro-conductive glass of scribing good pattern is lain against in the double dish, and conducting surface is poured chemical etching liquid into up, and a little gets final product to soak the electro-conductive glass upper surface.Behind 40 ℃ of etching 11min, take out with tweezers and to place 5%～10% sodium hydrate aqueous solution with the surperficial acid solution that neutralizes, take out and use a large amount of distilled water flushings, afterwards with a little acetone or alcohol drip washing, place 50 ℃ of drying in oven then.
The adhesive tape of protection usefulness is taken off, cleaned conductive layer surface, can obtain having the conductive electrode of pattern, in order to making the usefulness of device with ethanol.
Second step: little glass making
Selecting diameter for use is that the solid copper facing bloom of 70mm is a compacting tool set, polished surface vis-a-vis, a little silicone oil of coating on the polished surface (preventing the adhesion of nylon wire and mould in pressing process), the big or small nylon wire piece identical with mould of cutting area places in the middle of the mould.Then mould is placed on the hydropress, at room temperature under 6.50Mpa pressure, suppress 10min.
Select for use the little lattice of outsourcing nylon as little glass of base material, little lattice specification is long 180 μ m, wide 130 μ m, high 70 μ m.Between the little lattice of nylon is intercommunication, electrophoresis particle can move between little lattice, agglomeration still exists, adopt pressure sintering that the little lattice of nylon are suppressed, it is suppressed into the little lattice of the display unit with limited microchannel, so just avoid the migration of electrophoresis liquid between little lattice, can eliminate the shortcoming of the reunion and the image attenuation of large tracts of land charged corpuscle, also solved the problem that surface tension is big, can is difficult of single micro unit simultaneously.
After compacting is finished, take out the little lattice piece of nylon, clean, dry, adopt the shape of the little lattice of observation by light microscope nylon, with microphotograph analysis hot compression deformation effect with a little tetrachloroethylene solvent.
The key technical indexes of electrophoretic display device, EDD is contrast, response time and the serviceable life etc. of device.The agglomeration of electrophoresis particle is a key influence factor.It is the main method that solves particle aggregation that electrophoresis particle is enclosed in the single small display unit, and microcapsules and little glass of technology are most popular now two kinds of methods with the display unit microminiaturization.
The 3rd step: the making of little glass of type electrophoresis prototype display device
(1) the heelpiece electrode preparation is chosen the little lattice sheet of nylon of preparation, determines little lattice piece of 3.5 * 3.5cm.((middle of 6 * 6cm) conducting surface evenly is coated with the poly-vinyl alcohol solution that last layer thickness is about 15 μ m to 3.5 * 3.5cm) ITO electro-conductive glass making display pattern or pattern-free, the little lattice of the nylon of above-mentioned preparation are sticking thereon, and making it bonding plain with suitable pressure, oven dry 10min are stand-by down at 30～40 ℃.
Select else with the thick mylar of 100 μ m, cut out the square of 5 * 5cm size, the adopting process icking tool is made the demonstration chamber of size a 3.5 * 3.5cm in its middle.Then this is had the mylar that shows the chamber and stick on the above-mentioned ito glass that pastes the little lattice of nylon, and make and show that the chamber just in time comprises the little lattice of nylon and coincide with epoxy resin.So just made hearth electrode.
(2) preparation of display device coating thickness on the mylar in the demonstration of the formation on the hearth electrode that above-mentioned steps is made chamber is the epoxy resin of 5 μ m, get the ITO electro-conductive glass of another sheet 6 * 6cm, make the one side along boning along the back of aliging with a side of the mylar that scribbles epoxy resin.The osculum that will stay about 1mm during making on one side of mylar as inlet so that can.
Draw the electrophoresis disclosing solution for preparing with micro syringe, enter,, influence the attractive in appearance and color developing (, need slowly drive out of, and then carry out can) of device if bubble is arranged in case bubble enters from the even can of inlet.After treating that device is filled, with the bonding edge of adhesive (epoxy resin) and inlet to play the effect of air locking.
Embodiment 8 (little glass of type electrophoretic display device, EDD)
At white black track producing particle mass ratio is that 15: 1 and electric field intensity are under the 0.02V/ μ m condition, and the electrophoresis disclosing solution of studying different particle concentrations shows the influence of contrast.
Fig. 5 is for showing the change curve of contrast with particle concentration.Along with the increase of particle concentration, device shows that contrast presents elder generation and improves the trend that afterwards reduces, and particle concentration shows that at 10% o'clock contrast reaches maximal value 15.60.This is that the athletic meeting of particle in dispersion liquid is subjected to certain obstruction because particle concentration is when increasing, and electrophoretic property descends, and makes the whiteness value that shows descend to some extent, and blackness value rises to some extent, so show contrast decline.Therefore should select suitable particle concentration, particle concentration is best near 10%.
Embodiment 9 (little lattice type electrophoretic display device, EDD performance evaluation)
Overall particle concentration be 10% and electric field intensity be under the condition of 0.02V/ μ m, the different electrophoresis disclosing solutions white, the black track producing particle mass ratio of research show the influence of contrast.
Fig. 6 is for showing the change curve of contrast with white black track producing particle mass ratio.Along with increase white, the black track producing particle mass ratio, device shows that contrast presents and improves the trend that afterwards reduces earlier, and is 10: 1～15: 1 o'clock at the particle ratio, and the demonstration contrast reaches higher value 15.60～15.70.So selection is white, the black track producing particle mass ratio was best near 10: 1 or 15: 1.
Embodiment 10 (little lattice type electrophoretic display device, EDD performance evaluation)
Under 10% particle concentration, 10: 1 the condition of white black track producing particle mass ratio, study different electric field intensity and drive the influence that electric inks show contrasts.
Fig. 7 is for showing the change curve of contrast with electric field intensity.Along with the increase of electric field intensity, device shows that contrast increases gradually, when electric field intensity is 0.02V/ μ m, shows that contrast reaches maximal value 15.65, continues to increase electric field intensity, shows that contrast then descends.Therefore electric field intensity is best near 0.02V/ μ m.
Embodiment 11 (little lattice type electrophoretic display device, EDD performance evaluation)
Be about 10% in overall particle concentration, white black track producing particle mass ratio is that 10: 1 and electric field intensity are under the condition of 0.02V/ μ m, the electric ink of studying different macromolecule resin concentration is prepared into the influence of the demonstration contrast of electrophoretic display device, EDD.
Fig. 8 is for showing the change curve of contrast with resin concentration.Earlier increase the trend that afterwards reduces along with the increase device of macromolecule resin concentration shows that contrast presents, near 2.5%, reach maximal value 15.50.Macromolecule resin plays function of stabilizer in dispersion liquid, can control the electrophoresis behavior of electrophoresis particle well, makes more tending towards stability of its motion.But, when resin concentration is excessive, can influence the movement velocity of electrophoresis particle again, thereby influence the response time of device, therefore the size of resin concentration should be controlled at 1.0～3.0% in dispersion liquid, is best at 1.5～2.5% o'clock.
Embodiment 12 (little lattice type electrophoretic display device, EDD performance evaluation)
The overall particle concentration of electrophoresis liquid is 10%, and white black track producing particle mass ratio is 10: 1, and the macromolecule resin stabilizer concentration is 2.5%, and driving electric field intensity is 0.02V/ μ m.With this understanding, adopting interelectrode distance is that 100 μ m prepare electrophoresis prototype display device, the research color developing effect.
Fig. 9, Figure 10 are respectively the black and white character pattern display photos that electric field intensity is 0.02V/ μ m, seven sections black and white digital pattern display photos.Display pattern is clear among the figure, the profile lines are level and smooth, shows that contrast can reach 15.60.
Clearly, those of ordinary skill in the art can be on the basis that does not deviate from spirit and scope of the invention makes modifications and variations in to the present invention.Therefore, this invention is intended to cover the of the present invention various modifications and variations that fall in appended claims of the present invention and the equivalent scope thereof.
Claims (3)
1. electrophoresis showed liquid and preparation method thereof, it is characterized in that: in the ball milling bottle, add zellon 5～50mL, 0.1 charge control agent polyisobutylene mono butonediimide series, 0.1～0.5g spreading agent sorbitan trioleate series and the hyper-dispersant Solspersl7000 of～1.0g, 0.1～1.0g macromolecule resin stabilizing agent phenolics, acrylate or polyisobutylene, 3.0～6.0g particle diameter is the hollow TiO of 50～150nm
2, TiO nano particle or carbon black nano particle; With 2mm zirconia zirconium pearl is abrasive media, and ball milling 20～30h under rotating speed 500～800r/min filters suspension with 200 mesh sieve then, and mother liquor is stored in the vial, promptly obtains electrophoresis disclosing solution.
2. electrophoresis showed liquid and preparation method thereof as claimed in claim 1 is characterized in that: TiO
2When particle is white particles, prepare the white particles electrophoresis disclosing solution; When TiO or carbon black particle are black particles, prepare the black particles electrophoresis disclosing solution.
3. electrophoresis showed liquid and preparation method thereof as claimed in claim 1, it is characterized in that: with the black and white single-particle electrophoresis disclosing solution for preparing according to white black track producing particle mass ratio (10～15): 1 ratio mixes and makes the two particle electrophoresises of black and white and show liquid, with ultrasonic instrument ultrasonic dispersion 30min under the condition of 100W, 58KHz, obtain the two particle electrophoresises of finely dispersed black and white and show liquid.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103513488A (en) * | 2012-06-29 | 2014-01-15 | 索尼公司 | Electrophoresis device and display |
| JP2018177858A (en) * | 2017-04-04 | 2018-11-15 | 日本化薬株式会社 | Carbon black-dispersed phenolic resin, epoxy resin composition and method for producing the same |
| CN112180650A (en) * | 2020-09-22 | 2021-01-05 | 深圳秋田微电子股份有限公司 | Color electrophoretic display liquid and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103513488A (en) * | 2012-06-29 | 2014-01-15 | 索尼公司 | Electrophoresis device and display |
| JP2018177858A (en) * | 2017-04-04 | 2018-11-15 | 日本化薬株式会社 | Carbon black-dispersed phenolic resin, epoxy resin composition and method for producing the same |
| CN112180650A (en) * | 2020-09-22 | 2021-01-05 | 深圳秋田微电子股份有限公司 | Color electrophoretic display liquid and preparation method thereof |
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