CN102213888B - Preparation method of electrophoretic display solution - Google Patents
Preparation method of electrophoretic display solution Download PDFInfo
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- CN102213888B CN102213888B CN 201110088392 CN201110088392A CN102213888B CN 102213888 B CN102213888 B CN 102213888B CN 201110088392 CN201110088392 CN 201110088392 CN 201110088392 A CN201110088392 A CN 201110088392A CN 102213888 B CN102213888 B CN 102213888B
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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 the development of computer technology and popularizing of 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-size.With respect to traditional paper, the electrophoretic display device (EPD) cost is slightly high, but can combine closely with the digital information technology, can circulate repeatedly and to use, production run does not need to consume large 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) consists of by two relative electrodes 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 to show data or image.Electrophoretic display device, EDD continues to show data and does not consume extra power, unless it receives the electric signal 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, namely photetching is scribed glass technique and high-speed full-automatic cup technique processed, and is all higher to the requirement of instrument and equipment, and filling and sealing is comparatively complicated.Photetching is scribed a glass technique: be coated with substrate coating one deck radiation curing material 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 curing, then with the solvent of solubilized radiation curing material will be uncured radiation curing material remove the little cup structure of formation.High-speed full-automatic cup technique processed: be coated with transparency carrier coating one deck thermosetting substance of conductive film, then on the Glass transition temperature of thermosetting substance, with a punch it is carried out rolling pressing die cup processed, solidify finally by modes such as cooling or illumination.
Little glass the fluid-tight packing technique that enters has two kinds of one-part form and two-period forms.It is first the encapsulated layer material to be scattered in the electrophoresis liquid in advance that one-part form enters the fluid-tight packing technique, and layering is floating to the surface rapidly after electrophoresis liquid is filled, and final curing becomes encapsulating film.It is first electrophoresis liquid to be injected little cup that two-period form enters the fluid-tight packing technique, the encapsulated layer material is coated on the electrophoresis liquid again, and then the encapsulated layer material is through solidifying to form encapsulating film.
The development of electrophoretic display technology is in the eve of industrialization in the international coverage, although each major company releases state-of-the-art technology and new product frequently, but still is laboratory sample, not yet enters large-scale production.Trace it to its cause, except the 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 simultaneously electrophoretic display device, EDD 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 the limitation of prior art and one or more problems that shortcoming produces.
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 the charge control agent polyisobutylene mono butonediimide of～1.0g is serial, 0.1～0.5g spreading agent sorbitan trioleate 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; Take 2mm zirconia zirconium pearl as abrasive media, then ball milling 20～30h under rotating speed 500～800r/min filters suspension with 200 mesh sieve, and mother liquor is stored in the vial, namely 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 for providing a 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 for explaining together with the description principle of the present invention.
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 nylon photo;
Fig. 4 is the contrast black-and-white display photo of the little lattice of nylon;
Fig. 5 is that the display comparison degree is with the change curve of particle concentration;
Fig. 6 is that the display comparison degree is with the change curve of white black track producing particle mass ratio;
Fig. 7 is that the display comparison degree is with the change curve of electric field intensity;
Fig. 6 is that the display comparison degree is with the change curve of resin concentration;
Fig. 9 is that electric field intensity is 0.02V/ μ m, and the black and white character pattern shows photo;
Figure 10 is that electric field intensity is 0.02V/ μ m, and seven sections black and white digital patterns show photo.
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 to etch at the ito glass of conduction 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, 40 ℃～60 ℃ lower oven dry 30min in baking oven with clear water.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 the adhesive tape about thickness 0.5mm entirely to be layered on the ITO conductive layer, it is protected, flatten compacting, enter with Anti-bubble, cause leaking erosion easily in the etching process and spot occurs.Then (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.With Steel Ruler and technique 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, to guarantee to etch away the ITO layer surface of pattern model without remaining adhesive tape.Repair cutter with technique pattern edge is modified, guarantee the clean and tidy neat of edge.
(2) the chemical etching technique 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, to take out and use a large amount of distilled water flushings, then a little the acetone or alcohol drip washing of rear usefulness place 50 ℃ of drying in oven.
The adhesive tape of protection usefulness is taken off, cleaned conductive layer surface with ethanol, can obtain being with figuratum conductive electrode, in order to making the usefulness of device.Fig. 2 is the etching effect picture.
Second step: the making of little cup (the little lattice of nylon)
Selecting diameter is that the solid copper facing bloom of 70mm is compacting tool set, polished surface vis-a-vis, a little silicone oil of polished surface coating (preventing the adhesion of nylon wire and mould in pressing process), the nylon wire piece that the cutting size is identical with mould 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 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.Intercommunication between the little lattice of nylon, 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 avoided the migration of electrophoresis liquid between little lattice, can eliminate the shortcoming of reunion and the image attenuation of large tracts of land charged corpuscle, large, the can hard problem of the surface tension that has also solved single micro unit simultaneously.
After compacting is finished, take out the little lattice piece of nylon, clean with a little tetrachloroethylene solvent, dry, adopt the shape of the little lattice of observation by light microscope nylon, with microphotograph analysis hot compression deformation effect.
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 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 two kinds of methods with the display unit microminiaturization now.
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 larger distortion, a plocoid spot appears in the cross-point of co-ordination, has played the effect that little lattice is divided into complete independent display 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 of～1.0g series (T151, T152), 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; Take 2mm zirconia zirconium pearl as abrasive media, then ball milling 20～30h under rotating speed 500～800r/min filters suspension with 200 mesh sieve, and mother liquor is stored in the vial, namely obtains electrophoresis disclosing solution.
(1) the little lattice sheet of nylon of preparation is chosen in the preparation of heelpiece electrode, determines little lattice piece of 3.5 * 3.5cm.((poly-vinyl alcohol solution that a layer thickness is about 10～15 μ m is evenly coated in the middle of 6 * 6cm) conducting surface 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 make it bonding plain with suitable pressure, stand-by at 30～40 ℃ of lower oven dry 10min.
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 will be somebody's turn to do with the mylar that shows the chamber and stick on the above-mentioned ito glass that pastes the little lattice of nylon with epoxy resin, and make and show that the chamber just in time comprises the little lattice of nylon and coincide.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 aliging rear bonding well with the side edge of the mylar that scribbles epoxy resin.The osculum that will stay on one side of mylar about 1mm during making as inlet so that can.
Draw the electrophoresis disclosing solution for preparing with micro syringe, enter from the even can of inlet, enter with Anti-bubble, affect the attractive in appearance and color developing (if bubble is arranged, need slowly drive out of, and then carry out can) of device.After 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, then builds the bread board circuit according to circuit theory, 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 displaying 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 the preparation of device, test at the voltage stabilizing electrophoresis apparatus, 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.Be 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 at pressure, contrast can reach 15: 1.
The selection of device detection condition
The display comparison degree of device detection is the ratio of white reflection rate and black reflectivity, and the white reflection rate is larger, and relative contrast also can be larger.The concentration of overall particle concentration, white black track producing particle mass ratio, electric field intensity, stabilizing agent macromolecule resin is on the highly significant that affects of display comparison degree, so the display effect that the display comparison degree is estimated 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; Take 2mm zirconia zirconium pearl as abrasive media, then ball milling 20h under rotating speed 500r/min filters suspension with 200 mesh sieve, and mother liquor is stored in the vial, namely 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; Take 2mm zirconia zirconium pearl as abrasive media, then ball milling 25h under rotating speed 700r/min filters suspension with 200 mesh sieve, and mother liquor is stored in the vial, namely 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; Take 2mm zirconia zirconium pearl as abrasive media, then ball milling 30h under rotating speed 800r/min filters suspension with 200 mesh sieve, and mother liquor is stored in the vial, namely 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, 50 ℃ of lower oven dry 30min in baking oven with clear water.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 the adhesive tape about thickness 0.5mm entirely to be layered on the ITO conductive layer, it is protected, flatten compacting, enter with Anti-bubble, cause leaking erosion easily in the etching process and spot occurs.Then (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.With Steel Ruler and technique 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, to guarantee to etch away the ITO layer surface of pattern model without remaining adhesive tape.Repair cutter with technique pattern edge is modified, guarantee the clean and tidy neat of edge.
(2) the chemical etching technique 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, to take out and use a large amount of distilled water flushings, then a little the acetone or alcohol drip washing of rear usefulness place 50 ℃ of drying in oven.
The adhesive tape of protection usefulness is taken off, cleaned conductive layer surface with ethanol, can obtain being with figuratum conductive electrode, in order to making the usefulness of device.
Second step: little glass making
Selecting diameter is that the solid copper facing bloom of 70mm is compacting tool set, polished surface vis-a-vis, a little silicone oil of polished surface coating (preventing the adhesion of nylon wire and mould in pressing process), the nylon wire piece that the cutting size is identical with mould places in the middle of the mould.Then mould is placed on the hydropress, at room temperature under 0Mpa pressure, suppress 10min.
Select 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.Intercommunication between the little lattice of nylon, 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 avoided the migration of electrophoresis liquid between little lattice, can eliminate the shortcoming of reunion and the image attenuation of large tracts of land charged corpuscle, large, the can hard problem of the surface tension that has also solved single micro unit simultaneously.
After compacting is finished, take out the little lattice piece of nylon, clean with a little tetrachloroethylene solvent, dry, adopt the shape of the little lattice of observation by light microscope nylon, with microphotograph analysis hot compression deformation effect.
The 3rd step: the making of little glass of type electrophoresis prototype display device
(1) the little lattice sheet of nylon of preparation is chosen in the preparation of heelpiece electrode, determines little lattice piece of 3.5 * 3.5cm.((poly-vinyl alcohol solution that a layer thickness is about 10 μ m is evenly coated in the middle of 6 * 6cm) conducting surface 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 make it bonding plain with suitable pressure, stand-by at 30～40 ℃ of lower oven dry 10min.
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 will be somebody's turn to do with the mylar that shows the chamber and stick on the above-mentioned ito glass that pastes the little lattice of nylon with epoxy resin, and make and show that the chamber just in time comprises the little lattice of nylon and coincide.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 aliging rear bonding well with the side edge of the mylar that scribbles epoxy resin.The osculum that will stay on one side of mylar about 1mm during making as inlet so that can.
Draw the electrophoresis disclosing solution for preparing with micro syringe, enter from the even can of inlet, enter with Anti-bubble, affect the attractive in appearance and color developing (if bubble is arranged, need slowly drive out of, and then carry out can) of device.After 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, then builds the bread board circuit according to circuit theory, 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 displaying 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, 50 ℃ of lower oven dry 30min in baking oven with clear water.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 the adhesive tape about thickness 0.5mm entirely to be layered on the ITO conductive layer, it is protected, flatten compacting, enter with Anti-bubble, cause leaking erosion easily in the etching process and spot occurs.Then (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.With Steel Ruler and technique 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, to guarantee to etch away the ITO layer surface of pattern model without remaining adhesive tape.Repair cutter with technique pattern edge is modified, guarantee the clean and tidy neat of edge.
(2) the chemical etching technique 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, to take out and use a large amount of distilled water flushings, then a little the acetone or alcohol drip washing of rear usefulness place 50 ℃ of drying in oven.
The adhesive tape of protection usefulness is taken off, cleaned conductive layer surface with ethanol, can obtain being with figuratum conductive electrode, in order to making the usefulness of device.
Second step: little glass making
Selecting diameter is that the solid copper facing bloom of 70mm is compacting tool set, polished surface vis-a-vis, a little silicone oil of polished surface coating (preventing the adhesion of nylon wire and mould in pressing process), the nylon wire piece that the cutting size is identical with mould places in the middle of the mould.Then mould is placed on the hydropress, at room temperature under 3.20Mpa pressure, suppress 10min.
Select 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.Intercommunication between the little lattice of nylon, 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 avoided the migration of electrophoresis liquid between little lattice, can eliminate the shortcoming of reunion and the image attenuation of large tracts of land charged corpuscle, large, the can hard problem of the surface tension that has also solved single micro unit simultaneously.
After compacting is finished, take out the little lattice piece of nylon, clean with a little tetrachloroethylene solvent, dry, adopt the shape of the little lattice of observation by light microscope nylon, with microphotograph analysis hot compression deformation effect.
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 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 two kinds of methods with the display unit microminiaturization now.
The 3rd step: the making of little glass of type electrophoresis prototype display device
(1) the little lattice sheet of nylon of preparation is chosen in the preparation of heelpiece electrode, determines little lattice piece of 3.5 * 3.5cm.((poly-vinyl alcohol solution that a layer thickness is about 13 μ m is evenly coated in the middle of 6 * 6cm) conducting surface 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 make it bonding plain with suitable pressure, stand-by at 30～40 ℃ of lower oven dry 10min.
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 will be somebody's turn to do with the mylar that shows the chamber and stick on the above-mentioned ito glass that pastes the little lattice of nylon with epoxy resin, and make and show that the chamber just in time comprises the little lattice of nylon and coincide.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 aliging rear bonding well with the side edge of the mylar that scribbles epoxy resin.The osculum that will stay on one side of mylar about 1mm during making as inlet so that can.
Draw the electrophoresis disclosing solution for preparing with micro syringe, enter from the even can of inlet, enter with Anti-bubble, affect the attractive in appearance and color developing (if bubble is arranged, need slowly drive out of, and then carry out can) of device.After 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 from the even can of inlet, enter with Anti-bubble, affect the attractive in appearance and color developing (if bubble is arranged, need slowly drive out of, and then carry out can) of device.After 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 to etch at the ito glass of conduction 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, 50 ℃ of lower oven dry 30min in baking oven with clear water.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 the adhesive tape about thickness 0.5mm entirely to be layered on the ITO conductive layer, it is protected, flatten compacting, enter with Anti-bubble, cause leaking erosion easily in the etching process and spot occurs.Then (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.With Steel Ruler and technique 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, to guarantee to etch away the ITO layer surface of pattern model without remaining adhesive tape.Repair cutter with technique pattern edge is modified, guarantee the clean and tidy neat of edge.
(2) the chemical etching technique 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, to take out and use a large amount of distilled water flushings, then a little the acetone or alcohol drip washing of rear usefulness place 50 ℃ of drying in oven.
The adhesive tape of protection usefulness is taken off, cleaned conductive layer surface with ethanol, can obtain being with figuratum conductive electrode, in order to making the usefulness of device.
Second step: little glass making
Selecting diameter is that the solid copper facing bloom of 70mm is compacting tool set, polished surface vis-a-vis, a little silicone oil of polished surface coating (preventing the adhesion of nylon wire and mould in pressing process), the nylon wire piece that the cutting size is identical with mould places in the middle of the mould.Then mould is placed on the hydropress, at room temperature under 6.50Mpa pressure, suppress 10min.
Select 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.Intercommunication between the little lattice of nylon, 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 avoided the migration of electrophoresis liquid between little lattice, can eliminate the shortcoming of reunion and the image attenuation of large tracts of land charged corpuscle, large, the can hard problem of the surface tension that has also solved single micro unit simultaneously.
After compacting is finished, take out the little lattice piece of nylon, clean with a little tetrachloroethylene solvent, dry, adopt the shape of the little lattice of observation by light microscope nylon, with microphotograph analysis hot compression deformation effect.
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 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 two kinds of methods with the display unit microminiaturization now.
The 3rd step: the making of little glass of type electrophoresis prototype display device
(1) the little lattice sheet of nylon of preparation is chosen in the preparation of heelpiece electrode, determines little lattice piece of 3.5 * 3.5cm.((poly-vinyl alcohol solution that a layer thickness is about 15 μ m is evenly coated in the middle of 6 * 6cm) conducting surface 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 make it bonding plain with suitable pressure, stand-by at 30～40 ℃ of lower oven dry 10min.
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 will be somebody's turn to do with the mylar that shows the chamber and stick on the above-mentioned ito glass that pastes the little lattice of nylon with epoxy resin, and make and show that the chamber just in time comprises the little lattice of nylon and coincide.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 aliging rear bonding well with the side edge of the mylar that scribbles epoxy resin.The osculum that will stay on one side of mylar about 1mm during making as inlet so that can.
Draw the electrophoresis disclosing solution for preparing with micro syringe, enter from the even can of inlet, enter with Anti-bubble, affect the attractive in appearance and color developing (if bubble is arranged, need slowly drive out of, and then carry out can) of device.After 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)
Be that 15: 1 and electric field intensity are under the 0.02V/ μ m condition at white black track producing particle mass ratio, study the impact of the electrophoresis disclosing solution display comparison degree of different particle concentrations.
Fig. 5 is that the display comparison degree is with the change curve of particle concentration.Along with the increase of particle concentration, device display comparison degree presents and improves first the trend that reduces afterwards, and particle concentration is 10% the time, and the display comparison degree reaches maximal value 15.60.This is that the athletic meeting of particle in dispersion liquid is subject to certain obstruction because particle concentration is when increasing, and electrophoretic property descends, so that the whiteness value that shows descends to some extent, blackness value rises to some extent, so the display comparison degree descends.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 impact of the electrophoresis disclosing solution display comparison degree of different white, the black track producing particle mass ratioes of research.
Fig. 6 is that the display comparison degree is with the change curve of white black track producing particle mass ratio.Along with increase white, the black track producing particle mass ratio, device display comparison degree presents and improves first the trend that reduces afterwards, and is 10: 1～15: 1 o'clock at the particle ratio, and the display comparison degree 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 the impact that different electric field intensity drive electric ink display comparison degree.
Fig. 7 is that the display comparison degree is with the change curve of electric field intensity.Along with the increase of electric field intensity, device display comparison degree increases gradually, and when electric field intensity was 0.02V/ μ m, the display comparison degree reached maximal value 15.65, and continuing increases electric field intensity, and the display comparison degree 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 impact of the display comparison degree of electrophoretic display device, EDD.
Fig. 8 is that the display comparison degree is with the change curve of resin concentration.Along with the increase device display comparison degree of macromolecule resin concentration presents the trend of first increases and then decreases, near 2.5%, reach maximal value 15.50.Macromolecule resin plays stabilizing agent in dispersion liquid, can control well the electrophoresis behavior of electrophoresis particle, makes more tending towards stability of its motion.But, when resin concentration is excessive, can affect the movement velocity of electrophoresis particle again, thereby affect the response time of device, therefore the size of resin concentration should be controlled at 1.0～3.0% in dispersion liquid, be the best 1.5～2.5% the time.
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.
It is that the black and white character pattern demonstration photo of 0.02V/ μ m, seven sections black and white digital patterns show photos that Fig. 9, Figure 10 are respectively electric field intensity.Display pattern is clear among the figure, lines of outline is level and smooth, and the display comparison degree 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 the charge control agent polyisobutylene mono butonediimide of～1.0g is serial, 0.1～0.5g spreading agent sorbitan trioleate series and hyper-dispersant Solspers17000,0.1～1.0g macromolecule resin stabilizing agent phenolics, polyisobutylene or stabilizing agent acrylate, 3.0～6.0g particle diameter is the hollow TiO of 50～150nm
2, TiO nano particle or carbon black nano particle; Take 2mm zirconia zirconium pearl as abrasive media, then ball milling 20～30h under rotating speed 500～800r/min filters suspension with 200 mesh sieve, and mother liquor is stored in the vial, namely 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: the black and white single-particle electrophoresis disclosing solution for preparing is mixed according to the ratio of white black track producing particle mass ratio 10:1～15:1 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.
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