CN103360794B - Method for preparing mesoporous oxide hollow particles and liquid crystal display containing mesoporous oxide hollow particles - Google Patents
Method for preparing mesoporous oxide hollow particles and liquid crystal display containing mesoporous oxide hollow particles Download PDFInfo
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- CN103360794B CN103360794B CN201210087645.4A CN201210087645A CN103360794B CN 103360794 B CN103360794 B CN 103360794B CN 201210087645 A CN201210087645 A CN 201210087645A CN 103360794 B CN103360794 B CN 103360794B
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- Liquid Crystal (AREA)
- Liquid Crystal Substances (AREA)
Abstract
The invention discloses a method for preparing mesoporous oxide hollow particles and a liquid crystal display containing the mesoporous oxide hollow particles. The liquid crystal display comprises a first substrate, a second substrate and a liquid crystal composition which is formed between the first substrate and the second substrate, wherein the liquid crystal composition comprises a liquid crystal molecule and a mesoporous oxide hollow particle. The mesoporous oxide hollow particle provided by the invention is easy to prepare and high in stability because the particle cannot be modified due to the light influence, so that the service life of the display can be prolonged.
Description
Technical field
The present invention relates to a kind of Hole oxide hollow granule (mesoporous oxide hollowparticle), and relate to a kind of liquid crystal display especially and comprise Hole oxide hollow granule.
Background technology
Polymer-dispersed liquid crystal (polymer-dispersed liquid crystal, PDLC) main being scattered in organic polymer by micron-sized liquid crystal molecule is formed, wherein the refraction coefficient of liquid crystal molecule does not mate with the refraction coefficient of organic polymer, therefore, without under electric field action, light can be presented opaque shape by liquid crystal molecule scattering, and the refraction coefficient of liquid crystal molecule can be made under electric field action to mate with the refraction coefficient of polymkeric substance, thus presents pellucidity.
Because PDLC does not need light polarizing film and alignment film, therefore can be applicable to make on large-sized liquid crystal display, advertisement plate (banner) or electronics curtain (smart window).
The method for making of polymer-dispersed liquid crystal (polymer-dispersed liquid crystal, PDLC) comprises (1) polymerization phase separation method (polymerization induced phase separation); (2) temperature phase separation method (temperature induced phase separation); (3) solvent phase separation method (solvent induced phaseseparation); (4) method such as microcapsules partition method (microencapsulation), first three methods first makes liquid crystal molecule and polymeric material produce to be separated, then liquid crystal is present in polymkeric substance.4th kind of method first makes liquid crystal mix with monomer, adds coupling agent (binder) afterwards and makes monomer polymerization, and liquid crystal molecule is confined in polymkeric substance to form liquid crystal capsule.
But, under PDLC may be exposed to sunlight for a long time, make polymkeric substance apt to deteriorate and damage, and the method step making PDLC is traditionally complicated.
Summary of the invention
In order to solve the problem, the present invention proposes a kind of liquid crystal display of adding Hole oxide hollow granule and making it above-mentioned.
The invention provides a kind of method for making of Hole oxide hollow granule, comprise the following steps: (a) mixes a template, an interfacial agent and a solvent to form a mixed solution, is formed on the surface of this template to make this interfacial agent; B () adds an inorganic particulate in this mixed solution, and carry out a sol gel reaction (sol-gel reaction), to form an inorganic oxide with nucleocapsid structure (core-shell); C () removes this template and this interfacial agent, to form this Hole oxide hollow granule.
The present invention separately provides a kind of liquid crystal display, comprising: a first substrate; One second substrate; And a liquid-crystal composition, be formed between this first substrate and this second substrate, wherein this liquid-crystal composition comprises a liquid crystal molecule and a Hole oxide hollow granule (mesoporous oxide hollow particle).
Hole oxide hollow-particle provided by the present invention, its preparation is easy, and its stability high (can not go bad by illumination effect), the serviceable life of display can be improved.
Accompanying drawing explanation
Accompanying drawing described herein is used to provide a further understanding of the present invention, forms a application's part, does not form limitation of the invention.In the accompanying drawings:
Fig. 1 is a sectional view, in order to liquid crystal display of the present invention to be described.
Fig. 2 is a transmission electron microscope (Transmission electron microscopy, TEM) figure, in order to the structure of Hole oxide hollow granule of the present invention to be described.
Fig. 3 is the graph of a relation of applying voltage (applied voltage) corresponding penetrance (transmittance, %), in order to the penetrance of liquid crystal display to visible ray under different applying voltage to be described.
Drawing reference numeral:
100 ~ liquid crystal display
102 ~ first substrate
202 ~ second substrate
150 ~ liquid-crystal composition
152 ~ liquid crystal molecule
154 ~ Hole oxide hollow granule
Embodiment
For above and other object of the present invention, feature and advantage can be become apparent, cited below particularly go out preferred embodiment, and coordinate institute's accompanying drawings, be described in detail below.
The invention provides a kind of method for making of Hole oxide hollow granule, comprise the following steps (a)-(c).First, carry out step (a), hybrid template, interfacial agent and solvent, to form mixed solution, are formed on the surface of template to make interfacial agent.
Above-mentioned template comprises polymethylmethacrylate (Polymethylmethacrylate, PMMA), polystyrene (polystyrene, PS), or other macromolecule spheroids all can.The particle size of template is about 100nm-2000nm, is preferably about 300-700nm, and the size of template can determine the size of the Hole oxide hollow granule of follow-up formation.
Above-mentioned interfacial agent comprises gelatin (gelatin), segmented copolymer (block polymer), long chain type interfacial agent or above-mentioned combination.Segmented copolymer comprises polyethoxy-poly-propoxy block copolymer (polyoxyethylene-polyoxyoropylene block polymer) or polyglycol (PolyethyleneGlycols, PEG), wherein polyethoxy-poly-propoxy block copolymer such as poloxamer 403 (P123), poloxamer 407 (F127), poloxamer 402 (L122), poloxamer 181 (L61), poloxamer401 (L121), poloxamer 185 (P65), PE64 or poloxamer 338 (F108).
Long-chain interfacial agent comprises C
8-20the anionic interfacial agent of alkyl, C
8-20the cationic interfacial agent of alkyl or above-mentioned combination.C
8-20the anionic interfacial agent such as SDS (sodium dodecyl sulfate, SDS) or ten hexichol alkyl sulfonic acid sodium (sodiumdodecylbenzene sulfonate, SDBS) of alkyl.C
8-20cationic interfacial agent such as cetyl trimethyl ammonium bromide (the cetyl trimethylammonium bromide of alkyl, CTMAB), DTAB (dodecyl trimethyl ammonium bromide, DTMAB), hexadecyltrimethylammonium chloride (cetyl trimethylammonium chloride, CTMAB), Cetyltrimethylammonium bromide (octadecyl trimethylammonium bromide, or OTAC (octadecyl trimethylammonium chloride OTMAB), OTMAC).
Above-mentioned solvent comprises water, ethanol, isopropyl alcohol, propyl alcohol, acetone, toluene (toluene), trimethylbenzene (1,3,5-trimethylbenzene), other polarity or non-polar solvent or above-mentioned combination.The selection of solvent is different along with the difference of used interfacial agent, is not limited to the above-mentioned solvent mentioned, as long as the solvent that interfacial agent can be dissolved, all in the scope that the present invention protects.
Afterwards, carry out step (b), add inorganic particulate in mixed solution, and carry out sol gel reaction (sol-gel reaction), to form the inorganic oxide with nucleocapsid structure (core-shell), wherein sol gel reaction is carried out under pH value is the condition of about 4-6.
It is noted that, being added with of interfacial agent helps make inorganic particulate can carry out condensation reaction (condensation reaction) on the surface of template, and then forms the inorganic oxide with nucleocapsid structure (core-shell).In addition, the Mixing ratio by weight example of interfacial agent and inorganic particulate is about 1/10-10/1, is preferably about 1/5-5/1.
Moreover before carrying out step (c), method for making comprises carries out hydro-thermal reaction (hydrothermalreaction) to oxide, and wherein the temperature of hydro-thermal reaction is about 50-100 DEG C, and the time of hydro-thermal reaction is about 1-200 hour.
Hydro-thermal reaction can make crystallization again after oxide dissolution, the inorganic oxide that thus generating structure is comparatively stable, and hydro-thermal reaction is better carries out under acid condition, and the pH value of its hydro-thermal reaction is about 4-6.
Afterwards, carry out step (c), remove template and interfacial agent, to form Hole oxide hollow granule.The method removing template and interfacial agent comprises carries out calcine technology to inorganic oxide.
In one embodiment, calcine technology such as uses high temperature furnace pipe, calcines at 300-800 DEG C to inorganic oxide, to remove template and interfacial agent, to obtain Hole oxide hollow granule.
It is noted that, according to international pure chemistry and applied chemistry alliance (international union of pureand applied chemistry, IUPAC) regulation, according to the hole mean grain size of porous material, porous material is divided into three kinds, the material being greater than about 50nm when aperture is macroscopic void material (macroporous), aperture is Hole material (mesoporous) between the material of 2-50nm, and the material that aperture is less than about 2nm is small holes material (microporous).Therefore, " Hole oxide hollow-particle " alleged by the present invention herein refers to that oxide is Hole material, and its pore size is about 2-50nm.
The Hole oxide hollow granule that method for making of the present invention is formed comprises monox, aluminium oxide, titanium dioxide, zinc paste or other inorganic oxides.
In addition, also surfaction can be carried out, to change the surface nature of Hole oxide hollow granule to Hole oxide hollow granule of the present invention.
In one embodiment, carry out the finishing of monox hollow granule by silane compound, make the silicon oxide surface of water wettability (hydrophilic) become hydrophobicity (hydrophobic).
Moreover the refractive index via the Hole oxide hollow granule of above-mentioned method for making gained is about 1.40-1.50, and its particle size is about 100nm-2000nm, is preferably about 300-700nm.
Learnt by above-mentioned steps, the present invention goes out the Hole oxide hollow sphere of dispersed high (well-dispersed) by solid-state templated synthesis, wherein the large I of oxide hollow sphere adjusts along with the size of template, and the dispersiveness of hollow ball by interfacial agent and inorganic particulate addition and determine.
In addition, refer to Fig. 1, the invention provides a kind of liquid crystal display 100, it comprises first substrate 102; Second substrate 202; And liquid-crystal composition 150 is formed between first substrate 102 and second substrate 202, wherein liquid-crystal composition 150 comprises liquid crystal molecule 152 and Hole oxide hollow granule 154.It should be noted that first substrate 102 and second substrate 202 can be the substrates that thin film transistor base plate, colored filter substrate, transparency carrier or thin film transistor (TFT) are combined with colored filter.
Hole oxide hollow granule 154 is by above-mentioned method for making gained, and its refractive index is about 1.40-1.50, and its particle size is about 100nm-2000nm.
Moreover liquid crystal molecule 152 is 0.01-1 with the weight ratio of Hole oxide hollow granule 154.It is noted that, liquid crystal molecule 152 can enter in Hole oxide hollow granule 154, therefore, contributes to reducing the density variation between Hole oxide hollow-particle and liquid crystal molecule, and improves the dispersiveness (dispersion) of liquid crystal.
Above-mentioned liquid crystal molecule 152 can be nematic (Nematic), stratose type (Smectic) or cholesterol type (Cholesteric) liquid crystal material, MLC6080, BL006 or ZLI4792 that wherein nematic liquid crystalline material is such as commercially available, smectic liquid crystal material such as CS1031.Cholesterol liquid crystal material such as CB-15.It is noted that, except above-mentioned material, as long as the liquid crystal molecule that can produce liquid crystal phase is all in the scope that the present invention protects.
Moreover, due to impressed voltage can be utilized to rotate liquid crystal molecule, make the refractive index of the refractive index of liquid crystal molecule and Hole oxide hollow-particle close, regulate and control the penetrance of display.In addition, by the concentration of adjustment Hole oxide hollow-particle, to adjust the photoelectric characteristic of display, therefore, make display have the advantage of impressed voltage and penetrance linear relationship, and there is the advantage of high penetration or high reflectance.
It is noted that, existing PDLC is because under being exposed to sunlight for a long time, making polymkeric substance apt to deteriorate and damage, and the method step making PDLC is traditionally complicated.And Hole oxide hollow-particle provided by the present invention, its preparation is easy, and its stability high (can not go bad by illumination effect), the serviceable life of display can be improved.
Liquid crystal display provided by the present invention is except can be applicable to penetration display (transmissivedisplay), and future is also potential is applied to reflected displaying device (reflective display) or semi-penetrating trans display (transflective display).
[embodiment]
Embodiment 1 makes Hole monox hollow granule
First, get 0.50 gram of polymethylmethacrylate (Polymethylmethacrylate, PMMA) ball powder (diameter is about 300nm), be dissolved in 50 grams of water, also stir 3 hours again with ultrasonic vibrating after 3 hours, methyl methacrylate (PMMA) is dispersed in water.
Get after 0.15 gram of gelatin (gelatin) (as solid-state template) is dissolved in 30 grams of water, pour in the aqueous solution containing PMMA ball, mixed solution stirs 3 hours with ultrasonic vibrating after 3 hours again.
Then, be that the sodium silicate aqueous solution of 4 is poured in above-mentioned mixed solution by pH, to carry out sol gel reaction (sol-gel reaction), the reaction time is 6 hours.
Afterwards, then through hydro-thermal reaction at 100 DEG C 24 hours, finally under air with 500 DEG C of calcinings 3 hours, to remove gelatin, to obtain Hole monox hollow ball.
Refer to Fig. 2, transmission electron microscope (Transmission electronmicroscopy, the TEM) figure of its display embodiment 1, clear view can to have the structure of hollow ball to monox by figure.
Embodiment 2
The method for making of embodiment 2 is similar to embodiment 1, and difference is only that the interfacial agent of embodiment 2 is the hexadecyltrimethylammonium chloride (cetyl trimethylammonium chloride, CTMAB) of 0.15 gram.
Experimental result shows, and embodiment 2 can obtain the monox with hollow ball structure equally.
Embodiment 3
The method for making of embodiment 3 is similar to embodiment 1, and difference is only that the interfacial agent of embodiment 3 is the polyglycol (PEG10000) of 0.15 gram.
Experimental result shows, and embodiment 2 can obtain the monox with hollow ball structure equally.
Embodiment 4
The method for making of embodiment 4 is similar to embodiment 1, and difference is only that the interfacial agent of embodiment 4 is the polyglycol (PEG300000) of 0.15 gram.
Experimental result shows, and embodiment 4 can obtain the monox with hollow ball structure equally.
Embodiment 5 makes liquid crystal display
By the Hole monox hollow granule of embodiment 1 and liquid crystal molecule MLC6080 according to 0.00625g: 0.2g part by weight mix, with an obtained liquid-crystal composition.
Above-mentioned liquid-crystal composition is filled between thin film transistor base plate and colored filter substrate, to form liquid crystal display.
Fig. 3 shows the penetrance (transmittance of liquid crystal display to visible ray under different applying voltage (applied voltage) of embodiment 5, %), as shown in Figure 3, applying voltage and penetration present a linear relationship (linear property).
Embodiment 6 makes liquid crystal display
By the Hole monox hollow granule of embodiment 2, and modify trimethyl chlorosilane ClSi (CH in its surface
3)
3.Its method of modifying is as follows:
Get appropriate Hole monox hollow granule, add in the silane ethanolic solution containing hydrophobicity functional group, reflux after 3-5 hour, hydrophobic Hole monox hollow ball particle after filtering drying, can be obtained.
Afterwards, by Hole monox hollow granule and the liquid crystal molecule MLC6080 after modifying according to 0.005g: 0.2g part by weight mix, to obtain a liquid-crystal composition.
Above-mentioned liquid-crystal composition is filled between thin film transistor base plate and colored filter substrate, to form liquid crystal display.
Experimental result shows, compared with the Hole monox hollow granule of unmodified, the liquid crystal display that in modification, the Hole monox hollow granule of trimethyl chlorosilane forms, because hydrophobic trimethyl chlorosilane can reduce the acting force to liquid crystal molecule, therefore, the driving voltage of liquid crystal display can be reduced.And Hole oxide hollow-particle provided by the present invention, its preparation is easy, and its stability high (can not go bad by illumination effect), the serviceable life of display can be improved.
Although the present invention discloses as above with several preferred embodiment; so itself and be not used to limit the present invention; have in any art and usually know the knowledgeable; without departing from the spirit and scope of the present invention; when doing arbitrary change and retouching, therefore protection scope of the present invention is when being as the criterion depending on the right person of defining.
Claims (7)
1. a liquid crystal display, is characterized in that, comprising:
One first substrate;
One second substrate; And
One liquid-crystal composition, be formed between described first substrate and described second substrate, wherein said liquid-crystal composition comprises multiple liquid crystal molecule and multiple Hole oxide hollow granule, and the described liquid crystal molecule of part is arranged in part described Hole oxide hollow granule.
2. liquid crystal display as claimed in claim 1, it is characterized in that, the refractive index of described Hole oxide hollow granule is 1.40-1.50.
3. liquid crystal display as claimed in claim 1, it is characterized in that, the weight ratio of described liquid crystal molecule and described Hole oxide hollow granule is 0.01-10.
4. liquid crystal display as claimed in claim 1, it is characterized in that, the particle size of described Hole oxide hollow granule is 100nm-2000nm.
5. liquid crystal display as claimed in claim 1, it is characterized in that, described Hole oxide hollow granule is inorganic oxide.
6. liquid crystal display as claimed in claim 5, it is characterized in that, described Hole oxide hollow granule comprises monox, aluminium oxide, titanium dioxide or zinc paste.
7. liquid crystal display as claimed in claim 1, it is characterized in that, described liquid crystal display comprises penetration, reflective and semi-penetrating trans display.
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