CN1308716A - Light-polarizing particles of improved particle size distribution - Google Patents
Light-polarizing particles of improved particle size distribution Download PDFInfo
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- CN1308716A CN1308716A CN99808446A CN99808446A CN1308716A CN 1308716 A CN1308716 A CN 1308716A CN 99808446 A CN99808446 A CN 99808446A CN 99808446 A CN99808446 A CN 99808446A CN 1308716 A CN1308716 A CN 1308716A
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- Prior art keywords
- precursor
- particle
- liquid
- light
- light valve
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- 239000002245 particle Substances 0.000 title claims abstract description 59
- 238000009826 distribution Methods 0.000 title description 4
- 239000002243 precursor Substances 0.000 claims abstract description 36
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 9
- 239000011630 iodine Substances 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 42
- 239000006194 liquid suspension Substances 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 21
- -1 alkaloid acidic salt Chemical class 0.000 claims description 11
- 239000008187 granular material Substances 0.000 claims description 11
- 230000010287 polarization Effects 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 150000002894 organic compounds Chemical class 0.000 claims description 7
- 229910052736 halogen Inorganic materials 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 229930013930 alkaloid Natural products 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 150000004820 halides Chemical class 0.000 claims description 5
- 150000002367 halogens Chemical class 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- LOUPRKONTZGTKE-WZBLMQSHSA-N Quinine Chemical compound C([C@H]([C@H](C1)C=C)C2)C[N@@]1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OC)C=C21 LOUPRKONTZGTKE-WZBLMQSHSA-N 0.000 claims description 3
- 238000004220 aggregation Methods 0.000 claims description 3
- 230000002776 aggregation Effects 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 230000006872 improvement Effects 0.000 claims description 2
- 150000001455 metallic ions Chemical class 0.000 claims description 2
- 235000001258 Cinchona calisaya Nutrition 0.000 claims 1
- LOUPRKONTZGTKE-UHFFFAOYSA-N cinchonine Natural products C1C(C(C2)C=C)CCN2C1C(O)C1=CC=NC2=CC=C(OC)C=C21 LOUPRKONTZGTKE-UHFFFAOYSA-N 0.000 claims 1
- 150000002431 hydrogen Chemical class 0.000 claims 1
- 239000002861 polymer material Substances 0.000 claims 1
- 229960000948 quinine Drugs 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 230000006641 stabilisation Effects 0.000 claims 1
- 238000011105 stabilization Methods 0.000 claims 1
- 150000001340 alkali metals Chemical class 0.000 abstract description 2
- 229910001508 alkali metal halide Inorganic materials 0.000 abstract 1
- 229910001615 alkaline earth metal halide Inorganic materials 0.000 abstract 1
- 239000000725 suspension Substances 0.000 description 12
- 230000003287 optical effect Effects 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000003381 stabilizer Substances 0.000 description 9
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 8
- 238000001556 precipitation Methods 0.000 description 8
- 239000007787 solid Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 229920003023 plastic Polymers 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 239000006228 supernatant Substances 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000005684 electric field Effects 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- MLFHJEHSLIIPHL-UHFFFAOYSA-N isoamyl acetate Chemical compound CC(C)CCOC(C)=O MLFHJEHSLIIPHL-UHFFFAOYSA-N 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 3
- UNMYWSMUMWPJLR-UHFFFAOYSA-L Calcium iodide Chemical class [Ca+2].[I-].[I-] UNMYWSMUMWPJLR-UHFFFAOYSA-L 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 150000003797 alkaloid derivatives Chemical class 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- OCLTZILENWBWIY-HKPQTANOSA-N (r)-[(2s,4s,5r)-5-ethenyl-1-azabicyclo[2.2.2]octan-2-yl]-(6-methoxyquinolin-4-yl)methanol;molecular iodine;sulfuric acid;dihydroiodide Chemical compound I.I.II.II.OS(O)(=O)=O.OS(O)(=O)=O.OS(O)(=O)=O.C([C@H]([C@H](C1)C=C)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OC)C=C21.C([C@H]([C@H](C1)C=C)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OC)C=C21.C([C@H]([C@H](C1)C=C)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OC)C=C21.C([C@H]([C@H](C1)C=C)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OC)C=C21 OCLTZILENWBWIY-HKPQTANOSA-N 0.000 description 2
- LCZUOKDVTBMCMX-UHFFFAOYSA-N 2,5-Dimethylpyrazine Chemical compound CC1=CN=C(C)C=N1 LCZUOKDVTBMCMX-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 2
- WFDIJRYMOXRFFG-UHFFFAOYSA-N acetic acid anhydride Natural products CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 2
- 150000008043 acidic salts Chemical class 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- 229940042776 anhydrous calcium iodide Drugs 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229940117955 isoamyl acetate Drugs 0.000 description 2
- 230000033001 locomotion Effects 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- GVEVNOSZLMMBOR-UHFFFAOYSA-N pyrazine-2,5-dicarboxylic acid;dihydrate Chemical compound O.O.OC(=O)C1=CN=C(C(O)=O)C=N1 GVEVNOSZLMMBOR-UHFFFAOYSA-N 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
- 239000011669 selenium Substances 0.000 description 2
- JPJALAQPGMAKDF-UHFFFAOYSA-N selenium dioxide Chemical compound O=[Se]=O JPJALAQPGMAKDF-UHFFFAOYSA-N 0.000 description 2
- 239000001934 2,5-dimethylpyrazine Substances 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000006253 efflorescence Methods 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 235000012771 pancakes Nutrition 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011802 pulverized particle Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- ZNCXUFVDFVBRDO-UHFFFAOYSA-N pyridine;sulfuric acid Chemical compound [H+].[O-]S([O-])(=O)=O.C1=CC=[NH+]C=C1 ZNCXUFVDFVBRDO-UHFFFAOYSA-N 0.000 description 1
- 229960001463 quinine bisulfate Drugs 0.000 description 1
- RONWGALEIBILOG-VMJVVOMYSA-N quinine sulfate Chemical compound [H+].[H+].[O-]S([O-])(=O)=O.C([C@H]([C@H](C1)C=C)C2)C[N@@]1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OC)C=C21.C([C@H]([C@H](C1)C=C)C2)C[N@@]1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OC)C=C21 RONWGALEIBILOG-VMJVVOMYSA-N 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/03—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on ceramics or electro-optical crystals, e.g. exhibiting Pockels effect or Kerr effect
- G02F1/055—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on ceramics or electro-optical crystals, e.g. exhibiting Pockels effect or Kerr effect the active material being a ceramic
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/17—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on variable-absorption elements not provided for in groups G02F1/015 - G02F1/169
- G02F1/172—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on variable-absorption elements not provided for in groups G02F1/015 - G02F1/169 based on a suspension of orientable dipolar particles, e.g. suspended particles displays
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3008—Polarising elements comprising dielectric particles, e.g. birefringent crystals embedded in a matrix
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/0009—Materials therefor
Landscapes
- Physics & Mathematics (AREA)
- Nonlinear Science (AREA)
- Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
- Polarising Elements (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
A method of making particles of light-polarizing material comprising reacting a precursor suitable for forming polyhalide particles with elemental iodine and a hydrohalide or an ammonium, alkali metal, or alkaline earth metal halide wherein the average size and/or median size of the precursor is less than 1 micron.
Description
Invention field
The present invention relates to be used for liquid suspension and light valve, film and solidify the suspending liquid aspect, improved the manufacture method of the light polarization particle of size-grade distribution.
Background
Knownly modulate light with light valve six more than ten years were arranged,, light valve can be described as the cell that forms by two layers of walls as employed in this article, the distance that midfeather is very little, at least one wall is transparent, on two walls electrode is housed all, generally is the form of transparent conductive coating.A kind of optical modulation element is contained in this chamber, and it can be a kind of liquid suspension of particle, or one deck distributes therein and the plastic sheeting of the droplet of particle-liquid suspending liquid in embedding.
Liquid suspension (being sometimes referred to as liquid light valve suspension in this article) contains the granule that is suspended in the liquid suspension medium.Therefore when not applying electric field, the particle performance in the liquid suspension goes out Brownian movement at random, and according to the structure of cell, kind and the concentration and the light contained energy of particle, the light beam by this cell can reflect, transmission or absorption.At this moment light valve is in dark relatively closure (OFF) state.Yet when applying electric field by the light valve suspension in the light valve, particle is with regard to marshalling, and for many kinds of suspending liquid, most of light can pass through cell.At this moment light valve just is in transparent relatively opening (ON) state.
Light valve is recommended to be used for many purposes, comprises for example alphanumeric display, TV demonstration, window, sunshade, shadow shield, mirror, glasses etc., is used for controlling the light quantity by them.Also to be recognized as be " spd " or " SPD " to Xu Shu light valve in this article.
For many application, activable material is plastic sheeting rather than liquid suspension preferably.Such as, in being used as the light valve of variable light inlet window, the plastic sheeting that is distributed with the liquid suspension droplet therein just is better than single liquid suspension of using, because by using film can avoid hydrostatic effects, for example relevant with high liquid suspension fluid column bulging also can be avoided possible spillage risk.Use another advantage of plastic sheeting to be that in plastic sheeting, particle generally just is present in the very little drop, therefore when activating film repeatedly, tangible congregation can not take place with voltage.
Therefore, " the light valve film " that uses in this article is the film of liquid suspension droplet of particle of distributing therein.
At United States Patent (USP) 5,409, disclose in 734 by the class light valve film of homogeneous phase solution through being separated and making.The light valve film of making through crosslinked emulsions is disclosed in the United States Patent (USP) 5,463,491 and 5,463,492 that transfers assignee of the present invention.All these patents and other patent and other source of enumerating in this article are all incorporated by reference in this article.
For (being called sheet polarizers sometimes at curing suspending liquid such as light polarization plate, they cuttings can be made the polarization Sunglasses lenses sun clips or as optical filtering) in application, the light polarization particle can be dispersed in, or is distributed in the sheet of suitable filmogen (as cellulose acetate or polyvinyl alcohol (PVA) etc.).In the prior art, the method for making the curing suspending liquid that sheet polarizers uses is known.Yet, solidifying in the suspending liquid at these, particle is irremovable.See United States Patent (USP) 2,178,996 and 2,041,138.
Liquid light valve suspension
1. liquid suspension medium and stabilizing agent
Liquid light valve suspension can be any liquid light valve suspension well known in the prior art, can prepare according to known technology.The term of Shi Yonging " liquid light valve suspension " refers to a kind of disperseed therein many short grained " liquid suspension medium " in this article.This " liquid suspension medium " contains the liquid of the anti-electricity of one or more non-water, and preferred dissolution has at least a polymeric type stabilizing agent therein, and its effect is the tendency that reduces this particle aggregation, and keeps their to disperse and be the state of suspending liquid.
Liquid light valve suspension of the present invention can comprise anyly proposes previously, is used for the liquid suspension medium of in light valve suspended particle.Can use in the prior art the liquid suspension medium that uses here, such as, but be not limited to those disclosed liquid suspension medium in 175 and 4,407,565 at United States Patent (USP) 4,247.In general, select one or both liquid suspension mediums or be dissolved in wherein polymerization stabilizer, make under gravitational equilibrium, to maintain particles suspended.
When using polymerization stabilizer, it can be the solid polymer of single variety, this polymkeric substance can and particle surface combination, but also can be dissolved in one or more on-aqueous liquids in the liquid suspension medium.In addition, can there be two or more to serve as the solid polymerization stabilizing agent of polymerization-stable system.Such as; this particle can be coated with first kind of solid polymerization stabilizing agent; as the solid polymerization stabilizing agent of NC Nitroncellulose (in fact it provides a kind of plane surface coating to particle) and one or more other types (it with first kind of solid polymerization stabilizing agent in conjunction with or be connected; and be dissolved in the liquid suspension medium), provide dispersion and space protection to particle.As at United States Patent (USP) 5,463, described in 492, the liquid polymeric stabilizing agent can be used for promoting, particularly promotes the light valve film in SPD.
2. particle
As everyone knows, inorganic and organic granular can be used in the light valve suspension.Yet, the present invention relates to a kind of improved method for preparing particle, this particle is the polyhalide (referring to perhalide in the prior art sometimes) of organic compound, as alkaloidal acidic salt etc.Polyhalide particle of the present invention can be an opticity, as halogen-containing light polarization material, and the polyhalide of biological example alkali acidic salt.(" alkaloid " speech of Shi Yonging refers to alkaloid in this article, as " chemical dictionary " (Chemical Dictionary) of Hackh the 4th edition, and McGraw-Hill books company, New York, defined in 1969).As everyone knows, if the polyhalide of preparation alkaloid acidic salt, this alkaloid part can be as " chemical dictionary " the defined quinine alkaloid at above-mentioned Hackh.United States Patent (USP) 2,178,996 and 2,289,712 have at length mentioned the purposes of the polyhalide of quinine alkaloid acidic salt.These particles can be light absorbing or catoptrical.This particle can also be the hydrogenation polyhalide of quinine alkaloid acidic salt, as at United States Patent (USP) 4,131, and many iodide of the dihydro Xin Keni pyridine sulfate of narration in 334.
Recently, at United States Patent (USP) 4,877, proposed to be used for the improved polyhalide particle with advantageous feature of light valve in 313,5,002,701,5,093,041 and 5,516,463.These " polyhalide particles " are by organic compound, and generally nitrogenous organic compound and elemental iodine and halogen acid or ammonium, alkali halide or alkaline-earth halide reaction obtain.In this article such organic compound is called " precursor ".
At USSR (Union of Soviet Socialist Republics) " general chemistry magazine " (The Journal of General Chemistry) the 20th volume, in 1005～1016 pages (1950), in the article of D.A.Godina and G.P.Faerman " optical property of many iodide and structure " polyhalide particle of the prior art has been discussed at length also.Such as quinine iodosulfate is many iodide of quinine bisulfate, the 10th edition (Merck ﹠amp of " Merck index " (The Merck Index); Co., Inc., Rahway, N.J.) " quinine iodosulfate " under one's name with 4C
20H
24N
2O
23H
2SO
42HII
46H
2The formula of O has provided its molecular formula.In polyiodide, imagination has formed chain with the iodine negative ion, and this compound is the high light polarizer.See United States Patent (USP) 4,877,313 and people's such as Teitelbaum " American Chemical Society's will " (JACS) 100 (1978), 3215～3217 pages.The term of Shi Yonging " polyhalide " refers to the compound as many iodide in this article, but wherein has at least some iodine negative ion to be replaced by other halogen anion.
As everyone knows, the polyhalide particle that can be used for light valve preferably has colloid size, the on average about 1 μ m or littler of the full-size of this particle in other words.The full-size of preferred most of polyhalide particles is less than half of blue light wavelength, i.e. 2000 or shorter are to keep light scattering extremely low.
Explanation of the present invention
The invention provides a kind of preparation method who is particularly suitable for as the polyhalide particle of liquid light valve suspension particle, this method comprises makes " precursor " and the halide reaction of elemental iodine and halogen acid or ammonium, alkaline metal or earth alkali metal with regulation particle size.This precursor can be before by with elemental iodine and halogen acid or ammonium, alkaline metal or alkaline-earth halide reaction, be used for forming any compound of organic polyhalide particle.Such as, this precursor can be a quinine alkaloid acidic salt (United States Patent (USP) 2,178,996 and 2,289,712), the alkaloid acidic salt (United States Patent (USP) 4 of hydrogenation, 131,334) or contain one or several can chelating the organic compound (United States Patent (USP) 4,877 of group of hydrogen, ammonium or metallic ion, 313,5,002,701,5,093,041 and 5,516,463), all these United States Patent (USP)s are all incorporated by reference at this.This precursor can be any color, but generally is made up of the crystal (being called " particle " in this article sometimes) of shallow white or off-white look.
We are surprised to find, if the average-size of precursor and/or median size less than 1 μ m, preferably less than 0.75 μ m, then the quality by the polyhalide particle of its manufacturing can be significantly improved.The pulverizing of precursor granules (reducing size) provides required granularity, this can be realized by any device that can reduce its size, as long as this process does not cause pulverized particle aggregation or caking, the advantage of pulverizing can be offset because assemble or lump, and the increase of particle effective dimensions can be caused actually.Such as, can use mortar and pestle, perhaps precursor granules is pulverized or is ground with bowl mill or any proper device, can be in dry state or wetting with liquid, perhaps with other solid, inert material with the help efflorescence.In addition, precursor granules can be collided mutually because being subjected to the effect of quick air motion, such as advertising with hypersonic air flow or air draught.
As what use in this article, if precursor granules or crystal are broken, reduced size in other words, that just means that its average-size and/or its median size have been reduced.The particle of Shi Yonging " size " means and refers to the full-size of particle in this article.
With embodiment preferred the present invention is described in the following embodiments.
A kind of polyhalide particle (crystal) of typical new-type prior art is a pyrazine-2, the many iodide of 5-dicarboxylic acid two hydration calcium iodides.The program that this crystal and its liquid suspension are used for light valve of making is disclosed in embodiment 1.
Embodiment 1 (prior art)
Make the prescription of many iodide crystal and liquid light valve suspension thereof
In a suitably big or small jar, add following reagent in the order shown:
160g 1/4sec ss type NC Nitroncellulose (doing) is dissolved in capryl acetate
In 6.98% solution
3g pyrazine-2,5-dicarboxylic acid dihydrate (precursor)
4.5g iodine
2.64g anhydrous calcium iodide
1.8g absolute methanol
0.33g jar and jolting about half an hour on the water cover.Jar is put into ultrasonic generator, become blue fully, approximately need 10 hours until solution.Examine under a microscope solution, to determine precursor, CaI
2Fully react with iodine, promptly do not have the unreacted precursor of significant amounts to exist.When initial fall time is 8～15 milliseconds, obtain maximum productive rate.If fall time is shorter than 8 milliseconds, just after adding methyl alcohol, adds about 0.05g water and prepare again.
Determine fall time by following operation.The suspending liquid of particle in the light valve suspending medium that forms is filled in the light valve chamber, and this light valve chamber comprises two glass sheet that have suitable electrode, therebetween at a distance of 5mil.Use such as the continuous light that in tungsten lamp, produces and shine this light valve suspension.On electrode, apply 10Hz voltage, the particle suspension liquid in light valve is excited with respect to base measurement 55V.Need about 2～3 milliseconds and make light valve reach opening, after about 20 milliseconds, disconnect electric field.Measure the fall time that light valve changes to complete closure state (OFF) subsequently.(seeing United States Patent (USP) 5,516,463 second hurdle, 37～48 row).
11, with this solution centrifugal 1hr, discard supernatant liquor under the 500rpm.Court transfers to 15min on the paper handkerchief with drainpipe.In pipe, sediment is put into the glass jar of having weighed, and notes precipitation weight.Every gram precipitation adds the 15g capryl acetate, jolting half an hour, makes the precipitation dispersion with ultrasonic Treatment 10hr again.
2, with the centrifugal 5～15min of dispersion liquid, decant is also collected supernatant liquor under the 500rpm.Fall time should be 8～12 milliseconds, if too high, centrifugal once more supernatant liquor.
9, centrifugal supernatant liquor half an hour under the 500rpm, and discard supernatant liquor, drainpipe is put into 15min on the paper handkerchief upside down.Collecting precipitation in the glass jar of having weighed, every gram precipitation adds 10g acetic anhydride isopentyl ester.Jolting half an hour, will precipitate dispersion with ultrasonic Treatment 10hr again.Be referred to as " initial concentration liquid " below.
At United States Patent (USP) 5,463,491 the 4th hurdle, the 48th～66 row has been narrated a kind of liquid plasticizer tri trimellitate n-pentyl ester (TNPTM), amount with 9g joins it in initial concentration liquid, puts into 60 ℃ rotary evaporating device 2hr together, and isoamyl acetate is evaporated.Can determine the amount of the TNPTM of adding by rule of thumb according to needing great granule density in the final concentrate that obtains (being dried initial concentration liquid).Can dilute final concentrate with required solvent or the mixed solvent that any other dense polymkeric substance can dissolve then.Can use other liquid plasticizer.
In order to prepare the concentrate that in SPD light valve film, uses, according to United States Patent (USP) 5,463, the guidance of an embodiment of 492, before the evaporation isoamyl acetate, in above-mentioned initial concentration liquid, do not add TNPTM, but can add liquid polymers, such as n-butyl acrylate/acrylic acid seven fluorine butyl ester/hydroxyethyl acrylate multipolymer.
Can carry out various changes to the running program of above-mentioned many iodide of manufacturing crystal,, perhaps change ultrasonic Treatment such as the quantity that changes some reactants, change centrifugation time or running program.
Embodiment 2 has provided in embodiment 1 precursor material that uses, i.e. pyrazine-2, the prior art manufacture method of 5-dicarboxylic acid dihydrate.
Embodiment 2 (prior art)
Pyrazine-2, the manufacture method of 5-dicarboxylic acid dihydrate
In a 1L round-bottomed flask that mechanical raking and reflux condenser be housed, add 2,5-dimethyl pyrazine (25g), pyridine (500mL), selenium dioxide (125g) and water (50mL).With potpourri backflow 11～12hr, behind about 20min, the solution of boiling presents orange red, and selenium is precipitated out gradually simultaneously.
Allow the suspending liquid cool to room temperature, filter out precipitation, be i.e. pyrazine-2, the potpourri of 5-dicarboxylic acid and selenium.With the reaction dissolvent drip washing flask and the stirrer that filter out.Reaction dissolvent turned back in the flask reuse.With the ammonium hydroxide washing precipitation of 2N, until all pyrazines-2, the 5-dicarboxylic acid all dissolves.With the flow velocity of 30mL/min ammonium hydroxide and the pyrazine-2 with 2N, the 5-dicarboxylic acid is together by slurried Darco activated charcoal (12～20 orders, chromatographic column 250g).
Concentrated hydrochloric acid (100mL) is joined in the colourless eluent of 400mL portion, obtain pyrazine-2, the white precipitate of 5-dicarboxylic acid filters out it, with hydrochloric acid and the washing of 20mL icy water of 20mL2N, uses the 20mL washing with acetone again.Make precipitation air-dryly behind the smell that does not have acetone, obtain precursor, i.e. pyrazine-2,5-dicarboxylic acid dihydrate is standby.
In order to represent the quality that the present invention has improved polyhalide particle as referred to herein, and, this improvement quantitatively need define several terms for being carried out.The optical density of light valve window test cabinet is the optical density " OD of its closure state (OFF) under activation condition not
Off".When adding voltage on the conductive coating (electrode) at test cabinet, contained liquid suspension or the particle in the film are orientated in the chamber, cause that transmitted light increases, and cause that optical density descends.When this chamber is activated when opening in other words, claim the optical density of this reduction to be " OD in this article
On".In order to carry out test herein, apply the effective value that frequency is 10KHz (RMS) 55V voltage, use the test cabinet of electrode gap as 5mil.Therefore, the electric field intensity that is applied on the test cabinet is 11V effective value/mil.In this article with OD
OffDivided by OD
OnBe referred to as the optical density ratio, or be referred to as ODR.Among the superincumbent embodiment 1, the fall time t that measures liquid suspension in the test cabinet is disclosed
dMethod.In general, wish that the light valve liquid suspension has bigger ODR and less t
dTherefore, in order to measure the gross properties of suspending liquid, we define its efficient E is the t of unit for its ODR with the second divided by it
dSuch as, a kind of optical density ratio of liquid suspension is 2.0, and fall time is 10 milliseconds (0.018 seconds), and calculating its efficient is exactly E=2.0/0.018=111.
Available E is high more good more.
Embodiment 3A
In an Erlenmeyer flask, with shown in the following substance dissolves of quantity contain in the capryl acetate solution (containing 0.11g water) of 1/4ss type NC Nitroncellulose of 6.98% dissolving in 132.5g:
4.5g iodine
2.64g anhydrous calcium iodide
1.8g methyl alcohol
0.53g water
In above-mentioned solution, add 3g the pyrazine-2 described in the embodiment 2 in front then by the art methods preparation, 5-dicarboxylic acid dihydrate (precursor), with flask be placed on 45 ℃ (Rockville, Maryland) model of Zhi Zaoing is 3hr in the water-bath jolting device of WB-20 by Elmeco engineering corporation.Then this suspending liquid is stirred 2hr with ultrasound wave.Write down the granularity of precursor in the following Table 1.
Embodiment 3B
Repeat embodiment 3A, just (Aveka company, Woodbury Minnesota) are called in this article in the machine of " flat mill " (pancake mill) and in advance precursor are pulverized by supplier, this machine has used the ultrasonic air air-flow, causes precursor granules sharp impacts each other.The granularity of this precursor is recorded in the following table 1.
From the Erlenmeyer flask, take out the suspending liquid of embodiment 3A and 3B, centrifugal according to the running program of embodiment 1, obtain initial concentration liquid.
Table 1 has gathered the data of the various suspending liquid of being narrated in embodiment 3A and 3B, be respectively the average-size and the median size of ODR, fall time, efficient and used precursor granules.
Table 1
The data of iodide suspending liquid more than two kinds relatively
First kind is the precursor preparation made from prior art
Second kind is with the precursor preparation of pulverizing
| The size of used precursor granules | Optical density compares * | Fall time * | Efficient * | ||
| Average-size | Median size | ||||
| Embodiment 3A | ?6.33μm | ????1.12μm | ??3.13 | ??23ms | ??136 |
| Embodiment 3B | ?0.74μm | ????0.68μm | ??3.00 | ??10.5ms | ??285 |
* for initial concentration liquid (as described in example 1 above), but behind initial reaction, have only the ultrasonic Treatment of 2hr, after the first and the 3rd centrifugation step, add the ultrasonic Treatment of jolting and 2hr.
Except pyrazine-2, beyond the 5-dicarboxylic acid dihydrate, in the prior art or any solid precursor that in invention from now on, uses,, can advantageously pulverize as disclosed in the present invention as long as can be used for making the polyhalide particle.
Though we do not wish to be fettered by any specific theory, the efficient why pulverizing can cause strengthening the polyhalide particle is described, but we think to pulverize why strengthen efficient, be because can form littler particle, and, therefore can produce the size-grade distribution suspending liquid littler than the polydispersity of prior art suspending liquid in that they begin growth approximately simultaneously.
Claims (12)
1. the manufacture method of a light polarization material granule, this method comprises and will be suitable for forming precursor and elemental iodine and halogen acid or ammonium, alkaline metal or the alkaline-earth halide reaction of polyhalide particle that wherein the average-size of this precursor and/or median size are less than 1 μ m.
2. method as claimed in claim 1, wherein the average-size of this precursor and/or median size are less than 0-75 μ m.
3. it is preceding for this precursor provides required granularity that method as claimed in claim 1, this method also are included in reaction, and its method is to reduce the granularity of precursor, but does not cause particle aggregation or the caking that has reduced size.
4. method as claimed in claim 1, wherein this precursor is the polyhalide of organic compound.
5. method as claimed in claim 4, wherein the polyhalide of organic compound is an alkaloid acidic salt etc.
6. method as claimed in claim 1, wherein this precursor is nitrogenous organic compound.
7. method as claimed in claim 1, wherein this precursor is the alkaloidal salt of quinine.
8. method as claimed in claim 1, wherein this precursor be contain one or several can chelating hydrogen, the organic compound of the group of ammonium or metallic ion.
9. according to the particle of any one described method preparation in the claim 1～8.
10. the improvement of being carried out in light valve, this light valve comprise the cell of the suspending liquid of the light polarization particle that contains in liquid suspension medium, and wherein particle is the particle according to claim 1.
11. contain the light polarization body of the many particles as claimed in claim 9 that are dispersed in the carrier, the polarization axle of these particles is orientated, and suppressed by vector is keeping motionless with substantially parallel state.
12. a liquid suspension, contain anti-electric liquid suspension medium, many be dispersed in wherein as claimed in claim 9 have do not wait the granule of shape shaft and be dissolved in wherein be used for make particle dispersion at stabilization of polymer material suspending liquid, at least a.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US9219898P | 1998-07-09 | 1998-07-09 | |
| US60/092,198 | 1998-07-09 |
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| CN1107199C CN1107199C (en) | 2003-04-30 |
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| CN99808446A Expired - Fee Related CN1107199C (en) | 1998-07-09 | 1999-07-09 | Light-polarizing particles of improved particle size distribution |
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| EP (1) | EP1105776A4 (en) |
| JP (1) | JP3947359B2 (en) |
| KR (1) | KR100391748B1 (en) |
| CN (1) | CN1107199C (en) |
| AU (1) | AU737670B2 (en) |
| BR (1) | BR9911937A (en) |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100345009C (en) * | 2002-10-08 | 2007-10-24 | 日东电工株式会社 | Polarizing device, optical film and image display |
| CN111471448A (en) * | 2020-05-11 | 2020-07-31 | 江苏铁锚玻璃股份有限公司 | Liquid bipolar color-changing particle, preparation method of electrochromic layer and electrochromic device |
| CN115093407A (en) * | 2022-06-20 | 2022-09-23 | 深圳市华科创智技术有限公司 | Method for preparing quinine iodosulfate nanorods in controllable manner under assistance of ball milling |
| CN115838357A (en) * | 2022-12-06 | 2023-03-24 | 深圳市华科创智技术有限公司 | Light valve, iodopyrazine, preparation method and application thereof |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101275728B1 (en) * | 2005-08-23 | 2013-06-14 | 엘지디스플레이 주식회사 | Flat panel display |
| KR101232136B1 (en) * | 2005-09-14 | 2013-02-12 | 엘지디스플레이 주식회사 | Method of repair an Liquid Crystal Cell, method of manufacturing Liquid Crystal Display Device using the same, and Liquid Crystal Display repaired using the same |
| SI3147317T1 (en) | 2015-09-28 | 2018-01-31 | Evonik Degussa Gmbh | Tripentylester of trimellitic acid |
| JPWO2022163492A1 (en) * | 2021-01-28 | 2022-08-04 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4422963A (en) * | 1977-05-11 | 1983-12-27 | Research Frontiers Incorporated | Light valve polarizing materials and suspensions thereof |
| US5002701A (en) * | 1989-02-10 | 1991-03-26 | Research Frontiers Incorporated | Light polarizing materials and suspensions thereof |
| US5093041A (en) * | 1990-07-30 | 1992-03-03 | Research Frontiers Incorporated | Light-polarizing material based on ethylenediamine polyacetic acid derivatives |
| US5409734A (en) * | 1992-01-10 | 1995-04-25 | Hankuk Glass Industries, Inc. | Making liquid suspension type light valve film |
| US5516463A (en) * | 1993-07-21 | 1996-05-14 | Research Frontiers Incorporated | Method of making light-polarizing particles |
| US5650872A (en) * | 1994-12-08 | 1997-07-22 | Research Frontiers Incorporated | Light valve containing ultrafine particles |
-
1999
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- 1999-07-09 JP JP2000559376A patent/JP3947359B2/en not_active Expired - Lifetime
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100345009C (en) * | 2002-10-08 | 2007-10-24 | 日东电工株式会社 | Polarizing device, optical film and image display |
| CN111471448A (en) * | 2020-05-11 | 2020-07-31 | 江苏铁锚玻璃股份有限公司 | Liquid bipolar color-changing particle, preparation method of electrochromic layer and electrochromic device |
| CN111471448B (en) * | 2020-05-11 | 2023-07-11 | 江苏铁锚玻璃股份有限公司 | Liquid bipolar color-changing particles, preparation method of electrochromic layer and electrochromic device |
| CN115093407A (en) * | 2022-06-20 | 2022-09-23 | 深圳市华科创智技术有限公司 | Method for preparing quinine iodosulfate nanorods in controllable manner under assistance of ball milling |
| CN115093407B (en) * | 2022-06-20 | 2024-05-03 | 深圳市华科创智技术有限公司 | Method for controllably preparing quinine iodized sulfate nanorods with assistance of ball milling |
| CN115838357A (en) * | 2022-12-06 | 2023-03-24 | 深圳市华科创智技术有限公司 | Light valve, iodopyrazine, preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1107199C (en) | 2003-04-30 |
| WO2000003178A1 (en) | 2000-01-20 |
| KR100391748B1 (en) | 2003-07-16 |
| JP2002520645A (en) | 2002-07-09 |
| EP1105776A1 (en) | 2001-06-13 |
| AU5209999A (en) | 2000-02-01 |
| BR9911937A (en) | 2001-03-27 |
| CA2336371C (en) | 2005-01-04 |
| EP1105776A4 (en) | 2005-04-13 |
| CA2336371A1 (en) | 2000-01-20 |
| KR20010071747A (en) | 2001-07-31 |
| AU737670B2 (en) | 2001-08-30 |
| JP3947359B2 (en) | 2007-07-18 |
| WO2000003177A1 (en) | 2000-01-20 |
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