CN101373286A - Method for preparing polymer dispersed liquid-crystal film - Google Patents
Method for preparing polymer dispersed liquid-crystal film Download PDFInfo
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- CN101373286A CN101373286A CNA2007101420700A CN200710142070A CN101373286A CN 101373286 A CN101373286 A CN 101373286A CN A2007101420700 A CNA2007101420700 A CN A2007101420700A CN 200710142070 A CN200710142070 A CN 200710142070A CN 101373286 A CN101373286 A CN 101373286A
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- film
- porous membrane
- liquid crystal
- crystal
- liquid
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000004983 Polymer Dispersed Liquid Crystal Substances 0.000 title claims description 39
- 239000004973 liquid crystal related substance Substances 0.000 claims abstract description 65
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 239000012528 membrane Substances 0.000 claims description 63
- 239000000463 material Substances 0.000 claims description 13
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 12
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 12
- 239000007767 bonding agent Substances 0.000 claims description 9
- 239000003822 epoxy resin Substances 0.000 claims description 5
- 229920000647 polyepoxide Polymers 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims description 3
- 239000004809 Teflon Substances 0.000 claims description 2
- 229920006362 Teflon® Polymers 0.000 claims description 2
- 229920000098 polyolefin Polymers 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 239000010408 film Substances 0.000 abstract description 64
- 239000010409 thin film Substances 0.000 abstract description 10
- 229920000642 polymer Polymers 0.000 abstract description 7
- 238000006116 polymerization reaction Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000011521 glass Substances 0.000 description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 6
- 239000003595 mist Substances 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 229920006395 saturated elastomer Polymers 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 238000002834 transmittance Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 235000010290 biphenyl Nutrition 0.000 description 3
- 239000004305 biphenyl Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 238000005191 phase separation Methods 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- 239000004416 thermosoftening plastic Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- HGAZMNJKRQFZKS-UHFFFAOYSA-N chloroethene;ethenyl acetate Chemical compound ClC=C.CC(=O)OC=C HGAZMNJKRQFZKS-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- HHNHBFLGXIUXCM-GFCCVEGCSA-N cyclohexylbenzene Chemical compound [CH]1CCCC[C@@H]1C1=CC=CC=C1 HHNHBFLGXIUXCM-GFCCVEGCSA-N 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Abstract
A method for preparing a polymer decentralization liquid-crystal thin-film comprises the steps of conglutinating a porous thin-film onto a conductive film, contacting the porous thin-film with the liquid-crystal, and then conglutinating another conductive film onto the porous thin-film. The method fills the thin-film provided with the micropore structure with the liquid-crystal to obtain the polymer decentralization liquid-crystal thin-film easily. Compared with the prior methods such as the polymerization split-phase method and the like, the method of the invention can greatly simplifies the preparation technology of the polymer decentralization liquid-crystal thin-film, reduce the production cost of the polymer decentralization liquid-crystal thin-film, and facilitate the industrialized mass production of the polymer decentralization liquid-crystal thin-film.
Description
Technical field
The invention relates to a kind of preparation method of polymer dispersed liquid-crystal film.
Background technology
(Polymer Dispersed Liquid Crystal, PDLC) film is a kind of flat-panel display device that new development is got up to Polymer Dispersed Liquid Crystal.In this film, liquid crystal material is dispersed in the polymeric matrix with the form of droplet.By the effect of extra electric field, film can present two kinds of different optical states of transmission and scattering.This Polymer Dispersed Liquid Crystal has the display brightness height and can be used for flexible LCD and the advantage of intelligent glass window etc.
The method for preparing at present polymer dispersed liquid-crystal film mainly contains following several:
(1) polymerization split-phase method (Polymerization Induced Phase Separation, PIPS)
It is that polymeric material is mixed mutually with low molecular weight liquid crystal, forms uniform solution, adopts heated polymerizable or ultraviolet polymerization, makes the solubleness of liquid crystal in polymer molecule reduce gradually, liquid crystal phase is separated form liquid crystal droplet.
(2) the temperature split-phase method (Temperture Induced Phase Separation, TIPS)
It is to prepare polymer dispersed liquid-crystal film by the cooling velocity of controlling the solution that is formed by liquid crystal and thermoplastic.
(3) the solvent split-phase method (Solvent Phase Separation, SPS)
It is that thermoplastic and liquid crystal are dissolved in the solvent, obtains polymer dispersed liquid-crystal film along with feasible being separated of volatilization of solvent.
(4) microcapsule method (Nematic Curviliner Aligned Phase, NCAP)
It is by liquid crystal is mixed with water-soluble polymers, forms emulsion through stirring, and is poured on the base material dry and make polymer dispersed liquid-crystal film.
In the said method, the preparation of PIPS method is simple relatively, has become the main method of preparation polymer dispersed liquid-crystal film at present.
For example, CN 1790118A discloses a kind of preparation method of Polymer Dispersed Liquid Crystal, it is characterized in that, is to mix between 2:8～5:5 monomer and liquid crystal material according to mass percent, adding glass microballoon, light trigger mix by a certain percentage, are coated between the two-layer transparent indium tin oxide conductive plastic film, by roller bearing extruding journey film, under the temperature between liquid crystal and clear 2 the above 0.5-150 of monomer mixed system ℃, the employing exposure intensity is 15-50mW/cm
2Ultraviolet light, shone 1-15 minute, be solidified into the PDLC film; The temperature that described cleaning point is liquid crystal and monomer mixed system when anisotropic body is converted into isotropic body.
But, extensive gradually along with the use of PDLC film, the continuous increase of demand wishes that accordingly the preparation method of PDLC film is more and more easier, production cost is more and more lower, therefore, is still waiting research for the preparation method of PDLC film.
Summary of the invention
The objective of the invention is for the preparation method that overcomes polymer dispersed liquid-crystal film in the prior art is comparatively complicated, the shortcoming that preparation cost is higher provides the preparation method of the low polymer dispersed liquid-crystal film of a kind of simple cost.
The invention provides a kind of preparation method of polymer dispersed liquid-crystal film, wherein, this method comprises and porous membrane is bonded on the conducting film coating of liquid crystalline on porous membrane, bonding another conducting film on this porous membrane then.
The present invention is by easily obtaining polymer dispersed liquid-crystal film having filling liquid crystal on the film of microcellular structure.Compare with methods such as existing polymerization split-phase methods, method of the present invention has been simplified the preparation technology of polymer dispersed liquid-crystal film greatly, has reduced the production cost of polymer dispersed liquid-crystal film, helps the industrialized mass of polymer dispersed liquid-crystal film.
Embodiment
The preparation method of polymer dispersed liquid-crystal film of the present invention comprises porous membrane is bonded on the conducting film, porous membrane is contacted with liquid crystal, then bonding another conducting film on this porous membrane.
Described porous membrane can be the various thin polymer films of using always with microcellular structure, these polymer thin-film materials are conventionally known to one of skill in the art, for example, the material of described porous membrane can be in polyolefin, polyurethane, epoxy resin, polyvinyl alcohol (PVA) and the teflon one or more.Described porous membrane can be commercially available.Also can prepare according to usual way.For example, polymeric material, pore-forming material and solvent can be used the spreader coating film forming then, obtain porous membrane after removing pore-forming material and drying.
The amount of the liquid crystal of required filling is relevant on the film of the mean diameter in the hole of described porous membrane and porosity and unit area.Porosity of the present invention is the number percent that the cumulative volume of finger-hole accounts for the porous membrane volume.The mean diameter in the hole of described porous membrane and porosity can be adjusted according to the amount of required liquid crystal.The mean diameter in described hole can be the 0.5-10 micron, is preferably the 2-5 micron.The mean diameter in described hole in preferable range, the mist degree of the polymer dispersed liquid-crystal film that can reduce finally to obtain.The described porosity of described porous membrane can be 20-70 volume %, is preferably 40-50 volume %.Described porosity is in preferable range, and the polymer dispersed liquid-crystal film mist degree that finally obtains is little, can guarantee the form of film simultaneously.
The thickness of porous membrane of the present invention can be the thickness of conventional polymer dispersed liquid-crystal film.Can suitably adjust as required.It generally can be the 5-30 micron.
The present invention is bonded in porous membrane on the conducting film earlier when the preparation polymer dispersed liquid-crystal film, and porous membrane is contacted with liquid crystal.The process of described contact makes liquid crystal evenly spread on the porous membrane.As long as described contact makes the liquid crystal of absorption 5-50 gram on every square metre of porous membrane.Described porous membrane has different liquid crystal saturated extent of adsorption according to the difference of the mean diameter in porosity and hole.In order to make liquid crystal adsorbance on the described porous membrane is 5 grams/square metre more than the porous membrane, only requires that described liquid crystal saturated extent of adsorption is at 5 grams/square metre get final product more than the porous membrane.The porosity of general described porous membrane and the mean diameter in hole all can satisfy the requirement of saturated extent of adsorption at 5 grams/square metre more than the porous membrane in the above-mentioned scope of mentioning.In addition, before the liquid crystal adsorbance on the described porous membrane reaches the liquid crystal saturated extent of adsorption, can be by regulating the liquid crystal adsorbance on every square metre of porous membrane the duration of contact of the control consumption of liquid crystal and described porous membrane and liquid crystal.In order to make the liquid crystal of absorption 5-50 gram on every square metre of porous membrane, generally in described contact process, the consumption of described liquid crystal can be 20 grams/square metre more than the porous membrane, the liquid crystal consumption is excessive can not to make porous membrane absorption than the more liquid crystal of liquid crystal saturated extent of adsorption, and therefore the consumption of preferred described liquid crystal is a 20-40 gram/square metre porous membrane.The time of described contact can be 20-80 minute.The method of described contact comprises coating, impregnating, as long as can make liquid crystal enter into the hole of porous membrane.In addition, when excessive liquid crystal contacts, after contact is finished, the excessive liquid crystal in porous membrane surface should be removed at described porous membrane, and then on this porous membrane bonding another conducting film.
Behind coating of liquid crystalline on the porous membrane, in order to make liquid crystal fully soak in the micropore, method of the present invention also can comprise this porous membrane that is adsorbed with liquid crystal was left standstill 1-5 hour.
The bonding agent of porous membrane of the present invention and the bonding usefulness of conducting film can be the various conventional bonding agents that use.For example, the bonding agent of described porous membrane and the bonding usefulness of conducting film can be polyvinyl alcohol (PVA) and/or epoxy resin.Described bonding agent can be commercially available.
Conducting film of the present invention can be the conventional conducting film that uses in the polymer dispersed liquid-crystal film.For example, can be indium tin oxide (ITO) glass-film.
In addition, porous membrane of the present invention can clean with alkali lye earlier before use, cleans with deionized water then, and oven dry gets final product.Described alkali lye for example can be the potassium hydroxide aqueous solution of 10 weight %.
Liquid crystal of the present invention can be the liquid crystal material of various routines, for example, can be biphenyl liquid crystal, cyclohexylbenzene liquid crystal and ester liquid crystal etc.Described liquid crystal can be commercially available.
Further specify preparation method of the present invention below by embodiment.
Embodiment 1
Present embodiment illustrates the preparation method of polymer dispersed liquid-crystal film of the present invention.
(a day eastern electrician produces, and thickness is 30 microns, and the mean diameter in hole is 2 microns with the tygon porous membrane with the potassium hydroxide aqueous solution of 10 weight %, porosity is 50 volume %, film size is 0.5 meter * 1 meter) clean, use washed with de-ionized water then three times, again 60 ℃ of oven dry down.
Going up bonding agent (polyvinyl alcohol (PVA), Jinhuada Chemical Agent Co., Ltd., Guangzhou City) on the silk-screen, porous membrane is adhered on this ito glass film with porous membrane ito glass film of the same area (Anhui Fangxing Science Co., Ltd's product).The liquid crystal (biphenyl liquid crystal, Luquan City novel electron material factory) of coating 50 grams left standstill 80 minutes on this porous membrane.Then that the upper strata is excessive liquid crystal scrapes off, and this liquid crystal that scrapes off is collected and is weighed, and the amount that obtains this liquid crystal that scrapes off is 34 grams.Therefore, the amount of liquid crystal that adsorbs on every square metre of porous membrane is 32 grams.
Other gets an ito glass film same as described above, and bonding agent same as described above on the silk-screen is adhered to this ito glass film on the porous membrane then on it, obtains polymer dispersed liquid-crystal film.
Embodiment 2
Present embodiment illustrates the preparation method of polymer dispersed liquid-crystal film of the present invention.
(a day eastern electrician produces, and thickness is 10 microns, and the mean diameter in hole is 5 microns with the epoxy resin porous membrane with the potassium hydroxide aqueous solution of 10 weight %, porosity is 40 volume %, film size is 0.5 meter * 1 meter) clean, use washed with de-ionized water then three times, again 60 ℃ of oven dry down.
Going up bonding agent (polyvinyl alcohol (PVA), Jinhuada Chemical Agent Co., Ltd., Guangzhou City) on the silk-screen, porous membrane is adhered on this ito glass film with porous membrane ito glass film of the same area (Anhui Fangxing Science Co., Ltd's product).The liquid crystal (biphenyl liquid crystal, Luquan City novel electron material factory) of coating 70 grams left standstill 40 minutes on this porous membrane.Then that the upper strata is excessive liquid crystal scrapes off, and this liquid crystal that scrapes off is collected and is weighed, and the amount that obtains this liquid crystal that scrapes off is 46 grams.Therefore, finally calculating the amount of liquid crystal that adsorbs on every square metre of porous membrane is 48 grams.
Other gets an ito glass film same as described above, and bonding agent same as described above on the silk-screen is adhered to this ito glass film on the porous membrane then on it, obtains polymer dispersed liquid-crystal film.
Embodiment 3
The performance of the polymer dispersed liquid-crystal film that the present embodiment explanation embodiment of the invention 1 makes.
By contact voltage regulator (Shanghai Precision Scientific Apparatus Co., Ltd, WGT-S) and transmittance mist degree analyzer (permanently strong science and technology, TDGC
2J-1) transmittance and the mist degree under driving voltage, saturation voltage and the saturation voltage of mensuration film, the result is as shown in table 1.
Embodiment 4
Measure the performance of the polymer dispersed liquid-crystal film that embodiment 2 makes according to the method for embodiment 3.The result is as shown in table 1.
Table 1
| The film source | Driving voltage (V) | Saturation voltage (V) | Transmittance under the saturation voltage (%) | Mist degree under the saturation voltage (%) |
| Embodiment 1 | 30 | 70 | 95 | 6 |
| Embodiment 2 | 28 | 69 | 96 | 5 |
As can be seen from Table 1, the driving voltage and the saturation voltage of the polymer dispersed liquid-crystal film that the embodiment of the invention 1 and embodiment 2 make are all lower, in addition, the transmittance height under the saturation voltage, mist degree is low, can be used as polymer dispersed liquid-crystal film and uses.
Claims (9)
1. the preparation method of a polymer dispersed liquid-crystal film is characterized in that, this method comprises porous membrane is bonded on the conducting film, porous membrane is contacted with liquid crystal, then bonding another conducting film on this porous membrane.
2. method according to claim 1, wherein, the mean diameter in the hole of described porous membrane is the 0.5-10 micron, porosity is 20-70 volume %.
3. method according to claim 2, wherein, the mean diameter in the hole of described porous membrane is the 2-5 micron, porosity is 40-50 volume %.
4. method according to claim 1, wherein, the thickness of described porous membrane is the 5-30 micron.
5. method according to claim 1, wherein, described contact makes the liquid crystal of absorption 5-50 gram on every square metre of porous membrane.
6. method according to claim 1 or 5, wherein, the consumption of described liquid crystal is that 20 grams/square metre more than the porous membrane, the time of described contact is 20-80 minute.
7. according to any described method among the claim 1-4, wherein, the material of described porous membrane is one or more in polyolefin, polyurethane, epoxy resin, polyvinyl alcohol (PVA) and the teflon.
8. method according to claim 1, wherein, the bonding agent of described porous membrane and the bonding usefulness of conducting film is polyvinyl alcohol (PVA) and/or epoxy resin.
9. method according to claim 1, wherein, described conducting film is the indium tin oxide glass-film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101420700A CN101373286B (en) | 2007-08-22 | 2007-08-22 | Method for preparing polymer dispersed liquid-crystal film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101420700A CN101373286B (en) | 2007-08-22 | 2007-08-22 | Method for preparing polymer dispersed liquid-crystal film |
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| Publication Number | Publication Date |
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| CN101373286A true CN101373286A (en) | 2009-02-25 |
| CN101373286B CN101373286B (en) | 2010-12-08 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017010021A (en) * | 2015-06-18 | 2017-01-12 | フォトン・ダイナミクス・インコーポレーテッド | High resolution and fast switching electro-optic modulator for tft inspection |
| US11500238B2 (en) | 2018-11-30 | 2022-11-15 | Oxford University Innovation Limited | Methods of manufacturing polymer dispersed liquid crystal films |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2702058B1 (en) * | 1993-02-23 | 1995-04-07 | Thomson Csf | Process for obtaining composite materials based on polymer and liquid crystals with dichroic dyes. |
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2007
- 2007-08-22 CN CN2007101420700A patent/CN101373286B/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017010021A (en) * | 2015-06-18 | 2017-01-12 | フォトン・ダイナミクス・インコーポレーテッド | High resolution and fast switching electro-optic modulator for tft inspection |
| US11500238B2 (en) | 2018-11-30 | 2022-11-15 | Oxford University Innovation Limited | Methods of manufacturing polymer dispersed liquid crystal films |
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| Publication number | Publication date |
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| CN101373286B (en) | 2010-12-08 |
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