CN101225308A - Method for preparing polymer dispersion liquid crystal material by ultraviolet-heating step-polymerization process - Google Patents
Method for preparing polymer dispersion liquid crystal material by ultraviolet-heating step-polymerization process Download PDFInfo
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Abstract
The invention in particular relates to a preparation method of polymer dispersing liquid crystal film by an ultraviolet irradiating-heating plus stepwise initiated polymerization and phase separation method, belonging to the functional material field, which is applied in the preparation of electric controlled intelligent glass. The preparation method is characterized in that: the nematic liquid crystal, the monomer which can be polymerized under ultraviolet light, the light initiator, the thermal polymerized monomer and the glass microsphere is blended and then are clipped between two pieces of transparent conductive film plated with indium tin oxide, and then film with the thickness of 20 Mum if formed and is irradiated by the ultraviolet light with the wavelength of 365nm at 0 to 25 degrees; the intensity of the ultraviolet light is 20.0mW/m<2> and the illumination time is 1 to 10 minutes; the thermal polymerization temperature is 60 to 100 degrees, the holding time is 5 to 8 hours, at last the PDLC film is prepared by solidification. The polymer dispersing liquid crystal film has the advantages that: because of the stepwise polymerization crosslinking reaction which is carried out by selecting the monomer polymerized by ultraviolet and thermal polymerized monomer and irradiating and heating under ultraviolet light, the electro-optic performance the PDLC film is improved, the network strength of the polymer is enhanced, meanwhile, the bonding force of the interface between the polymer network and the ITO film are reinforced.
Description
Technical field
The invention belongs to field of functional materials, particularly a kind of employing ultraviolet light irradiation-heating substep initiated polymerization phase-splitting (PIPS) method prepares Polymer Dispersed Liquid Crystal (PDLC) film, and it is applied to the preparation method of automatically controlled intelligent glass.
Background technology
Intelligent glass is that optical properties such as a kind of transmitance, reflectivity or color can wait the glass of regulating by electric field, temperature, magnetic field.(Polymer dispersed liquidcrystals, PDLC) film is the compound electrooptical material of a kind of liquid crystal/polymer to the Polymer Dispersed Liquid Crystal that the present invention adopts.PDLC is applied in automatically controlled intelligent glass field, by regulating extra electric field glass is changed between transparent and opaque two states.Automatically controlled intelligent glass has energy-saving and environmental protection, protection privacy, safety, sound insulation and regulates and control advantages such as convenient, can be widely used in places such as high-grade office building, residential building, television station, Surveillance center.
Pdlc film is the nematic liquid crystal droplet to be dispersed in the polymeric matrix and the optical thin film that forms.The PDLC film is a kind of novel liquid crystal functional materials, has good electro-optical characteristic, comprises lower threshold voltage and saturation voltage, time of response and higher contrast ratio faster, and can make the film of different shape, all thickness at an easy rate.This liquid crystal/polymer composite is clipped in two-layer transparent tin indium oxide (ITO) conductive glass or the transparent ITO conductive plastic film, and just can be prepared into transmitance can be with the automatically controlled intelligent glass of electric field controls.When not applying electric field, random alignment is vowed in the sensing of liquid crystal droplet in the PDLC film, because light is by the ordinary refraction index (n of liquid crystal droplet
o) with specific refractory power (n by polymeric matrix
p) do not match, multiple reflection and refraction take place in light on liquid crystal and polymer interface, thereby the automatically controlled intelligent glass material of preparation is intensive scattering states (opaque); When the normal orientation along the PDLC film applied electric field, liquid crystal droplet points to vowed along electric field orientation, if select the ordinary refraction index (n of liquid crystal for use
o) with the specific refractory power (n of polymkeric substance
p) be complementary, light in film, do not take place the reflection and the refraction and directly transmit, the PDLC film is clear state; After electric field is closed, the sensing of the liquid crystal molecule in the PDLC film in the liquid crystal droplet vow with the effect of macromolecule network anchoring energy under reply at random and point to, the PDLC film becomes the scattering of light attitude again.
Automatically controlled intelligent glass prepare the most key link be how to guarantee pdlc film satisfactory stability performance with and good electro-optical properties.The domestic and international at present research to pdlc film mainly is conceived to shorten the pdlc film time of response, reduces aspects such as driving voltage and raising contrast gradient.The photoelectric properties of pdlc film and polymkeric substance macromolecule network structure are closely related, so the selection of photo polymerization monomer and the electro-optical properties that is mixed to the PDLC film have material impact.
In automatically controlled intelligent glass preparation process; the situation that causes the ITO plastics film to break away from cohesive force undertighten between liquid crystal/polymer composite and the two-layer ITO plastics film appears and through regular meeting also; this has brought very big difficulty for large-scale explained hereafter; not only reduce the performance quality of product, also had a strong impact on the economic benefit of product.
Summary of the invention
The purpose of this invention is to provide a kind of method of improving the automatically controlled intelligent glass material of preparation, the intelligent glass material of preparation can come controlling polymers macromolecule network structure by uv photopolymerization monomer and the monomeric allotment of thermopolymerization, improve the electro-optical properties of PDLC film, strengthen cohesive force between liquid crystal/polymer composite and the two-layer ITO plastics film, and the thermostability of raising PDLC film, well solve the practical problems in producing.
UV-light-heating step polymerization prepares the method for polymer dispersion liquid crystal material, be clipped in after it is characterized in that nematic liquid crystal, UV-light polymerisable monomer, light trigger, thermopolymerization monomer and glass microballon mixed in the middle of two nesa coatings that are coated with tin indium oxide (ITO), even with roll-in, shine with UV-light, sample is heated, room temperature is reduced in the insulation back in air, be solidified into pdlc film.
The UV-light polymerisable monomer is acrylate, methacrylic ester, styryl, and diacetyl, the quantity of active function groups is 1～5.The thermopolymerization monomer is Resins, epoxy and the fatty amine epoxy hardener that contains the conjugate ring oxygen groups.Light trigger is that benzil ketals is (as benzil dimethyl ketal, i.e. benzoin dimethylether.Trade name is Irgacure 651) or fragrant ketone (as benzophenone, sulfo-anthrone etc.).
The making processes step is:
(1) UV-light polymerisable monomer and thermopolymerization monomer are mixed by mass ratio at 1.5: 1 are polymerisable monomer.
(2) with nematic liquid crystal be mixed after polymerisable monomer mix at 7: 3 by mass ratio, at room temperature (0 ℃～25 ℃) form isotropic liquid.
(3) add light trigger in isotropic liquid and form mixed system, photoinitiator levels is 1.0～5.0% of an isotropic liquid quality.
(4) adding particle diameter to mixed system is the glass microballon of 20 μ m, the thickness of control pdlc film.The content of glass microballon is about 0.5～1.0% of mixed system total mass.
(5) after being mixed, nematic liquid crystal, UV-light polymerisable monomer, light trigger, thermopolymerization monomer and glass microballon be clipped in the middle of two nesa coatings that are coated with tin indium oxide (ITO), even with roll-in, forming the thick rete of 20 μ m, is that the UV-light of 365nm is shone with wavelength down at 0～25 ℃.The uv photopolymerization temperature is controlled at 0.5～1.0 ℃ of polymerisable monomer/more than the nematic liquid crystal mixed system clearing point by the temperature control platform, and ultraviolet ray intensity is 20.0mW/m
2, light application time is 1～10 minute; Thermopolymerization temperature subsequently is 60～100 ℃, and the heat tracing time is 5～8 hours, finally is solidified into pdlc film.
Ultraviolet ray intensity can be regulated by the distance of regulating ultraviolet lamp and sample, thus control pdlc film rate of polymerization.Polymerisable monomer/nematic liquid crystal mixed system clearing point i.e. the temperature of this mixed system anisotropy when isotropic transition, and available differential scanning calorimetry (DSC) is accurately measured.
UV-light polymerisable monomer chemical structure is shown in chemical structural formula 1～2:
Chemical structural formula 1: tri (propylene glycol) diacrylate (TPGDA)
Chemical structural formula 2: pentaerythritol triacrylate (PETA)
Thermopolymerization monomer chemical structure is shown in chemical structural formula 3～4:
Chemical structural formula 3:DGEBA Resins, epoxy, n=0.03
Chemical structural formula 4: fatty amine epoxy hardener Jeffamine D-400
The invention has the advantages that: by selecting UV-light polymerisable monomer and thermopolymerization monomer, through ultraviolet light irradiation and the step-by-step polymerization crosslinking reaction that adds the above-mentioned polymerization system of thermal initiation, formation has the very macromolecule network of high crosslink density, improve the cross-linking density of PDLC film, reach the electro-optical properties that improves the PDLC film simultaneously, the purpose that strengthens the interfacial adhesion between polymer network intensity and raising macromolecule network and the ITO film.
Description of drawings
Fig. 1 is the electro-optical properties curve of embodiment among the present invention (sample 1) and comparative example (sample 2).
Fig. 2～3 are respectively PDLC film macromolecule network scanning electron microscope (SEM) photos in embodiment 1 and the comparative example among the present invention.
Embodiment
The tri (propylene glycol) diacrylate (TPGDA) that will contain acrylate-functional groups mixes by mass ratio with pentaerythritol triacrylate (PETA) at 2: 1, as the uv photopolymerization monomer; The DGEBA Resins, epoxy and the fatty amine epoxy hardener Jeffamine D-400 that will contain the conjugate ring oxygen groups mix by mass ratio at 1: 1, as the uv photopolymerization monomer.Above-mentioned UV-light polymerisable monomer and thermopolymerization monomer are mixed by mass ratio at 1.5: 1, and with this mixed system as polymerization single polymerization monomer.Above-mentioned two kinds of polymerisable monomer materials are all from the commercially available prod, without being further purified.The nematic liquid crystal of selecting for use among the present invention is SLC1717 (Shijiazhuang Yongshenghuaqing Liquid Crystal Co., Ltd, Tc=92 a ℃).Nematic liquid crystal and the above-mentioned polymerisable monomer that is mixed are mixed by mass ratio at 7: 3, and at room temperature (20 ℃) form isotropic liquid.Light trigger Irgacure651 content is 5.0% of monomer total mass.Adding particle diameter is the glass microballon of 20 μ m, the thickness of control pdlc film.The content of glass microballon is about 0.5～1.0% of mixed system total mass.
To be clipped in behind nematic liquid crystal, UV-light polymerisable monomer, light trigger, thermopolymerization monomer and the nano microsphere uniform mixing in the middle of two nesa coatings that are coated with ITO, even with roll-in, forming the thick rete of 20 μ m, is that the UV-light of 365nm is shone with wavelength down at 0 ℃.Ultraviolet ray intensity is 20.0mW/m
2, light application time is 5.0 minutes, afterwards the sample that obtains is put into baking oven, and Heating temperature is 90 ℃, and be 5 hours heat-up time, and sample is cold going to room temperature in air, promptly obtains the PDLC film of embodiment 1.Promptly get required automatically controlled intelligent glass material with the above-mentioned pdlc film that makes and glass are compound.
The electric light curve of PDLC film that records above-mentioned preparation with the liquid crystal comprehensive parameter tester is shown in Fig. 1 (sample 1).Scanning electron microscope (SEM) picture of PDLC film macromolecule network as shown in Figure 2 among the embodiment 1.
Embodiment (sample 1) adopts ultraviolet light irradiation-heating step-by-step polymerization method preparation, and wherein the monomeric mass ratio of UV-light polymerisable monomer and thermopolymerization is 1.5: 1, and nematic liquid crystal is 7: 3 with the mass ratio of the polymerisable monomer that is mixed.Comparative example (sample 2) adopts traditional ultraviolet light irradiation method preparation, identical among uv photopolymerization monomer and the embodiment, and the mass ratio of nematic liquid crystal and polymerisable monomer is similarly 7: 3, does not contain the thermopolymerization monomer.The electric light curve of PDLC film as can be seen from Fig. 1, compare with the comparative example that adopts traditional single ultraviolet light irradiation method preparation, although the threshold voltage of embodiment and saturation voltage are higher, embodiment has time of response and bigger contrast gradient faster.
From Fig. 2～3 scanning electron microscope pictures as can be seen, adopt the embodiment (sample 1) of ultraviolet light irradiation-heating step-by-step polymerization method preparation to compare with the comparative example (sample 2) that adopts traditional ultraviolet light irradiation method preparation, the mesh of macromolecule network is less among the embodiment.
With the nematic liquid crystal among the embodiment 1, UV-light polymerisable monomer, light trigger, thermopolymerization monomer and nano microsphere uniform mixing, after the uv photopolymerization process identical with embodiment 1, the sample that obtains is put into baking oven, Heating temperature is 90 ℃, be 6 hours heat-up time, sample is cold going to room temperature in air, promptly obtains the PDLC film of embodiment 2.
Embodiment 3
With the nematic liquid crystal among the embodiment 1, UV-light polymerisable monomer, light trigger, thermopolymerization monomer and nano microsphere uniform mixing, after the uv photopolymerization process identical with embodiment 1, the sample that obtains is put into baking oven, Heating temperature is 90 ℃, be 8 hours heat-up time, sample is cold going to room temperature in air, promptly obtains the PDLC film of embodiment 3.
Experimental result shows that the electro-optical properties difference of the PDLC film of preparation is little among the electro-optical properties of the PDLC film of embodiment 2～3 and the embodiment 1.This shows also that in the above-described embodiments after heat polymerization process was heated to 5 hours, the reaction of Resins, epoxy and fatty amine epoxy hardener was finished substantially.
Comparative example
The tri (propylene glycol) diacrylate (TPGDA) that will contain acrylate-functional groups mixes by mass ratio with pentaerythritol triacrylate (PETA) at 2: 1, as the uv photopolymerization monomer.Nematic liquid crystal SLC1717 and above-mentioned UV-light polymerisable monomer are mixed by mass ratio at 7: 3, and at room temperature (20 ℃) form isotropic liquid.Light trigger Irgacure 651 content are 5.0% of monomer total mass.Adding particle diameter is the glass microballon of 20 μ m, the thickness of control pdlc film.The content of glass microballon is about 0.5～1.0% of mixed system total mass.
With being clipped in behind nematic liquid crystal, UV-light polymerisable monomer, light trigger and the nano microsphere uniform mixing in the middle of two nesa coatings that are coated with ITO, even with roll-in, form the thick rete of 20.0 μ m, shine with the UV-light of 365nm down at 0 ℃.Ultraviolet ray intensity is 20.0mW/m
2, light application time is 5.0 minutes, promptly obtains the PDLC film of comparative example.
Compare with embodiment 1～3, do not add the thermopolymerization monomer that contains Resins, epoxy and fatty amine epoxy hardener in the comparative example.Comparative example does not carry out heat treated finish ultraviolet polymerization under ultraviolet light irradiation after.
The electric light curve of PDLC film is shown in Fig. 1 (sample 2) in the comparative example.Scanning electron microscope (SEM) picture of PDLC film macromolecule network as shown in Figure 3 in the comparative example.
In sum, the present invention is by selecting UV-light polymerisable monomer and thermopolymerization monomer, through ultraviolet light irradiation and the step-by-step polymerization crosslinking reaction that adds the above-mentioned polymerization system of thermal initiation, formation has the very macromolecule network of high crosslink density, improve the cross-linking density of PDLC film, thereby improve the electro-optical properties of PDLC film.The electric light curve of PDLC film is compared with the comparative example that adopts single ultraviolet light irradiation method preparation as can be seen from Fig. 1, although the threshold voltage of embodiment and saturation voltage are higher, embodiment has time of response and bigger contrast gradient faster.
Claims (2)
1. UV-light-heating step polymerization prepares the method for polymer dispersion liquid crystal material, be clipped in after it is characterized in that nematic liquid crystal, UV-light polymerisable monomer, light trigger, thermopolymerization monomer and glass microballon mixed in the middle of two nesa coatings that are coated with tin indium oxide, even with roll-in, shine with UV-light, room temperature is reduced in sample heating, insulation back in air, be solidified into pdlc film; The UV-light polymerisable monomer is acrylate, methacrylic ester, styryl, and diacetyl, the quantity of active function groups is 1～5; The thermopolymerization monomer is Resins, epoxy and fatty amine epoxy hardener; Light trigger is benzil dimethyl ketal or benzophenone or sulfo-anthrone.
2. UV-light-heating step polymerization prepares the method for polymer dispersion liquid crystal material according to claim 1, it is characterized in that the making processes step is:
(1) UV-light polymerisable monomer and thermopolymerization monomer are mixed by mass ratio at 1.5: 1 are polymerisable monomer;
(2) with nematic liquid crystal be mixed after polymerisable monomer mix at 7: 3 by mass ratio, form isotropic liquids at 0 ℃～25 ℃;
(3) add light trigger in isotropic liquid and form mixed system, photoinitiator levels is 1.0～5.0% of an isotropic liquid quality;
(4) adding particle diameter to mixed system is the glass microballon of 20 μ m, the thickness of control pdlc film, and the content of glass microballon is 0.5～1.0% of mixed system total mass;
(5) nematic liquid crystal, UV-light polymerisable monomer, light trigger, thermopolymerization monomer and the glass microballon after mixing forms the thick rete of 20 μ m, is that the UV-light of 365nm is shone with wavelength down at 0～25 ℃; The uv photopolymerization temperature is controlled at 0.5～1.0 ℃ of polymerisable monomer/more than the nematic liquid crystal mixed system clearing point by the temperature control platform, and ultraviolet ray intensity is 20.0mW/m
2, light application time is 1～10 minute; Thermopolymerization temperature subsequently is 60～100 ℃, and the heat tracing time is 5～8 hours, finally is solidified into pdlc film.
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Family Cites Families (3)
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| JPH06102490A (en) * | 1992-09-19 | 1994-04-15 | Semiconductor Energy Lab Co Ltd | Production of dispersion type liquid crystal electrooptical device |
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