CN100537705C - A kind of preparation method of polymer dispersed liquid-crystal film - Google Patents
A kind of preparation method of polymer dispersed liquid-crystal film Download PDFInfo
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- CN100537705C CN100537705C CNB2007100261016A CN200710026101A CN100537705C CN 100537705 C CN100537705 C CN 100537705C CN B2007100261016 A CNB2007100261016 A CN B2007100261016A CN 200710026101 A CN200710026101 A CN 200710026101A CN 100537705 C CN100537705 C CN 100537705C
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Abstract
The invention belongs to liquid crystal material uses and association area, be the preparation method of a kind of Polymer Dispersed Liquid Crystal (PDLC) film, with 1,2-two positive alkene butylbenzene acetylides, rigidity bifunctional acrylate's class polymerisable monomer, methyl methacrylate mixed by mass ratio in 8: 2: 3～8: 3: 2, and polymerization single polymerization monomer and the row type liquid crystal of this mixture as polymer dispersed liquid-crystal film mixed by mass ratio in 2: 8～8: 2, at room temperature formed isotropic liquid.To be clipped in behind isotropic liquid, 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 rete, more than the clearing point of isotropic liquid, shine with the UV-light of 365nm in 0.5～3 ℃ and obtain the PDLC film.The present invention can improve the driving voltage of PDLC material, thereby strengthens the stability that polymer network intensity improves PDLC thin-film electro optical property.
Description
Technical field
The invention belongs to field of application of liquid crystal, is a kind of preparation method of polymer dispersed liquid-crystal film specifically.
Background technology
Polymer Dispersed Liquid Crystal (Polymer dispersed liquid crystals is called for short PDLC) film is the compound electrooptical material of a kind of liquid crystal/polymer.The PDLC film can be applicable to electric-controlled light-regulating glass art and flexible liquid crystal screen, by regulating extra electric field the PDLC film is changed between transparent and opaque two states.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.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.
The most key link of PDLC film preparation be how to guarantee pdlc film have the 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.When the preparation dimming glass was used pdlc film, the driving voltage that reduces pdlc film was even more important.Because at present in the world dimming glass with the driving voltage of pdlc film more than 36 volts, the driving voltage of the product of for example Japanese plate pin company is about 110 volts.The preparation driving voltage has important academic significance and vast market potentiality at the dimming glass pdlc film of safety voltage below 36 volts.The electro-optical 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 PDLC film preparation process, it is not enough and make the electro-optical properties stability of PDLC film not reach the phenomenon of application requiring also the macromolecule network mechanical strength to occur through regular meeting.
Summary of the invention
The objective of the invention is to propose a kind of preparation method with the stable PDLC film of low driving voltage, polymer network intensity height, electro-optical properties.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of polymer dispersed liquid-crystal film, carry out according to the following steps:
1. press mass ratio with 1,2-two positive alkene butylbenzene acetylides, rigidity bifunctional acrylate's class polymerisable monomer, methyl methacrylate mixes by 8:2:3～8:3:2, and with the polymerization single polymerization monomer of this mixture as polymer dispersed liquid-crystal film;
2. with nematic liquid crystal and step 1. the polymerization single polymerization monomer of gained to press mass ratio 2:8～8:2 mixed even, at room temperature form isotropic liquid;
3. 2. light trigger, glass microballon and step are clipped in behind the gained isotropic liquid uniform mixing in two transparent indium tin oxide-coated glasses or the transparent tin indium oxide conductive plastic film, press evenly, form rete;
4. at a certain temperature, temperature is controlled at above 0.5～3.0 ℃ of the clearing point of isotropic liquid, with 3. gained rete 1～5 minute of ultraviolet irradiation step, makes rete be solidified into polymer dispersed liquid-crystal film.
Purpose of the present invention can also further realize by following technical measures:
The formulation method of aforesaid polymer dispersed liquid-crystal film, wherein said step 1. in, 1, the chemical structure of 2-two positive alkene butylbenzene acetylides is:
The preparation method of aforesaid polymer dispersed liquid-crystal film, wherein said step 1. in, the chemical structure of rigidity bifunctional acrylate's class polymerisable monomer is:
The preparation method of aforesaid polymer dispersed liquid-crystal film, wherein said step 3. in, photoinitiator levels is 1%～5.0% of an isotropic liquid total mass.
The preparation method of aforesaid polymer dispersed liquid-crystal film, wherein said step 3. in, the glass microballon particle diameter is 15～20 μ m, content is 0.5～1.0% of Polymer Dispersed Liquid Crystal polymerization single polymerization monomer total mass.
The preparation method of aforesaid polymer dispersed liquid-crystal film, wherein said step 3. in, thicknesses of layers is 15～20.0 μ m.
The preparation method of aforesaid polymer dispersed liquid-crystal film, wherein said step 4. in, shine with the UV-light of 365nm, ultraviolet ray intensity is 20.0～60.0mW/m
2
The preparation method of aforesaid polymer dispersed liquid-crystal film, wherein said step 4. in, temperature is-10～+ 30 ℃.
Advantage of the present invention is: 1. owing to 1, after 2-two positive alkene butylbenzene acetylides have liquid crystal liquid crystal property and liquid crystal material blend, can not have a strong impact on the clearing point of mixture, be easy to the clearing point of liquid crystal material; 2. because 1,2-two positive alkene butylbenzene acetylide viscosity are lower, molecule does not have polarity, help that molecule spreads in photopolymerization reaction, so the mesh of macromolecule network greatly in the prepared PDLC film, driving voltage is lower; 3. 1, contain two phenyl ring in the molecule of 2-two positive alkene butylbenzene acetylides, the mechanical strength height of prepared macromolecule network, shrinkability are little, help forming stable macromolecule network, thereby can prepare the stable PDLC film of electro-optical properties.Therefore, the present invention uses 1, and 2-two positive alkene butylbenzene acetylides can prepare and have low driving voltage (36 volts following) and the stable PDLC film of electro-optical properties.
Description of drawings
Fig. 1 is the electro-optical properties curve of the embodiment of the invention two and comparative example one.
Fig. 2 is PDLC macromolecule network scanning electron microscope (SEM) photo of the embodiment of the invention two.
Fig. 3 is PDLC macromolecule network scanning electron microscope (SEM) photo of comparative example one.
Fig. 4 be the embodiment of the invention two with the OFF state transmitance of comparative example one with the incident wavelength change curve.
Embodiment
Embodiment one
Present embodiment is the preparation method of a kind of low driving voltage, high-contrast PDLC film, carries out according to the following steps:
(1) with 1,2-two positive alkene butylbenzene acetylides, rigidity bifunctional acrylate's class polymerisable monomer, methyl methacrylate mixes by mass ratio 8:2:3, and with this mixed system as polymerization single polymerization monomer.1, the chemical structure of 2-two positive alkene butylbenzene acetylene is:
The chemical structure of rigidity bifunctional acrylate's class polymerisable monomer is:
(2) polymerization single polymerization monomer with nematic liquid crystal and Polymer Dispersed Liquid Crystal mixes by mass ratio at 2: 8, and at room temperature (0.5 ℃) forms isotropic liquid, and the nematic liquid crystal of selecting for use is SLC7011-100 (Shijiazhuang Yongshenghuaqing Liquid Crystal Co., Ltd).
(3) will be clipped in behind light trigger, glass microballon and the isotropic liquid uniform mixing in two transparent indium tin oxide-coated glasses or the transparent tin indium oxide conductive plastic film, press evenly, form the thick rete of 15 μ m.Light trigger is Irgacure 651 (Tokyo changes into company), and content is 1.0% of isotropic liquid total mass.The glass microballon particle diameter is 15 μ m, control pdlc film thickness, the content of glass microballon be about Polymer Dispersed Liquid Crystal the polymerization single polymerization monomer total mass 0.5%.
(4) at-10 ℃ of UV-irradiation retes of using 365nm down, ultraviolet ray intensity is 60.0mW/m
2, light application time is 1 minute, obtains the PDLC film, promptly gets required automatically controlled intelligent glass material with the pdlc film that makes and glass are compound then.Ultraviolet ray intensity can be regulated by the distance of regulating ultraviolet lamp and sample, thus control pdlc film rate of polymerization.Polymerization temperature is controlled at 0.5～3.0 ℃ of polymerisable monomer/more than the nematic liquid crystal mixed system clearing point by the temperature control platform, 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.
Embodiment two
Present embodiment is the preparation method of a kind of low driving voltage, high-contrast PDLC film, carries out according to the following steps:
(1) with 1,2-two positive alkene butylbenzene acetylides, rigidity bifunctional acrylate's class polymerisable monomer, methyl methacrylate mix by mass ratio 8:3:2, and with this mixed system as polymerization single polymerization monomer.
(2) polymerization single polymerization monomer with nematic liquid crystal and Polymer Dispersed Liquid Crystal mixes by mass ratio 6:4, and at room temperature (0.5 ℃) forms isotropic liquid, and the nematic liquid crystal of selecting for use is SLC7011-100 (Shijiazhuang Yongshenghuaqing Liquid Crystal Co., Ltd).
(3) will be clipped in behind light trigger, glass microballon and the isotropic liquid uniform mixing in two transparent indium tin oxide-coated glasses or the transparent tin indium oxide conductive plastic film, press evenly, form the thick rete of 18 μ m.Light trigger is Irgacure 651 (Tokyo changes into company), and content is 2.5% of isotropic liquid total mass.The glass microballon particle diameter is 18 μ m, control pdlc film thickness, the content of glass microballon be about Polymer Dispersed Liquid Crystal the polymerization single polymerization monomer total mass 0.8%.
(4) at 0 ℃ of UV-irradiation rete of using 365nm down, ultraviolet ray intensity is 40.0mW/m
2, light application time is 3.0 minutes, obtains the PDLC film, promptly gets required automatically controlled intelligent glass material with the pdlc film that makes and glass are compound then.Ultraviolet ray intensity can be regulated by the distance of regulating ultraviolet lamp and sample, thus control pdlc film rate of polymerization.Polymerization temperature is controlled at 0.5～3.0 ℃ of polymerisable monomer/more than the nematic liquid crystal mixed system clearing point by the temperature control platform, 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.
Embodiment three
Present embodiment is the preparation method of a kind of low driving voltage, high-contrast PDLC film, carries out according to the following steps:
(1) with 1,2-two positive alkene butylbenzene acetylides, rigidity bifunctional acrylate's class polymerisable monomer, methyl methacrylate mix by mass ratio 8:3:2, and with this mixed system as polymerization single polymerization monomer.
(2) polymerization single polymerization monomer with nematic liquid crystal and Polymer Dispersed Liquid Crystal mixes by mass ratio 8:2, and at room temperature (0.5 ℃) forms isotropic liquid, and the nematic liquid crystal of selecting for use is SLC7011-100 (Shijiazhuang Yongshenghuaqing Liquid Crystal Co., Ltd).
(3) will be clipped in behind light trigger, glass microballon and the isotropic liquid uniform mixing in two transparent indium tin oxide-coated glasses or the transparent tin indium oxide conductive plastic film, press evenly, form the thick rete of 20 μ m.Light trigger is Irgacure 651 (Tokyo changes into company), and content is 5% of isotropic liquid total mass.The glass microballon particle diameter is 20 μ m, control pdlc film thickness, the content of glass microballon be about Polymer Dispersed Liquid Crystal the polymerization single polymerization monomer total mass 1%.
(4) at 30 ℃ of UV-irradiation retes of using 365nm down, ultraviolet ray intensity is 20.0mW/m
2, light application time is 5 minutes, obtains the PDLC film, promptly gets required automatically controlled intelligent glass material with the pdlc film that makes and glass are compound then.Ultraviolet ray intensity can be regulated by the distance of regulating ultraviolet lamp and sample, thus control pdlc film rate of polymerization.Polymerization temperature is controlled at 0.5～3.0 ℃ of polymerisable monomer/more than the nematic liquid crystal mixed system clearing point by the temperature control platform, 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.
The electric light curve of PDLC film that records embodiment two with the liquid crystal comprehensive parameter tester is shown in Fig. 1 (Sample 1), and ordinate is a transmitance among the figure, and abscissa is for applying voltage.Scanning electron microscope (SEM) picture of the PDLC film macromolecule network of embodiment two as shown in Figure 2.Shown in Fig. 4 (Sample 1), ordinate is a transmitance to the OFF state transmitance of the PDLC film of embodiment two among the figure with the incident wavelength change curve, and abscissa is a wavelength.
Comparative example one
Present embodiment is that 8:5 mix with rigidity bifunctional acrylate class polymerisable monomer and methyl methacrylate by mass ratio as the comparative example of embodiment two, and with this mixed system as polymerization single polymerization monomer.Selecting nematic liquid crystal for use is SLC7011-100 (Shijiazhuang Yongshenghuaqing Liquid Crystal Co., Ltd).Nematic liquid crystal and the above-mentioned polymerisable monomer that is mixed are mixed by mass ratio 6:4, and at room temperature (2.3 ℃) 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.With being clipped in behind nematic liquid crystal, 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 certain 3.0 ℃.Ultraviolet ray intensity is 20.0mW/m
2, light application time is 5.0 minutes, obtains the PDLC film, promptly gets required automatically controlled intelligent glass material with the pdlc film that makes and glass are compound then.
The electric light curve of PDLC film is shown in Fig. 1 (Sample 2) in the comparative example, and ordinate is a transmitance among the figure, and abscissa is for applying voltage.Scanning electron microscope (SEM) picture of PDLC film macromolecule network as shown in Figure 3.Shown in Fig. 4 (Sample 2), ordinate is a transmitance to the OFF state transmitance of PDLC film among the figure with the incident wavelength change curve, and abscissa is a wavelength.
As can be seen, and do not contain 1 from Fig. 1 curve, the comparative example of 2-two positive alkene butylbenzene acetylides is compared, and contains 1, and the embodiment of 2-two positive alkene butylbenzene acetylides has lower threshold voltage and saturation voltage, and driven saturated voltage is less than 36 volts.
Verified by weathering test simultaneously, adopt the PDLC film of methyl methacrylate/SLC7011-100 system preparation, after the electric field switch 2000 times, contrast gradient has descended 37%.And adopting the PDLC film of embodiment and the preparation of comparative example system, after the electric field switch 10000 times, contrast gradient is declined by less than 2%.Therefore from the angle of electro-optical properties stability, both contained 1,2-two positive alkene butylbenzene acetylides contain rigidity bifunctional acrylate class polymerisable monomer again, contain the PDLC film of rigidity bifunctional acrylate class polymerisable monomer system preparation, have good electro-optical properties stability.
From reducing the angle of driven saturated voltage, both contained 1, the PDLC film that 2-two positive alkene butylbenzene acetylides contain the preparation of rigidity bifunctional acrylate class polymerisable monomer system again has lower driving voltage.But the system that does not contain rigidity bifunctional acrylate class polymerisable monomer is difficult to carry out polymerization under UV-irradiation, therefore ideal PDLC film is both to have contained 1, and 2-two positive alkene butylbenzene acetylides contain the PDLC film of rigidity bifunctional acrylate class polymerisable monomer system preparation again.
From the scanning electron microscope picture of Fig. 2 and Fig. 3 as can be seen, embodiment is bigger than the mesh of the macromolecule network of comparative example, so embodiment has lower driving voltage
As can be seen, embodiment compares with comparative example from Fig. 4 curve, and the OFF state transmitance of embodiment in visible wavelength range is higher.
Claims (7)
1. the preparation method of a polymer dispersed liquid-crystal film is characterized in that: carry out according to the following steps:
1. press mass ratio with 1,2-two positive alkene butylbenzene acetylides, rigidity bifunctional acrylate's class polymerisable monomer, methyl methacrylate mixes by 8:2:3～8:3:2, and with the polymerization single polymerization monomer of this mixture as polymer dispersed liquid-crystal film, 1, the chemical structure of 2-two positive alkene butylbenzene acetylides is:
2. with nematic liquid crystal and step 1. the polymerization single polymerization monomer of gained to press mass ratio 2:8～8:2 mixed even, at room temperature form isotropic liquid;
3. 2. light trigger, glass microballon and step are clipped in behind the gained isotropic liquid uniform mixing in two transparent indium tin oxide-coated glasses or the transparent tin indium oxide conductive plastic film, press evenly, form rete;
4. at a certain temperature, temperature is controlled at above 0.5～3.0 ℃ of the clearing point of isotropic liquid, with 3. gained rete 1～5 minute of ultraviolet irradiation step, makes rete be solidified into polymer dispersed liquid-crystal film.
2. the preparation method of polymer dispersed liquid-crystal film as claimed in claim 1 is characterized in that: described step 1. in, the chemical structure of rigidity bifunctional acrylate's class polymerisable monomer is:
3. the preparation method of polymer dispersed liquid-crystal film as claimed in claim 1 is characterized in that: described step 3. in, photoinitiator levels is 1%～5.0% of an isotropic liquid total mass.
4. the preparation method of polymer dispersed liquid-crystal film as claimed in claim 1 is characterized in that: described step 3. in, the glass microballon particle diameter is 15～20 μ m, content is 0.5～1.0% of Polymer Dispersed Liquid Crystal polymerization single polymerization monomer total mass.
5. the preparation method of polymer dispersed liquid-crystal film as claimed in claim 1 is characterized in that: described step 3. in, thicknesses of layers is 15～20.0 μ m.
6. the preparation method of polymer dispersed liquid-crystal film as claimed in claim 1 is characterized in that: described step 4. in, shine with the UV-light of 365nm, ultraviolet ray intensity is 20.0～60.0mW/m
2
7. the preparation method of polymer dispersed liquid-crystal film as claimed in claim 1 is characterized in that: described step 4. in, described certain temperature is-10～+ 30 ℃.
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Cited By (1)
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|---|---|---|---|---|
| EP2864444B1 (en) * | 2012-06-26 | 2018-08-01 | Merck Patent GmbH | Method of preparing a birefringent polymer film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2864444B1 (en) * | 2012-06-26 | 2018-08-01 | Merck Patent GmbH | Method of preparing a birefringent polymer film |
| US10100253B2 (en) | 2012-06-26 | 2018-10-16 | Merck Patent Gmbh | Method of preparing a birefringent polymer film |
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