CN102053417A - Polymer dispersed liquid crystal three steady-state membrane and preparation method thereof - Google Patents
Polymer dispersed liquid crystal three steady-state membrane and preparation method thereofDownload PDFInfo
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Abstract
Translated fromChineseDescription
Translated fromChinese技术领域technical field
本发明涉及一种聚合物分散液晶膜，尤其是涉及一种聚合物分散液晶三稳态膜及其制备方法。The invention relates to a polymer dispersed liquid crystal film, in particular to a polymer dispersed liquid crystal tristable film and a preparation method thereof.
背景技术Background technique
聚合物分散液晶(Polymer Dispersed Liquid Crystal，PDLC)是把聚合物与向列相(nematic)液晶及衬垫料以某个比例混合起来，夹在两片柔性透明导电薄膜之间，经过相分离，向列相液晶从聚合物中析出形成液晶微滴，聚合物固化把液晶微滴包裹在其中，形成的一种复合膜。复合膜不加电场时，由于聚合物的折射率与向列相液晶的折射率不匹配，因此会造成光散射，复合膜对光是关态；复合膜当施加电场后，聚合物的折射率与向列相液晶的折射率相匹配，造成光透射，复合膜对光是开态；该复合膜具有的散射关态和透射开态，这两个稳态都零场稳定，该复合膜也有反式工作模式，不加电场时透明，加电场时反而散射。PDLC膜是20世纪80年代发明的高科技产品，已经作为调光玻璃在高档建筑装修领域获得越来越多的应用，并且在大屏幕显示、全息光栅、电子纸等许多领域具有应用价值，现在也还是液晶器件研究者关注的热门课题。胆甾相液晶双稳态(Bistable State of Cholesteric Liquid Crystal)是胆甾相液晶的平面态具有可见光布拉格选择反射亮态和焦锥态为散射暗态，这两个态能零场稳定，是应用在电子纸上的一种技术。在对PDLC膜的研究中，人们也已经获得了聚合物分散胆甾相液晶(PolymerDispersed Cholesteric Liquid Crystal，PDCLC)双稳态膜，其具有布拉格反射关态和透射开态，布拉格选择反射波长调节在可见光波段，不是在红外光波段，因此对红外光是吸收和透射的，不能起到可转换的节能窗功能。胆甾相液晶可以是由胆甾醇的酯和卤化物形成的液晶，也可以是由手性向列相形成的液晶。手性分子是如果将其分割成两半，它的一半与另一半都不会重叠，也就是这两半不能互成镜像关系，就说它有手性，具有这种性质的分子就叫手性分子，含有手性分子的液晶就叫手性液晶，手性液晶(胆甾相液晶)具有旋光性、布拉格选择反射等光学特性。双频液晶(Dual-frequency liquidcrystal)是介电转换液晶，在低频电压驱动下呈现为正性液晶(Δε＝ε||-ε⊥＞0)，施加电场后液晶分子平行于电场方向排列，而在高频电压驱动下呈现为负性液晶(Δε＝ε||-ε⊥＜0)，施加电场后液晶分子垂直于电场方向排列。手性双频液晶即聚合物手性双频液晶，其是在双频液晶中添加手性剂配制出的具有介电转换性质的胆甾相液晶。Polymer Dispersed Liquid Crystal (PDLC) is a mixture of polymers, nematic liquid crystals and spacers in a certain ratio, sandwiched between two flexible transparent conductive films, and undergoes phase separation. Nematic liquid crystals are precipitated from the polymer to form liquid crystal droplets, and the polymer solidifies to wrap the liquid crystal droplets in it to form a composite film. When no electric field is applied to the composite film, since the refractive index of the polymer does not match the refractive index of the nematic liquid crystal, it will cause light scattering, and the composite film is off to light; when the composite film is applied with an electric field, the refractive index of the polymer Matching the refractive index of the nematic liquid crystal, resulting in light transmission, the composite film is in an open state for light; the composite film has a scattering off state and a transmission on state, and these two stable states are zero-field stable, and the composite film also has Trans-working mode, transparent when no electric field is applied, but scattered when electric field is applied. PDLC film is a high-tech product invented in the 1980s. It has been used more and more in the field of high-end building decoration as a switchable glass, and has application value in many fields such as large-screen display, holographic grating, and electronic paper. Now It is also a hot topic for researchers of liquid crystal devices. Bistable State of Cholesteric Liquid Crystal (Bistable State of Cholesteric Liquid Crystal) is a planar state of cholesteric liquid crystal with visible light Bragg selective reflection bright state and focal conic state as scattering dark state. A technology on electronic paper. In the research on PDLC film, people have also obtained polymer dispersed cholesteric liquid crystal (PolymerDispersed Cholesteric Liquid Crystal, PDCLC) bistable film, which has Bragg reflection off state and transmission on state, Bragg selective reflection wavelength adjustment in The visible light band is not in the infrared light band, so it absorbs and transmits infrared light, and cannot function as a switchable energy-saving window. The cholesteric liquid crystal may bea liquid crystal formed of a cholesteryl ester and a halide, or may be a liquid crystal formed of a chiral nematic phase. A chiral molecule is that if it is divided into two halves, one half of it will not overlap with the other half, that is, the two halves cannot be mirror images of each other, so it is said to have chirality, and a molecule with this property is called a chiral molecule. Liquid crystals containing chiral molecules are called chiral liquid crystals. Chiral liquid crystals (cholesteric liquid crystals) have optical properties such as optical activity and Bragg selective reflection. Dual-frequency liquid crystal (Dual-frequency liquid crystal) is a dielectric switching liquid crystal, which appears as a positive liquid crystal (Δε=ε|| -ε⊥ >0) under the drive of a low-frequency voltage. After an electric field is applied, the liquid crystal molecules are aligned parallel to the direction of the electric field, while Driven by high-frequency voltage, it appears as negative liquid crystal (Δε=ε|| -ε⊥ <0), and the liquid crystal molecules are arranged perpendicular to the direction of the electric field after the electric field is applied. Chiral dual-frequency liquid crystals are polymer chiral dual-frequency liquid crystals, which are cholesteric liquid crystals with dielectric conversion properties prepared by adding chiral agents to dual-frequency liquid crystals.
发明内容Contents of the invention
本发明所要解决的技术问题是提供一种具有散射关态、半透明开态和可见光散射加红外光布拉格反射关态三种稳态的聚合物分散液晶三稳态膜及其制备方法。The technical problem to be solved by the present invention is to provide a polymer-dispersed liquid crystal tristable film with three stable states of scattering off state, translucent on state and visible light scattering plus infrared Bragg reflection off state and its preparation method.
本发明解决上述技术问题所采用的技术方案为：一种聚合物分散液晶三稳态膜，其特征在于包括两层柔性透明导电薄膜和设置于所述的柔性透明导电薄膜之间的聚合物分散液晶层，所述的柔性透明导电薄膜的内侧表面上设置有透明导电薄层电极，所述的聚合物分散液晶层主要是由预聚物、手性双频液晶材料和衬垫材料充分搅拌均匀混合制成。The technical solution adopted by the present invention to solve the above-mentioned technical problems is: a polymer dispersed liquid crystal tristable film, which is characterized in that it includes two layers of flexible transparent conductive films and a polymer dispersed film arranged between the flexible transparent conductive films. Liquid crystal layer, the inner surface of the flexible transparent conductive film is provided with a transparent conductive thin-layer electrode, and the polymer dispersed liquid crystal layer is mainly composed of a prepolymer, a chiral dual-frequency liquid crystal material and a gasket material and fully stirred evenly Mix made.
所述的聚合物分散液晶层的厚度为30μm，所述的预聚物和所述的手性双频液晶材料的重量比为1∶(1～3)，所述的衬垫材料在所述的聚合物分散液晶层中的含量为1～10个/mm2。The thickness of the polymer-dispersed liquid crystal layer is 30 μm, the weight ratio of the prepolymer and the chiral dual-frequency liquid crystal material is 1: (1-3), and the gasket material is in the The content of the polymer dispersed liquid crystal layer is 1-10/mm2 .
所述的预聚物主要由可聚合单体、链转移剂和光引发剂组成，各组分的重量百分比为：可聚合单体丙氧基壬苯基丙烯酸酯为15～25％、可聚合单体三羟甲基丙烷三丙烯酸酯为65～75％、链转移剂癸二酸为3～5％、光引发剂1173为3～5％。The prepolymer is mainly composed of polymerizable monomers, chain transfer agents and photoinitiators, and the weight percentage of each component is: Bulk trimethylolpropane triacrylate is 65-75%, chain transfer agent sebacic acid is 3-5%, and photoinitiator 1173 is 3-5%.
所述的可聚合单体、所述的链转移剂和所述的光引发剂的重量百分比为：可聚合单体丙氧基壬苯基丙烯酸酯为20％、可聚合单体三羟甲基丙烷三丙烯酸酯为70％、链转移剂癸二酸为5％、光引发剂1173为5％。The weight percentages of the described polymerizable monomer, the described chain transfer agent and the described photoinitiator are: 20% of the polymerizable monomer propoxy nonyl phenyl acrylate, 20% of the polymerizable monomer trimethylol Propane triacrylate was 70%, chain transfer agent sebacic acid was 5%, photoinitiator 1173 was 5%.
所述的手性双频液晶材料主要是由S811液晶手性添加剂和双频液晶配制而成，所述的S811液晶手性添加剂和所述的双频液晶的质量比为1∶9；所述的双频液晶为由质量百分比为20％的MBBA液晶和质量百分比为80％的DT91液晶配制成的混合物。The chiral dual-frequency liquid crystal material is mainly prepared from S811 liquid crystal chiral additive and dual-frequency liquid crystal, and the mass ratio of the S811 liquid crystal chiral additive to the dual-frequency liquid crystal is 1:9; The dual-frequency liquid crystal is a mixture prepared by MBBA liquid crystal with a mass percentage of 20% and DT91 liquid crystal with a mass percentage of 80%.
所述的手性双频液晶材料的螺距为0.5～2μm，所述的手性双频液晶材料的布拉格反射光波长为0.75～3μm。The helical pitch of the chiral dual-frequency liquid crystal material is 0.5-2 μm, and the wavelength of the Bragg reflected light of the chiral dual-frequency liquid crystal material is 0.75-3 μm.
所述的衬垫材料为直径为30μm的塑料微球。The gasket material is plastic microspheres with a diameter of 30 μm.
所述的聚合物分散液晶层中聚合物的折射率、液晶寻常光的折射率、液晶非常光的折射率分别为1.5～1.55、1.5～1.55、1.7～1.75。The refractive index of the polymer in the polymer-dispersed liquid crystal layer, the ordinary optical refractive index of the liquid crystal, and the extraordinary optical refractive index of the liquid crystal are respectively 1.5-1.55, 1.5-1.55, and 1.7-1.75.
一种聚合物分散液晶三稳态膜的制备方法，其特征在于包括以下步骤：A preparation method of a polymer dispersed liquid crystal tristable film is characterized in that it comprises the following steps:
①按重量比1∶(1～3)称取预聚物和手性双频液晶材料，并以1～10个/mm2的含量加入衬垫材料，在常温下对预聚物、手性双频液晶材料和衬垫材料进行充分搅拌均匀混合；①Weigh the prepolymer and chiral dual-frequency liquid crystal material according to the weight ratio of 1: (1~3), and add the gasket material at a content of 1~10 pieces/mm2 . The dual-frequency liquid crystal material and the gasket material are fully stirred and evenly mixed;
所述的预聚物主要由可聚合单体、链转移剂和光引发剂组成，各组分的重量百分比为：可聚合单体丙氧基壬苯基丙烯酸酯为15～25％、可聚合单体三羟甲基丙烷三丙烯酸酯为65～75％、链转移剂癸二酸为3～5％、光引发剂1173为3～5％；The prepolymer is mainly composed of polymerizable monomers, chain transfer agents and photoinitiators, and the weight percentage of each component is: Bulk trimethylolpropane triacrylate is 65-75%, chain transfer agent sebacic acid is 3-5%, photoinitiator 1173 is 3-5%;
所述的手性双频液晶材料主要是由S811液晶手性添加剂和双频液晶配制而成，所述的S811液晶手性添加剂和所述的双频液晶的质量比为1∶9；所述的双频液晶为由质量百分比为20％的MBBA液晶和质量百分比为80％的DT91液晶配制成的混合物；The chiral dual-frequency liquid crystal material is mainly prepared from S811 liquid crystal chiral additive and dual-frequency liquid crystal, and the mass ratio of the S811 liquid crystal chiral additive to the dual-frequency liquid crystal is 1:9; The dual-frequency liquid crystal is a mixture prepared by MBBA liquid crystal with a mass percentage of 20% and DT91 liquid crystal with a mass percentage of 80%;
②分别在两层柔性透明导电薄膜的内侧表面上刻蚀出透明导电薄层电极；② Etch transparent conductive thin-layer electrodes on the inner surfaces of the two flexible transparent conductive films;
③将均匀混合好的混合物转印刷到两层柔性透明导电薄膜之间；③The uniformly mixed mixture is transferred and printed between two layers of flexible transparent conductive films;
④利用压合机将印刷有混合物的两层柔性透明导电薄膜挤压成复合膜；④Extrude the two-layer flexible transparent conductive film printed with the mixture into a composite film by using a laminating machine;
⑤对复合膜进行分离，使液晶从聚合物中充分析出，形成平均直径为3～5μm的液晶微滴，同时固化液晶微滴。⑤ Separating the composite film to fully separate the liquid crystal from the polymer to form liquid crystal droplets with an average diameter of 3-5 μm, and solidify the liquid crystal droplets at the same time.
所述的聚合物分散液晶三稳态膜具有散射关态、半透明开态和可见光散射加红外光布拉格反射关态三种稳态，当在透明导电薄层电极之间施加低频或直流电场，然后快速撤掉低频或直流电场后，聚合物分散液晶三稳态膜呈现散射关态；当在透明导电薄层电极之间施加低频或直流电场，然后以阶梯降电压方式撤掉低频或直流电场后，聚合物分散液晶三稳态膜呈现半透明开态；当在透明导电薄层电极之间施加高频电场，然后以阶梯降电压方式撤掉低频或直流电场后，聚合物分散液晶三稳态膜呈现可见光散射加红外光布拉格反射关态。The polymer-dispersed liquid crystal tristable film has three stable states: scattering off state, translucent on state and visible light scattering plus infrared Bragg reflection off state. When a low-frequency or DC electric field is applied between transparent conductive thin-layer electrodes, Then quickly remove the low-frequency or DC electric field, the polymer-dispersed liquid crystal tristable film exhibits a scattering off state; when a low-frequency or DC electric field is applied between the transparent conductive thin-layer electrodes, then the low-frequency or DC electric field is removed in a step-down voltage manner After that, the polymer-dispersed liquid crystal tristable film presents a translucent open state; when a high-frequency electric field is applied between the transparent conductive thin-layer electrodes, and then the low-frequency or DC electric field is removed in a step-down manner, the polymer-dispersed liquid crystal tristable film The state film presents the off state of visible light scattering and infrared light Bragg reflection.
与现有技术相比，本发明的优点在于利用预聚物、手性双频液晶材料和衬垫材料，通过充分搅拌均匀混合制成聚合物分散液晶层，使用这种聚合物分散液晶层制成的聚合物分散液晶膜具有散射关态、半透明开态和可见光散射加红外光布拉格反射关态三种稳态。Compared with the prior art, the present invention has the advantage of utilizing the prepolymer, chiral dual-frequency liquid crystal material and gasket material to form a polymer-dispersed liquid crystal layer through sufficient stirring and uniform mixing, and using this polymer-dispersed liquid crystal layer to make The polymer-dispersed liquid crystal film has three stable states: scattering off state, translucent on state and visible light scattering plus infrared Bragg reflection off state.
本发明的聚合物分散液晶三稳态膜在胆甾相液晶盒中，对于绿光波长的透光率T小畴＜40％，T大畴＞75％，大液晶微滴的PDCLC盒中T小畴＜10％，T大畴～50％，而焦锥态小畴和大畴是两个不同的稳定态，加上平面态也是稳定态，所以构成了三稳态。The polymer-dispersed liquid crystal tristable film of the present invention is in a cholesteric liquid crystal cell, for the light transmittance Tsmall domain of green light wavelength<40%, Tlarge domain >75%, in the PDCLC cell of large liquid crystal droplet TSmall domains < 10%, Tlarge domains ~ 50%, and focal conic small domains and large domains are two different stable states, plus the planar state is also a stable state, so it constitutes a tristable state.
本发明的聚合物分散液晶三稳态膜具有三种稳态，即：焦锥态小畴散射关态、焦锥态大畴半透明开态、平面态大畴可见光散射和红外光反射关态，将本发明应用于节能窗领域时，驱动到焦锥态大畴实现半透明开态；冬天里驱动到焦锥态小畴实现散射关态，又能有红外光透射；夏天里驱动到平面态大畴实现可见光散射关态，又能有红外光反射，尽管太阳辐射的波长范围很宽，但绝大部分能量集中在0.22～4μm的波段，占总能量的99％，可见光占43％，红外光占48.3％，紫外光占8.7％，红外光有显著的热效应，在节能窗上夏天把部分红外光发射掉，就减少了红外光透射，达到给室内降温的目的，冬天再让红外光进入室内，就增加了红外光透射，又达到给室内升温的目的。The polymer-dispersed liquid crystal tristable film of the present invention has three stable states, namely: focal conic state small domain scattering off state, focal conic state large domain translucent on state, planar state large domain visible light scattering and infrared light reflection off state , when the present invention is applied to the field of energy-saving windows, it can be driven to the focal conic state large domain to realize the translucent open state; it can be driven to the focal conic state small domain to realize the scattering off state in winter, and infrared light can be transmitted; it can be driven to the flat surface in summer The large domain of the state realizes visible light scattering and off state, and can also reflect infrared light. Although the wavelength range of solar radiation is very wide, most of the energy is concentrated in the 0.22-4μm band, accounting for 99% of the total energy, and visible light accounts for 43%. Infrared light accounts for 48.3%, and ultraviolet light accounts for 8.7%. Infrared light has a significant thermal effect. In summer, part of the infrared light is emitted from the energy-saving window, which reduces the transmission of infrared light and achieves the purpose of cooling the room. In winter, the infrared light When entering the room, the transmission of infrared light is increased, and the purpose of heating the room is achieved.
附图说明Description of drawings
图1为本发明的聚合物分散液晶三稳态膜的结构示意图；Fig. 1 is the structural representation of polymer dispersed liquid crystal tristable film of the present invention;
图2a为在电极之间施加约25伏的低频电场后液晶分子转向电场方向初始排列状态示意图；Figure 2a is a schematic diagram of the initial arrangement state of liquid crystal molecules turning to the direction of the electric field after applying a low-frequency electric field of about 25 volts between the electrodes;
图2b为本发明的聚合物分散液晶三稳态膜呈现的散射关态示意图；Fig. 2b is a schematic diagram of the scattering off state presented by the polymer-dispersed liquid crystal tristable film of the present invention;
图2c为本发明的聚合物分散液晶三稳态膜呈现的半透明开态示意图；Figure 2c is a schematic diagram of the translucent open state presented by the polymer-dispersed liquid crystal tristable film of the present invention;
图2d为在电极之间施加高频电场后液晶被驱动到场致向列相沿膜面排列态示意图；Figure 2d is a schematic diagram of liquid crystals being driven to the field-induced nematic phase alignment state along the film surface after applying a high-frequency electric field between the electrodes;
图2e为本发明的聚合物分散液晶三稳态膜呈现的散射加布拉格反射关态示意图。Fig. 2e is a schematic diagram of the off-state of scattering plus Bragg reflection presented by the polymer-dispersed liquid crystal tristable film of the present invention.
具体实施方式Detailed ways
以下结合附图实施例对本发明作进一步详细描述。The present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments.
实施例一：Embodiment one:
一种聚合物分散液晶三稳态膜，如图1所示，其包括两层柔性透明导电薄膜101、105和设置于两层柔性透明导电薄膜101、105之间的聚合物分散液晶层103，柔性透明导电薄膜101的内侧表面上设置有透明导电薄层电极102，柔性透明导电薄膜105的内侧表面上设置有透明导电薄层电极104，聚合物分散液晶层103的厚度为30μm，聚合物分散液晶层103中的液晶微滴106的平均直径为3～5μm；聚合物分散液晶层103主要是由预聚物、手性双频液晶材料和衬垫材料充分搅拌均匀混合制成，预聚物和手性双频液晶材料的重量比为1∶(1～3)，衬垫材料在聚合物分散液晶层中的含量为1～10个/mm2，预聚物、手性双频液晶材料和衬垫材料具体可根据实际情况配比。本发明的聚合物分散液晶层的厚度取30μm，是为了有更好的散射态，这是因为液晶微滴大散射次数少，增加聚合物分散液晶层的厚度就可以增加光传播路径上遇到的液晶微滴的个数，也就增加了散射次数。A kind of polymer dispersed liquid crystal tristable film, as shown in Figure 1, it comprises two layers of flexible transparent conductive films 101,105 and the polymer dispersed
在此具体实施例中，预聚物主要由可聚合单体、链转移剂和光引发剂组成，各组分的重量百分比为：可聚合单体丙氧基壬苯基丙烯酸酯为15～25％、可聚合单体三羟甲基丙烷三丙烯酸酯为65～75％、链转移剂癸二酸为3～5％、光引发剂1173(C10H12O2，2-羟基-2-甲基-1-苯丙酮)为3～5％。在实际配比时可按可聚合单体丙氧基壬苯基丙烯酸酯为20％、可聚合单体三羟甲基丙烷三丙烯酸酯为70％、链转移剂癸二酸为5％、光引发剂1173为5％的比例进行配比。In this specific embodiment, the prepolymer is mainly composed of polymerizable monomers, chain transfer agents and photoinitiators, and the weight percentage of each component is: the polymerizable monomer propoxy nonyl phenyl acrylate is 15% to 25% , the polymerizable monomer trimethylolpropane triacrylate is 65-75%, the chain transfer agent sebacic acid is 3-5%, the photoinitiator 1173 (C10 H12 O2 , 2-hydroxy-2-methyl Base-1-propiophenone) is 3 to 5%. In the actual proportioning, the polymerizable monomer propoxy nonyl phenyl acrylate is 20%, the polymerizable monomer trimethylolpropane triacrylate is 70%, the chain transfer agent sebacic acid is 5%, light The ratio of initiator 1173 is 5%.
在此具体实施例中，手性双频液晶材料主要是由S811液晶手性添加剂和双频液晶配制而成，S811液晶手性添加剂和双频液晶的质量比为1∶9；双频液晶为由质量百分比为20％的MBBA液晶和质量百分比为80％的DT91液晶配制成的混合物；手性双频液晶材料的螺距为0.5～2μm，手性双频液晶材料的布拉格反射光波长为0.75～3μm。手性双频液晶材料在低频时介电各向异性为正大于2；当频率为20kHz时，介电各向异性为零；当频率为50kHz时，介电各向异性为-2.3。In this specific embodiment, the chiral dual-frequency liquid crystal material is mainly prepared by S811 liquid crystal chiral additive and dual-frequency liquid crystal, the mass ratio of S811 liquid crystal chiral additive and dual-frequency liquid crystal is 1:9; the dual-frequency liquid crystal is A mixture prepared by MBBA liquid crystal with a mass percentage of 20% and DT91 liquid crystal with a mass percentage of 80%. 3 μm. The dielectric anisotropy of the chiral dual-frequency liquid crystal material is positive greater than 2 at low frequencies; when the frequency is 20kHz, the dielectric anisotropy is zero; when the frequency is 50kHz, the dielectric anisotropy is -2.3.
在此具体实施例中，聚合物分散液晶层103中聚合物的折射率np、液晶寻常光的折射率no、液晶非常光的折射率ne分别为1.5～1.55、1.5～1.55、1.7～1.75；如可分别选择为1.517、1.517和1.717。In this specific embodiment, the refractive index np of the polymer in the polymer-dispersed
本发明的聚合物分散液晶三稳态膜中的液晶微滴内有三维焦锥态小碎畴、二维焦锥态大畴和平面态大畴三种零场稳定结构，光学特性是三维焦锥态小碎畴对入射光有比较强的散射，是散射关态；二维焦锥态大畴对入射光有比较强的透射，是透射开态；平面态大畴对入射光有比较强的选择布拉格反射，是反射关态。具有这三种稳态的聚合物分散液晶三稳态膜的工作原理为：在透明导电薄层电极之间施加约25伏的低频电场(如25V，50kHz)，液晶呈现为正性胆甾相液晶，被驱动到场致向列相垂面排列初始状态，即使液晶分子转向电场方向初始排列状态201，如图2a所示；快速去掉电场，在聚合物球腔边界束缚条件和S811液晶手性添加剂为主的作用下，形成沿聚合物球腔界面排列三维焦锥态小碎畴构形，液晶微滴即不是各向同性的普通透明液体，也不是各向异性单轴双折射晶体，对入射光有比较强的散射，使聚合物分散液晶三稳态膜呈现散射关态202，如图2b所示；在透明导电薄层电极之间施加约25伏的低频电场，然后缓慢(以阶梯降电压方式)去掉电场，在电场束缚条件和S811液晶手性添加剂及球腔边界束缚条件的作用之下，单个液晶微滴形成一个焦锥态大单畴构形，整个聚合物分散液晶三稳态膜中不同液晶微滴形成二维焦锥态，而且焦锥态大单畴可以看作是一个液晶大分子，与螺旋轴平行的光振动分量恰好垂直于液晶分子，所以折射率n||＝no，而与螺旋轴垂直的光振动分量对应旋转的液晶分子，所以折射率n⊥＝(no+ne)/2，聚合物的折射率与焦锥态折射率之一n||＝no匹配，与n⊥不匹配，对入射光有比较强的透射，使聚合物分散液晶三稳态膜处于半透明开态203，如图2c所示；在透明导电薄层电极之间施加高频电场，液晶呈现为负性胆甾相液晶，被驱动到场致向列相沿膜面排列态204，如图2d所示，缓慢去掉电场，在电场和S811液晶手性添加剂为主的作用之下，每个液晶微滴都形成平面态大畴构形，平面态等效折射率是(no+ne)/2，与聚合物的折射率不匹配，再加上聚合物分散液晶三稳态膜比较厚，光传播路径上会遇到多个液晶微滴，所以对入射光聚合物分散液晶三稳态膜处于可见光散射加红外光布拉格反射关态205，如图2e所示。因此，本发明的聚合物分散液晶三稳态膜可以在建筑装修等领域得到特殊的应用，炎热夏天关态处于平面态，反射红外光，冬天关态处于小畴焦锥态，散射可见光和红外光，成为具有节能环保概念的功能调光玻璃的节能窗新技术、新应用。The liquid crystal droplet in the polymer-dispersed liquid crystal tristable film of the present invention has three zero-field stable structures of three-dimensional focal conic small fragmented domains, two-dimensional focal conic large domains and planar large domains, and the optical characteristics are three-dimensional focal The small fragmented domains in the cone state have relatively strong scattering to the incident light, which is the scattering off state; the large domains in the two-dimensional focal conic state have relatively strong transmission on the incident light, and are in the transmission on state; the large domains in the planar state have a relatively strong transmission on the incident light The selected Bragg reflection, is the reflection off state. The working principle of the polymer-dispersed liquid crystal tristable film with these three stable states is: apply a low-frequency electric field of about 25 volts (such as 25V, 50kHz) between the transparent conductive thin-layer electrodes, and the liquid crystal presents a positive cholesteric phase The liquid crystal is driven to the initial state of homeotropic nematic alignment, even if the liquid crystal molecules turn to the initial alignment state 201 in the direction of the electric field, as shown in Figure 2a; the electric field is quickly removed, and the boundary conditions of the polymer spherical cavity and the S811 liquid crystal chiral additive Under the main action, a three-dimensional focal conic small fragmented domain configuration is formed along the interface of the polymer spherical cavity. The liquid crystal droplet is neither an isotropic ordinary transparent liquid nor an anisotropic uniaxial birefringent crystal. The light has relatively strong scattering, so that the polymer-dispersed liquid crystal tristable film presents the scattering off state 202, as shown in Figure 2b; a low-frequency electric field of about 25 volts is applied between the transparent conductive thin-layer electrodes, and then slowly (decreasing in steps) voltage mode) to remove the electric field, under the electric field constraint conditions and the S811 liquid crystal chiral additive and the boundary constraint conditions of the spherical cavity, a single liquid crystal droplet forms a focal conic large single domain configuration, and the entire polymer disperses the liquid crystal tristable state Different liquid crystal droplets in the film form a two-dimensional focal conic state, and the large monodomain of the focal conic state can be regarded as a liquid crystal macromolecule, and the light vibration component parallel to the helical axis is just perpendicular to the liquid crystal molecule, so the refractive index n|| = no , and the light vibration component perpendicular to the helical axis corresponds to the rotating liquid crystal molecules, so the refractive index n⊥ = (no +ne )/2, one of the refractive index of the polymer and the focal conic refractive index n|| =no matches, does not match with n⊥ , and has relatively strong transmission to incident light, making the polymer dispersed liquid crystal tristable film in a translucent open state 203, as shown in Figure 2c; between the transparent conductive thin-layer electrodes Applying a high-frequency electric field, the liquid crystal appears as a negative cholesteric liquid crystal, which is driven to the field-induced nematic phase alignment state 204 along the film plane, as shown in Figure 2d, and the electric field is slowly removed, and the effect of the electric field and the S811 liquid crystal chiral additive is mainly Under this condition, each liquid crystal droplet forms a planar large domain configuration, and the equivalent refractive index of the planar state is (no +ne )/2, which does not match the refractive index of the polymer, and the polymer dispersed liquid crystal The tristable film is relatively thick, and many liquid crystal droplets will be encountered on the light propagation path, so the polymer dispersed liquid crystal tristable film is in the off-state 205 of visible light scattering and infrared light Bragg reflection for incident light, as shown in Figure 2e. Therefore, the polymer-dispersed liquid crystal tristable film of the present invention can be used in special applications in fields such as building decoration. In hot summer, the off state is in a planar state, reflecting infrared light, and in winter, the off state is in a small-domain focal conic state, scattering visible light and infrared light. Light has become a new technology and new application of energy-saving window with functional dimming glass with the concept of energy saving and environmental protection.
上述使用的丙氧基壬苯基丙烯酸酯是美国氰特特种表面技术公司生产的产品；三羟甲基丙烷三丙烯酸酯是天津市天骄化工有限公司生产的产品；链转移剂癸二酸是衢州化工厂生产的产品；光引发剂1173是北京英力科技发展有限公司生产的产品；双频液晶是河北迈尔斯通电子材料有限公司提供的双频液晶产品，其液晶寻常光的折射率为1.517，其液晶非常光的折射率为1.717；柔性透明导电薄膜是湖南三才光电信息材料有限公司生产的透明ITO导电膜产品；衬垫材料采用深圳纳微科技公司生产的产品，其为直径为30μm的塑料微球。The propoxy nonyl phenyl acrylate used above is a product produced by Cytek Special Surface Technology Co., Ltd.; trimethylolpropane triacrylate is a product produced by Tianjin Tianjiao Chemical Co., Ltd.; the chain transfer agent sebacic acid is produced by Quzhou The product produced by the chemical factory; the photoinitiator 1173 is a product produced by Beijing Yingli Technology Development Co., Ltd.; the dual-frequency liquid crystal is a dual-frequency liquid crystal product provided by Hebei Milstone Electronic Materials Co., Ltd., and the refractive index of the ordinary light of the liquid crystal is 1.517, the refractive index of the extraordinary light of liquid crystal is 1.717; the flexible transparent conductive film is a transparent ITO conductive film product produced by Hunan Sancai Optoelectronic Information Material Co., Ltd; of plastic microspheres.
实施例二：Embodiment two:
制备实施例一所述的聚合物分散液晶三稳态膜是在超净化的车间里进行的，制备方法主要包括以下步骤：The polymer-dispersed liquid crystal tristable film described in Preparation Example 1 is carried out in an ultra-clean workshop, and the preparation method mainly includes the following steps:
①按重量比1∶(1～3)称取预聚物和手性双频液晶材料，并以1～10个/mm2的含量加入衬垫材料，在常温下对预聚物、手性双频液晶材料和衬垫材料进行充分搅拌均匀混合；在此，预聚物、手性双频液晶材料和衬垫材料具体可根据实际情况配比。①Weigh the prepolymer and chiral dual-frequency liquid crystal material according to the weight ratio of 1: (1~3), and add the gasket material at a content of 1~10 pieces/mm2 . The dual-frequency liquid crystal material and the gasket material are fully stirred and evenly mixed; here, the specific ratio of the prepolymer, the chiral dual-frequency liquid crystal material and the gasket material can be adjusted according to the actual situation.
预聚物主要由可聚合单体、链转移剂和光引发剂组成，各组分的重量百分比为：可聚合单体丙氧基壬苯基丙烯酸酯为20％、可聚合单体三羟甲基丙烷三丙烯酸酯为70％、链转移剂癸二酸为5％、光引发剂1173为5％。The prepolymer is mainly composed of polymerizable monomers, chain transfer agents and photoinitiators. The weight percentage of each component is: 20% of polymerizable monomer propoxynonyl phenyl acrylate, 20% of polymerizable monomer trimethylol Propane triacrylate was 70%, chain transfer agent sebacic acid was 5%, photoinitiator 1173 was 5%.
手性双频液晶材料主要是由S811液晶手性添加剂和双频液晶配制而成，S811液晶手性添加剂和双频液晶的质量比为1∶9；双频液晶为由质量百分比为20％的MBBA液晶和质量百分比为80％的DT91液晶配制成的混合物。The chiral dual-frequency liquid crystal material is mainly prepared by S811 liquid crystal chiral additive and dual-frequency liquid crystal. The mass ratio of S811 liquid crystal chiral additive and dual-frequency liquid crystal is 1:9; A mixture prepared from MBBA liquid crystal and DT91 liquid crystal with a mass percentage of 80%.
②分别在两层柔性透明导电薄膜的内侧表面上刻蚀出透明导电薄层电极。② Etching transparent conductive thin-layer electrodes on the inner surfaces of the two flexible transparent conductive films respectively.
③将均匀混合好的混合物转印刷到两层柔性透明导电薄膜之间。③The uniformly mixed mixture is transferred and printed between two layers of flexible transparent conductive films.
④利用压合机将印刷有混合物的两层柔性透明导电薄膜挤压成复合膜。④ Extrude the two-layer flexible transparent conductive film printed with the mixture into a composite film by using a pressing machine.
⑤使用中等强度(约25mW)的紫外光照射复合膜1～3分钟以对复合膜进行相分离，使液晶从聚合物中充分析出，形成平均直径为3～5μm的液晶微滴，同时固化液晶微滴。在此，相分离和固化处理可采用紫外光固化技术，也可采用热固化技术。⑤Use medium-intensity (about 25mW) ultraviolet light to irradiate the composite film for 1 to 3 minutes to phase-separate the composite film, so that the liquid crystal is fully separated from the polymer, forming liquid crystal droplets with an average diameter of 3 to 5 μm, and curing the liquid crystal at the same time droplet. Here, the phase separation and curing treatment may adopt ultraviolet light curing technology or thermal curing technology.
上述制备方法制备得到聚合物分散液晶三稳态膜具有散射关态、半透明开态和可见光散射加红外光布拉格反射关态三种稳态，当在透明导电薄层电极之间施加低频或直流电场，然后快速撤掉低频或直流电场后，聚合物分散液晶三稳态膜呈现散射关态；当在透明导电薄层电极之间施加低频或直流电场，然后以阶梯降电压方式撤掉低频或直流电场后，聚合物分散液晶三稳态膜呈现半透明开态；当在透明导电薄层电极之间施加高频电场，然后以阶梯降电压方式撤掉低频或直流电场后，聚合物分散液晶三稳态膜呈现可见光散射加红外光布拉格反射关态。The polymer-dispersed liquid crystal tristable film prepared by the above preparation method has three stable states: scattering off state, translucent on state and visible light scattering plus infrared Bragg reflection off state. field, and then quickly remove the low-frequency or DC electric field, the polymer dispersed liquid crystal tristable film exhibits a scattering off state; when a low-frequency or DC electric field is applied between the transparent conductive thin layer electrodes, and then remove the low-frequency or After a DC electric field, the polymer-dispersed liquid crystal tristable film presents a translucent open state; when a high-frequency electric field is applied between the transparent conductive thin-layer electrodes, and then the low-frequency or DC electric field is removed in a step-down manner, the polymer-dispersed liquid crystal The tristable film presents an off-state of visible light scattering plus infrared Bragg reflection.
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