CN101768449A - Polymer dispersed liquid crystal composition, polymer dispersed liquid crystal layer and preparation method thereof, polymer dispersed liquid crystal film and preparation method thereof - Google Patents
Polymer dispersed liquid crystal composition, polymer dispersed liquid crystal layer and preparation method thereof, polymer dispersed liquid crystal film and preparation method thereof Download PDFInfo
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技术领域technical field
本发明涉及一种聚合物分散液晶组合物、聚合物分散液晶层及其制备方法、聚合物分散液晶膜及其制备方法。The invention relates to a polymer dispersed liquid crystal composition, a polymer dispersed liquid crystal layer and a preparation method thereof, a polymer dispersed liquid crystal film and a preparation method thereof.
背景技术Background technique
聚合物分散液晶(Polymer dispersed liquid crystals，PDLC)薄膜是一种光电复合材料，在聚合物分散液晶薄膜中，微米量级的液晶微滴分散在固态聚合物基体中。通过外加电场使聚合物分散液晶薄膜由不透明到透明之间变化，使薄膜的透光率可调。Polymer dispersed liquid crystals (Polymer dispersed liquid crystals, PDLC) film is a kind of optoelectronic composite material, in the polymer dispersed liquid crystal film, micron-sized liquid crystal droplets are dispersed in a solid polymer matrix. The polymer-dispersed liquid crystal film is changed from opaque to transparent by applying an electric field, so that the light transmittance of the film can be adjusted.
在制备的时候，将聚合物单体和液晶混合物加热到清亮点以上温度时，液晶从晶体态转化为液态，与聚合物单体充分混合，固化时外界环境温度对体系进行降温，在紫外光照下，聚合物单体发生固化，液晶从固化后的聚合物中分离出来，重新形成晶态的液晶分子，聚合在一起形成液晶微滴，固定在聚合物构成的网格结构内。During preparation, when the mixture of polymer monomer and liquid crystal is heated to a temperature above the clearing point, the liquid crystal is transformed from a crystalline state to a liquid state, fully mixed with the polymer monomer, and the external ambient temperature cools the system during curing. Under the conditions, the polymer monomer is solidified, the liquid crystal is separated from the cured polymer, and the crystalline liquid crystal molecules are re-formed, and they are aggregated together to form liquid crystal droplets, which are fixed in the grid structure formed by the polymer.
聚合物分散液晶薄膜本身的聚合物分散液晶为乳白色，通电后变为透明，颜色单一。目前，有一些通过在聚合物分散液晶中添加染料，使聚合物分散液晶薄膜的色彩丰富，但是因为染料的存在，影响聚合物和液晶的混合物清亮点以下温度的相分离进行、同时液晶微滴中存在染料分子，这些使得驱动电压升高、开态透过率降低，很难获得50V以下驱动电压、开态透过率达到70％以上的聚合物分散液晶薄膜。该类聚合物分散液晶薄膜被广泛应用于汽车车窗贴膜、窗帘、屏风等产品。The polymer-dispersed liquid crystal of the polymer-dispersed liquid crystal film itself is milky white, and becomes transparent after electrification, with a single color. At present, some dyes are added to the polymer-dispersed liquid crystal to make the color of the polymer-dispersed liquid crystal film rich, but because of the existence of the dye, it affects the phase separation of the mixture of the polymer and the liquid crystal at a temperature below the clearing point, and at the same time, the liquid crystal droplets There are dye molecules in the film, which increase the driving voltage and reduce the on-state transmittance. It is difficult to obtain a polymer-dispersed liquid crystal film with a drive voltage below 50V and an on-state transmittance of more than 70%. This type of polymer dispersed liquid crystal film is widely used in automotive window films, curtains, screens and other products.
发明内容Contents of the invention
本发明要解决的问题是，提供一种颜色为非白色的聚合物分散液晶层或聚合物分散薄膜、聚合物分散液晶层或聚合物分散薄膜的制备方法，非白色的聚合物分散液晶层或聚合物分散薄膜可以同时达到驱动电压小于等于40V，开态透过率达75％以上。The problem to be solved by the present invention is to provide a method for preparing a non-white polymer dispersed liquid crystal layer or polymer dispersed film, a polymer dispersed liquid crystal layer or a polymer dispersed film, and a non-white polymer dispersed liquid crystal layer or The polymer dispersed film can simultaneously achieve a driving voltage of less than or equal to 40V, and an open-state transmittance of more than 75%.
一种聚合物分散液晶组合物，所述聚合物分散液晶组合物的颜色为非白色，所述聚合物分散液晶组合物包括聚合物单体、液晶、染料、间隔子，所述的聚合物单体为三羟甲基丙烷二烯丙基醚或丙烯酸酯、所述的液晶为联苯氰化合物、所述的染料为蒽醌化合物；以聚合物分散液晶的总量计，聚合物的重量百分含量为30～50wt％，液晶的重量百分含量为50～70wt％，染料的重量百分含量为0.8～1.5wt％，间隔子的重量百分含量为0～3wt％。A polymer-dispersed liquid crystal composition, the color of the polymer-dispersed liquid crystal composition is non-white, and the polymer-dispersed liquid crystal composition includes polymer monomers, liquid crystals, dyes, spacers, and the polymer monomers The body is trimethylolpropane diallyl ether or acrylate, the liquid crystal is a biphenyl cyanide compound, and the dye is an anthraquinone compound; based on the total amount of polymer dispersed liquid crystals, the weight of the polymer is one hundred The component content is 30-50wt%, the weight percentage of liquid crystal is 50-70wt%, the weight percentage of dye is 0.8-1.5wt%, and the weight percentage of spacer is 0-3wt%.
本发明还提供一种聚合物分散液晶层，所述聚合物分散液晶层的颜色为非白色，所述聚合物分散液晶组合物包括聚合物单体、液晶、染料，所述的聚合物分散液晶层包括聚合物构成三维孔状体结构，所述孔内填充有液晶液滴，所述孔的平均孔径为2-5微米。The present invention also provides a polymer-dispersed liquid crystal layer, the color of the polymer-dispersed liquid crystal layer is non-white, the polymer-dispersed liquid crystal composition includes polymer monomers, liquid crystals, and dyes, and the polymer-dispersed liquid crystal The layer includes a polymer to form a three-dimensional hole structure, the holes are filled with liquid crystal droplets, and the average hole diameter of the holes is 2-5 microns.
上述聚合物分散液晶层的制备方法，将上述的聚合物分散液晶组合物固化得到聚合物分散液晶层。The preparation method of the above-mentioned polymer-dispersed liquid crystal layer comprises curing the above-mentioned polymer-dispersed liquid crystal composition to obtain the polymer-dispersed liquid crystal layer.
一种聚合物分散液晶薄膜，依次包括透明基材层、导电层、聚合物分散液晶层、导电层、透明基材层，所述的聚合物分散液晶层为上述的聚合物分散液晶层。A polymer-dispersed liquid crystal film comprises a transparent substrate layer, a conductive layer, a polymer-dispersed liquid crystal layer, a conductive layer, and a transparent substrate layer in sequence, and the polymer-dispersed liquid crystal layer is the above-mentioned polymer-dispersed liquid crystal layer.
一种上述的聚合物分散液晶薄膜制备方法，包括透明基材层上镀覆导电层得到两片带有导电层的透明基材层，将上述的聚合物分散液晶组合物加热至聚合物分散液晶组合中的液晶的清亮点或清亮点以上温度，搅拌均匀，涂覆在两片带有导电层的透明基材层之间，得到聚合物分散液晶薄膜组件，在液晶清亮点以下温度光固化，得到聚合物分散液晶薄膜。A method for preparing the above-mentioned polymer-dispersed liquid crystal film, comprising coating a conductive layer on a transparent substrate layer to obtain two transparent substrate layers with a conductive layer, heating the above-mentioned polymer-dispersed liquid crystal composition until the polymer-dispersed liquid crystal The temperature of the liquid crystal in the combination is at or above the clearing point, stirred evenly, and coated between two transparent substrate layers with a conductive layer to obtain a polymer-dispersed liquid crystal film assembly, which is cured at a temperature below the liquid crystal clearing point. A polymer-dispersed liquid crystal film was obtained.
采用本发明的非白色的聚合物分散液晶层或含有该聚合物分散液晶层的聚合物分散液晶薄膜，可以同时达到驱动电压小于等于40V，40V时的开态透过率达75％以上。使非白色的聚合物分散液晶层或聚合物分散液晶薄膜的开态透过率大大降低，使这类聚合物分散液晶薄膜可以适用于更多的对电压要求比较低的场合。By adopting the non-white polymer dispersed liquid crystal layer or the polymer dispersed liquid crystal film containing the polymer dispersed liquid crystal layer of the present invention, the driving voltage can be less than or equal to 40V at the same time, and the on-state transmittance at 40V can reach more than 75%. The on-state transmittance of the non-white polymer-dispersed liquid crystal layer or polymer-dispersed liquid crystal film is greatly reduced, so that this type of polymer-dispersed liquid crystal film can be applied to more occasions with relatively low voltage requirements.
附图说明Description of drawings
图1为本发明的实施例2制备的聚合物分散液晶薄膜开关100000次前后的光电曲线；Fig. 1 is the photoelectric curve before and after 100,000 times of the polymer dispersed liquid crystal film switch that the embodiment of the
图2为本发明的实施例2制备的聚合物分散液晶薄膜的扫描电镜图片(即SEM图)；Fig. 2 is the scanning electron microscope picture (being SEM picture) of the polymer dispersed liquid crystal thin film that the embodiment of the
图3为本发明的实施例2制备的聚合物分散液晶薄膜的在耐老化测试前后光电曲线。Figure 3 is the photoelectric curves of the polymer dispersed liquid crystal film prepared in Example 2 of the present invention before and after the aging resistance test.
图中的光电曲线1为实施例2样品开关100000次后的光电曲线、光电曲线2为实施例1样品随电压变化下的透过率变化特性曲线、光电曲线3为实施例2样品耐老化测试后随电压变化下的透过率变化特性曲线。The
具体实施方式Detailed ways
一种聚合物分散液晶组合物，所述聚合物分散液晶组合物的颜色为非白色，所述聚合物分散液晶组合物包括聚合物单体、液晶、染料、间隔子，所述的聚合物单体为三羟甲基丙烷二烯丙基醚或丙烯酸酯、所述的液晶为联苯氰化合物、所述的染料为蒽醌化合物；以聚合物分散液晶的总量计，聚合物的重量百分含量为30～50wt％，液晶的重量百分含量为50～70wt％，染料的重量百分含量为0.8～1.5wt％，间隔子的重量百分含量为0～3wt％。A polymer-dispersed liquid crystal composition, the color of the polymer-dispersed liquid crystal composition is non-white, and the polymer-dispersed liquid crystal composition includes polymer monomers, liquid crystals, dyes, spacers, and the polymer monomers The body is trimethylolpropane diallyl ether or acrylate, the liquid crystal is a biphenyl cyanide compound, and the dye is an anthraquinone compound; based on the total amount of polymer dispersed liquid crystals, the weight of the polymer is one hundred The component content is 30-50wt%, the weight percentage of liquid crystal is 50-70wt%, the weight percentage of dye is 0.8-1.5wt%, and the weight percentage of spacer is 0-3wt%.
本发明的发明人经过大量实验发现，采用上述的配方，聚合物单体、液晶、燃料之间的配合，使染料对聚合物的固化速度和固化程度影响相对现有技术较小，对聚合物分散液晶膜的开态透过率影响较小，同时液晶在温度降低、紫外光的照射作用下，从聚合物和液晶的混合物之间分离出来形成液晶微滴的分离成型较好，能形成孔径范围较大的液晶微滴，按照本发明的聚合物分散液晶组合物制备的聚合物分散液晶薄膜在40V时的开态透过率高达75％，大大降低了聚合物分散液晶薄膜的开启电压，同时保证了在40V下的开态透过率满足使用要求。The inventors of the present invention have found through a large number of experiments that, using the above-mentioned formula, the coordination between polymer monomers, liquid crystals, and fuels makes the effect of the dye on the curing speed and curing degree of the polymer relatively small compared with the prior art, and has little effect on the polymer. The on-state transmittance of the dispersed liquid crystal film is less affected, and at the same time, the liquid crystal is separated from the mixture of the polymer and the liquid crystal under the action of lowering the temperature and the irradiation of ultraviolet light to form a liquid crystal droplet. For liquid crystal droplets with a relatively large range, the on-state transmittance of the polymer-dispersed liquid crystal film prepared according to the polymer-dispersed liquid crystal composition of the present invention is as high as 75% at 40V, which greatly reduces the turn-on voltage of the polymer-dispersed liquid crystal film. At the same time, the on-state transmittance at 40V is guaranteed to meet the use requirements.
本发明还提供一种聚合物分散液晶层，所述聚合物分散液晶层的颜色为非白色，所述聚合物分散液晶组合物包括聚合物单体、液晶、染料，所述的聚合物分散液晶层包括聚合物构成三维孔状体结构，所述孔内填充有液晶液滴，所述孔的平均孔径为2-5微米。The present invention also provides a polymer-dispersed liquid crystal layer, the color of the polymer-dispersed liquid crystal layer is non-white, the polymer-dispersed liquid crystal composition includes polymer monomers, liquid crystals, and dyes, and the polymer-dispersed liquid crystal The layer includes a polymer to form a three-dimensional hole structure, the holes are filled with liquid crystal droplets, and the average hole diameter of the holes is 2-5 microns.
本领域的技术人员公知，填充液晶液滴的孔的孔径越大，则驱动电压越低。本发明的非白色聚合物分散液晶能达到40V以下的驱动电压，与孔的平均孔径为2-5微米有较为密切的关系。采用上述的聚合物分散液晶组合物可以制备得到孔的平均孔径为2-5微米的聚合物分散液晶。上述聚合物分散液晶层的制备方法，将上述的非白色聚合物分散液晶组合物固化得到聚合物分散液晶层。Those skilled in the art know that the larger the diameter of the hole filled with liquid crystal droplets, the lower the driving voltage. The non-white polymer dispersed liquid crystal of the present invention can reach a driving voltage below 40V, which is closely related to the average hole diameter of 2-5 microns. A polymer dispersed liquid crystal with an average pore diameter of 2-5 microns can be prepared by using the above polymer dispersed liquid crystal composition. The preparation method of the above-mentioned polymer-dispersed liquid crystal layer comprises curing the above-mentioned non-white polymer-dispersed liquid crystal composition to obtain the polymer-dispersed liquid crystal layer.
一种聚合物分散液晶薄膜，依次包括透明基材层、导电层、聚合物分散液晶层、导电层、透明基材层，所述的聚合物分散液晶层为上述的聚合物分散液晶层。A polymer-dispersed liquid crystal film comprises a transparent substrate layer, a conductive layer, a polymer-dispersed liquid crystal layer, a conductive layer, and a transparent substrate layer in sequence, and the polymer-dispersed liquid crystal layer is the above-mentioned polymer-dispersed liquid crystal layer.
一种上述的聚合物分散液晶薄膜制备方法，包括透明基材层上镀覆导电层得到两片带有导电层的透明基材层，将上述的聚合物分散液晶组合物加热至聚合物分散液晶组合中的液晶的清亮点或清亮点以上温度，搅拌均匀，涂覆在两片带有导电层的透明基材层之间，得到聚合物分散液晶薄膜组件，在液晶清亮点以下温度光固化，得到聚合物分散液晶薄膜。A method for preparing the above-mentioned polymer-dispersed liquid crystal film, comprising coating a conductive layer on a transparent substrate layer to obtain two transparent substrate layers with a conductive layer, heating the above-mentioned polymer-dispersed liquid crystal composition until the polymer-dispersed liquid crystal The temperature of the liquid crystal in the combination is at or above the clearing point, stirred evenly, and coated between two transparent substrate layers with a conductive layer to obtain a polymer-dispersed liquid crystal film assembly, which is cured at a temperature below the liquid crystal clearing point. A polymer-dispersed liquid crystal film was obtained.
所述的聚合物分散液晶组合物在固化前为透明油状物，固化后，形成非白色薄膜，即聚合物分散液晶薄膜，这是因为液晶在中间起到折射和散射的作用，使自然光线无法通过膜层。而本发明要解决的技术问题就是在添加染料的情况下，如何解决染料带来的聚合物分散液晶薄膜的一系列性能下降的问题。The polymer-dispersed liquid crystal composition is a transparent oil before curing, and after curing, a non-white film is formed, that is, a polymer-dispersed liquid crystal film. This is because the liquid crystal plays the role of refraction and scattering in the middle, so that natural light cannot through the film layer. The technical problem to be solved in the present invention is how to solve a series of performance degradation problems of the polymer-dispersed liquid crystal film caused by dyes when dyes are added.
优选地，所述的聚合物分散液晶组合物还含有交联剂、光引发剂，所述的联苯氰化合物为戊基联苯氰、庚基联苯氰、辛氧基联苯氰、戊基三联苯氰中的一种或几种；所述的蒽醌化合物为1-苯氨基-4-(甲基氨基)蒽醌。Preferably, the polymer-dispersed liquid crystal composition also contains a crosslinking agent and a photoinitiator, and the biphenylcyanide compound is pentylbiphenylcyanide, heptylbiphenylcyanide, octyloxybiphenylcyanide, pentylbiphenylcyanide, One or more of the base terphenylcyanides; the anthraquinone compound is 1-anilino-4-(methylamino)anthraquinone.
所述的交联剂为本领域的技术人员公知的增加单体的交联，起到改善聚合物分散薄膜组合物的刚性、柔性等性能的交联剂。所述的交联剂为异氰酸酯、硫醇化合物、乙烯基吡咯烷酮、十一烯酸异山梨醇酯中的一种或几种。The crosslinking agent is a crosslinking agent known to those skilled in the art to increase the crosslinking of monomers and improve the rigidity, flexibility and other properties of the polymer dispersed film composition. The crosslinking agent is one or more of isocyanate, thiol compound, vinylpyrrolidone, and isosorbide undecylenate.
所述的光引发剂为本领域的技术人员公知的光引发剂，如，紫外光引发剂2-羟基-2-甲基-1-苯基丙酮、1-羟基环己基苯甲酮、2-甲基1-(4-巯基苯基)-2-吗啉-1-丙酮和2-苄基-2-二甲氨基-1-(4-吗啉苄基)-1-丁酮、安息香双甲醚中的一种或几种。Described photoinitiator is the well-known photoinitiator of those skilled in the art, as, ultraviolet photoinitiator 2-hydroxyl-2-methyl-1-phenylacetone, 1-hydroxycyclohexyl benzophenone, 2- Methyl 1-(4-mercaptophenyl)-2-morpholine-1-propanone and 2-benzyl-2-dimethylamino-1-(4-morpholinebenzyl)-1-butanone, benzoin bis One or more of methyl ethers.
所述的聚合物单体为三羟甲基丙烷二烯丙基醚或丙烯酸酯，所述的三羟甲基丙烷二烯丙基醚为本领域的技术人员所公知，可商购，例如NORLAND公司生产的NOA65的主体树脂为三羟甲基丙烷二烯丙基醚，NOA65中还含有改善刚性和柔性的交联剂异氰酸酯、硫醇化合物。The polymer monomer is trimethylolpropane diallyl ether or acrylate, and the trimethylolpropane diallyl ether is well known to those skilled in the art and is commercially available, such as NORLAND The main resin of NOA65 produced by the company is trimethylolpropane diallyl ether, and NOA65 also contains crosslinking agent isocyanate and thiol compounds to improve rigidity and flexibility.
所述的异氰酸酯为本领域公知的异氰酸酯，如甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯、1，4-环乙烷二异氰酸酯中的一种。The isocyanate is known in the art, such as one of toluene diisocyanate, diphenylmethane diisocyanate, hexamethylene diisocyanate, and 1,4-cycloethane diisocyanate.
所述的丙烯酸酯为本领域的技术人员公知的各种丙烯酸酯，优选地所述的丙烯酸酯为丙烯酸羟丙酯、丙烯酸丁二醇酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丙酯、环氧丙烯酸酯、聚氨酯丙烯酸酯、丙烯酸胆固醇酯、甲基丙烯酸β-羟乙酯中的一种或几种。Described acrylate is various acrylate known to those skilled in the art, preferably described acrylate is hydroxypropyl acrylate, butylene glycol acrylate, methyl methacrylate, ethyl methacrylate, methyl methacrylate One or more of propyl acrylate, epoxy acrylate, urethane acrylate, cholesteryl acrylate, and β-hydroxyethyl methacrylate.
进一步优选地，所述的液晶为戊基联苯氰、庚基联苯氰、正辛氧基联苯氰、正戊基三联苯氰的混合物；以液晶的总量计，戊基联苯氰的重量百分含量为40～60wt％，庚基联苯氰的重量百分含量为10％～30％，戊基三联苯氰的重量百分含量为10％～30％，余量为辛基联苯氰。所述的辛基联苯氰的含量可以为零。Further preferably, the liquid crystal is a mixture of pentyl biphenyl cyanide, heptyl biphenyl cyanide, n-octyl biphenyl cyanide, and n-pentyl terphenyl cyanide; The weight percentage of cyanide is 40-60wt%, the weight percentage of heptyl biphenyl cyanide is 10%-30%, the weight percentage of pentyl terphenyl cyanide is 10%-30%, and the balance is octyl Biphenylcyanide. The content of said octylbiphenylcyanide can be zero.
所述的联苯氰化合物为本领域的技术人员公知的联苯氰化合物，可商购，如大立高分子工业股份有限公司生产的E7液晶由51％戊基联苯氰，25％庚基联苯氰，16％辛氧基联苯氰，8％戊基三联苯氰以上四种液晶混合得到。所述的蒽醌化合物为本领域技术人员公知的染料，可商购，例如，本发明选用的是国药集团化学试剂有限公司提供的油溶蓝N，即1-苯氨基-4-(甲基氨基)蒽醌。Described biphenylcyanide compound is the well-known biphenylcyanide compound of those skilled in the art, commercially available, as the E7 liquid crystal produced by Dali Polymer Industry Co., Ltd. by 51% amyl biphenylcyanide, 25% heptyl Biphenylcyanide, 16% octyloxybiphenylcyanide, and 8% amyl terphenylcyanide are obtained by mixing the above four liquid crystals. The anthraquinone compound is a dye well known to those skilled in the art, and is commercially available. For example, what the present invention selects is oil soluble blue N provided by Sinopharm Chemical Reagent Co., Ltd., i.e. 1-anilino-4-(methyl amino) anthraquinone.
所述的开态透过率为本领域的技术人员公知的，在开态即电场下，透过聚合物分散液晶薄膜的出射光与入射光的光强的比值，如果比值为100％，说明所有的入射光都透射成出射光，一般在入射光入射在聚合物分散液晶薄膜的表面会有部分入射光被漫反射和吸收，因此一般出射光与入射光的比值一般小于1，对于在关态，即切断电场的电源的情况下，聚合物分散液晶膜内的液晶微滴处于杂乱无章的状态，聚合物分散液晶呈现聚合物分散液晶组合物的颜色，即染料的颜色。如果染料是蓝色的，则在关态呈现不透光的蓝色，此时的关态透光率往往为3％左右，几乎接近于0，即完全不透光的状态，一般为3％左右。开态情况下，聚合物分散液晶薄膜中的液晶微滴的取向一致，聚合物分散液晶薄膜呈现透明，则开态透光率接近100％，一般为60％左右。The open state transmittance is well known to those skilled in the art. In the open state, that is, under the electric field, the ratio of the light intensity of the outgoing light through the polymer dispersed liquid crystal film to the light intensity of the incident light, if the ratio is 100%, it means All the incident light is transmitted into the outgoing light. Generally, when the incident light is incident on the surface of the polymer dispersed liquid crystal film, part of the incident light will be diffusely reflected and absorbed. Therefore, the ratio of the outgoing light to the incident light is generally less than 1. state, that is, when the power supply of the electric field is cut off, the liquid crystal droplets in the polymer-dispersed liquid crystal film are in a disordered state, and the polymer-dispersed liquid crystal exhibits the color of the polymer-dispersed liquid crystal composition, that is, the color of the dye. If the dye is blue, it will appear opaque blue in the off state. At this time, the light transmittance in the off state is often about 3%, which is almost close to 0, that is, the state of complete opacity, generally 3%. about. In the open state, the orientation of the liquid crystal droplets in the polymer dispersed liquid crystal film is consistent, the polymer dispersed liquid crystal film is transparent, and the light transmittance in the open state is close to 100%, generally about 60%.
染料为有机化合物，在长期的光照情况下，容易发生分解。本发明的发明人经过大量实验发现，当聚合物单体的重量百分含量为36～45wt％，液晶的重量百分含量为58～65wt％时，制备的聚合物分散液晶薄膜的稳定性进一步增强，耐老化性能更加稳定。Dyes are organic compounds that are prone to decomposition under long-term light conditions. The inventors of the present invention have found through a large number of experiments that when the weight percentage of the polymer monomer is 36 to 45 wt%, and the weight percentage of the liquid crystal is 58 to 65 wt%, the stability of the prepared polymer dispersed liquid crystal film is further improved. Enhanced, more stable aging resistance.
例如，本发明的实施例2，如图3所示的电光曲线1、3分别为，紫外光照射100h前后，用液晶综合参术测试仪测得的实施例2的聚合物分散液晶薄膜的电光曲线。For example, in
所述的对比度为本领域的技术人员公知的，光电曲线中最大透光率与关态透光率的比值为对比度。即如下面公式所示：其中，T最大透光率为光电曲线中最大透光率的值，T关态透光率为光电曲线中关态透光率的值。The contrast is well known to those skilled in the art, and the ratio of the maximum light transmittance to the off-state light transmittance in the photoelectric curve is the contrast. That is, as shown in the following formula: Among them, the maximum light transmittance of T is the value of the maximum light transmittance in the photoelectric curve, and the off-state light transmittance of T is the value of the off-state light transmittance in the photoelectric curve.
例如图3中的电光曲线1为刚刚制备得到的聚合物分散液晶薄膜采用液晶综合参术测试仪测得的电光曲线，该曲线中的最大透光率与关态透光率的比值为，75.85％÷4.61％＝16.5即电光曲线1的对比度为16.5。For example, the electro-
在紫外光下照射100h后，采用液晶综合参术测试仪测得的电光曲线，该曲线中的最大透光率与关态透光率的比值为74.52％÷4.66％＝16.0，即电光曲线1的对比度为16.0。After irradiating under ultraviolet light for 100 hours, the electro-optic curve measured by a liquid crystal comprehensive parameter tester shows that the ratio of the maximum light transmittance to the off-state light transmittance in the curve is 74.52% ÷ 4.66% = 16.0, that is, the electro-
则在紫外光下照射100h前后，对比度下降0.5，最大透过率减小1.33％，对比度的变化率为0.5÷16.5＝3.0％，聚合物分散液晶膜未发生明显黄变，说明本发明的实施例制备得到的聚合物分散液晶薄膜在紫外光照射下较稳定。紫外光照射老化实验属于破坏性实验，这样的照射强度相当于阳光下照射几年，因此，本发明的聚合物分散液晶薄膜的耐老化性能优异。Then before and after irradiating 100h under ultraviolet light, the contrast decreased by 0.5, the maximum transmittance decreased by 1.33%, the rate of change of the contrast was 0.5÷16.5=3.0%, and the polymer dispersed liquid crystal film did not have obvious yellowing, which illustrates the implementation of the present invention The prepared polymer-dispersed liquid crystal film is relatively stable under ultraviolet light irradiation. The ultraviolet light irradiation aging experiment is a destructive experiment, and such irradiation intensity is equivalent to several years of sunlight irradiation. Therefore, the polymer dispersed liquid crystal film of the present invention has excellent aging resistance.
所述的间隔子为本领域的技术人员公知的用于支撑出放置聚合物分散液晶膜的空间的物质，一般为玻璃微珠。间隔子主要用于控制两片导电膜间的间隙。可以根据设计的聚合物分散液晶薄膜的需要而确定是否含有间隔子，间隔子的含量可以为零。The spacer is a material known to those skilled in the art to support the space for placing the polymer-dispersed liquid crystal film, and is generally a glass bead. Spacers are mainly used to control the gap between two conductive films. Whether to contain spacers can be determined according to the needs of the designed polymer-dispersed liquid crystal film, and the content of spacers can be zero.
一种聚合物分散液晶薄膜，依次包括透明基材层、导电层、聚合物分散液晶层、导电层、透明基材层，所述的聚合物分散液晶层由含有上述的聚合物分散液晶组合物经固化得到。所述导电层为本领域的技术人员公知的导电层，如纳米铟锡金属氧化物导电层。A polymer-dispersed liquid crystal film, comprising a transparent substrate layer, a conductive layer, a polymer-dispersed liquid crystal layer, a conductive layer, and a transparent substrate layer, wherein the polymer-dispersed liquid crystal layer consists of the above-mentioned polymer-dispersed liquid crystal composition Obtained by curing. The conductive layer is a conductive layer known to those skilled in the art, such as a nano-indium tin metal oxide conductive layer.
所述透明基材层为本领域的技术人员公知的透明基材的材质，一般为玻璃、聚碳酸酯、聚对苯二甲酸乙二醇酯中的一种。The transparent substrate layer is a transparent substrate material known to those skilled in the art, generally one of glass, polycarbonate, and polyethylene terephthalate.
上述聚合物分散液晶薄膜制备方法，包括透明基材层上镀覆导电层得到两片带有导电层的透明基材层，将上述的聚合物分散液晶组合物加热至聚合物分散液晶组合中的液晶的清亮点或清亮点以上温度，搅拌均匀，涂覆在两片带有导电层的透明基材层之间，得到聚合物分散液晶薄膜组件，在液晶清亮点以下温度光固化，得到聚合物分散液晶薄膜。The method for preparing the polymer-dispersed liquid crystal film includes coating a conductive layer on the transparent substrate layer to obtain two transparent substrate layers with a conductive layer, and heating the above-mentioned polymer-dispersed liquid crystal composition to the temperature of the polymer-dispersed liquid crystal composition. Stir evenly at the clearing point of the liquid crystal or above the clearing point, and coat it between two transparent substrate layers with a conductive layer to obtain a polymer-dispersed liquid crystal film assembly, and light-cure it at a temperature below the clearing point of the liquid crystal to obtain a polymer Disperse liquid crystal film.
所述的带有导电层的透明基材为本领域的技术人员所公知，所述的带有导电层的透明基材可以为玻璃、聚氨酯、聚碳酸酯、聚酯树脂、乙酸酯树脂、聚醚砜树脂、聚碳酸酯树脂、聚酰胺树脂、聚酰亚胺树脂、聚烯烃树脂、聚氯乙烯树脂、聚苯乙烯树脂、聚乙烯醇树脂、聚烯丙基化树脂、聚苯硫醚树脂、聚偏1，1-二氯乙烯树脂和(甲基)丙烯酸树脂等。Described transparent substrate with conductive layer is well known to those skilled in the art, and described transparent substrate with conductive layer can be glass, polyurethane, polycarbonate, polyester resin, acetate resin, Polyethersulfone resin, polycarbonate resin, polyamide resin, polyimide resin, polyolefin resin, polyvinyl chloride resin, polystyrene resin, polyvinyl alcohol resin, polyallylated resin, polyphenylene sulfide resin, polyvinylidene chloride resin and (meth)acrylic resin, etc.
导电层为铟、锡、铝、锌等的氧化物或者混合氧化物。此导电膜可以通过真空蒸镀、溅射法、离子镀膜法和涂覆法等获得。The conductive layer is an oxide or a mixed oxide of indium, tin, aluminum, zinc, or the like. This conductive film can be obtained by vacuum evaporation, sputtering, ion plating and coating.
所述液晶的清亮点为本领域的技术人员公知的，即液晶由各相异性体转化为同向同形体时的温度。The clearing point of the liquid crystal is well known to those skilled in the art, that is, the temperature at which the liquid crystal transforms from an anisotropic body to an isotropic body.
以聚合物分散液晶的总量计，聚合物的重量百分含量为30～50wt％，液晶的重量百分含量为50～70wt％，染料的重量百分含量为0.8～1.5wt％，间隔子的重量百分含量为1.5～3wt％加入到容器中，混合均匀得到混合物。混合物加热到清亮点上0～50℃，搅拌均匀，涂布两片带有导电层的透明基材层(例如商购的ITO玻璃)之间，以3～15mw紫外光，在20～40℃下照射2～15分钟，固化成聚合物分散液晶薄膜即PDLC薄膜。Based on the total amount of polymer-dispersed liquid crystals, the weight percentage of the polymer is 30-50 wt%, the weight percentage of the liquid crystal is 50-70 wt%, the weight percentage of the dye is 0.8-1.5 wt%, and the spacer The weight percent content is 1.5-3wt%, put into the container, and mix uniformly to obtain the mixture. Heat the mixture to 0-50°C above the clearing point, stir evenly, coat between two transparent substrate layers (such as commercially available ITO glass) with a conductive layer, and use 3-15mw ultraviolet light at 20-40°C Under irradiation for 2 to 15 minutes, it is solidified into a polymer-dispersed liquid crystal film, that is, a PDLC film.
下面就具体的实施例对本发明进行进一步地说明：Below with regard to specific embodiment, the present invention is further described:
实施例1Example 1
称取30wt％聚合物单体为NOA65和70wt％液晶E7，共计100克，在容器中，加入1.5克的平均粒径为15um的玻璃微珠作为间隔子，称取1.2克1-苯氨基-4-(甲基氨基)蒽醌，混合均匀，得到混合物，所述的液晶E7的清亮点为80度，加热混合物到85℃左右，搅拌均匀，涂布在两片ITO玻璃之间，以365nm波长的紫外光、5mw/cm2光强、在25℃室温环境下照射4分钟，得到聚合物分散液晶薄膜A1。Weigh 30wt% polymer monomer as NOA65 and 70wt% liquid crystal E7, a total of 100 grams, in the container, add 1.5 grams of glass beads with an average particle diameter of 15um as a spacer, weigh 1.2 grams of 1-phenylamino- 4-(Methylamino)anthraquinone, mixed evenly to obtain a mixture, the liquid crystal E7 has a clearing point of 80 degrees, heated the mixture to about 85°C, stirred evenly, and spread it between two pieces of ITO glass at 365nm Ultraviolet light with a wavelength of 5 mw/cm2 light intensity was irradiated for 4 minutes at a room temperature of 25° C. to obtain a polymer dispersed liquid crystal film A1.
实施例2Example 2
同实施例1，区别点在于40wt％聚合物单体和60wt％液晶，聚合物单体和液晶的重量百分比为40∶60，得到聚合物分散液晶薄膜A2。Same as Example 1, the difference lies in 40wt% polymer monomer and 60wt% liquid crystal, the weight percentage of polymer monomer and liquid crystal is 40:60, and the polymer dispersed liquid crystal film A2 is obtained.
实施例3Example 3
同实施例1，区别点在于50wt％聚合物单体和50wt％液晶，聚合物单体和液晶的重量百分比为50∶50，得到聚合物分散液晶薄膜A3。Same as Example 1, the difference lies in 50wt% polymer monomer and 50wt% liquid crystal, the weight percentage of polymer monomer and liquid crystal is 50:50, and polymer dispersed liquid crystal film A3 is obtained.
实施例4Example 4
同实施例1，称取0.8克1-苯氨基-4-(甲基氨基)蒽醌，加入1.5克的平均粒径为15um的玻璃微珠作为间隔子，得到聚合物分散液晶薄膜A4。Same as Example 1, 0.8 gram of 1-anilino-4-(methylamino)anthraquinone was weighed, and 1.5 gram of glass beads with an average particle diameter of 15 um were added as spacers to obtain polymer dispersed liquid crystal film A4.
实施例5Example 5
同实施例1，区别在于使用的聚合物单体为混合单体，所述混合单体为60wt％丙烯酸羟丙酯和40wt％丙烯酸丁二醇酯构成，以0.05％安息香双甲醚作引发剂。得到聚合物分散液晶薄膜A5。Same as Example 1, the difference is that the polymer monomer used is a mixed monomer, and the mixed monomer is composed of 60wt% hydroxypropyl acrylate and 40wt% butylene glycol acrylate, and 0.05% benzoin dimethyl ether is used as an initiator . A polymer-dispersed liquid crystal film A5 was obtained.
实施例6Example 6
同实施例1，区别在于将加热后混合物涂覆在一片玻璃上，紫外光固化后，将固化得到的聚合物分散液晶层从玻璃上玻璃开，得到聚合物分散液晶层A6。Same as Example 1, the difference is that the heated mixture is coated on a piece of glass, and after being cured by ultraviolet light, the cured polymer-dispersed liquid crystal layer is removed from the glass to obtain the polymer-dispersed liquid crystal layer A6.
比较例1Comparative example 1
同实施例1，区别点在于25％聚合物单体和75％液晶，聚合物单体和液晶的重量百分比为25∶75。得到聚合物分散液晶薄膜B1。Same as Example 1, the difference lies in 25% polymer monomer and 75% liquid crystal, and the weight percentage of polymer monomer and liquid crystal is 25:75. A polymer-dispersed liquid crystal film B1 was obtained.
比较例2Comparative example 2
同实施例1，区别点在于60％聚合物单体和40％液晶，聚合物单体和液晶的重量百分比为60∶40。得到聚合物分散液晶薄膜B2。Same as Example 1, the difference lies in 60% polymer monomer and 40% liquid crystal, and the weight percentage of polymer monomer and liquid crystal is 60:40. A polymer-dispersed liquid crystal film B2 was obtained.
测试方法Test Methods
耐紫外光(UV)老化实验Anti-ultraviolet (UV) aging test
将聚合物分散液晶薄膜A1～A6在UV光照下340nm，0.63W/m2/nm，60℃，照射时间为100h，长春联诚仪器有限公司生产的LCT-5016C型号的液晶综合参数仪。The polymer-dispersed liquid crystal films A1-A6 were exposed to UV light at 340nm, 0.63W/m2/nm, 60°C, and the irradiation time was 100h, using the LCT-5016C liquid crystal comprehensive parameter instrument produced by Changchun Liancheng Instrument Co., Ltd.
开关实验switch experiment
将实施例1-6样品通过开关控制电场的开或者关，电场开关100000次后，对比度实验前后变化不到1.0，即可说明本发明具有较好的稳定性和使用寿命。The samples of Examples 1-6 were controlled to turn on or off the electric field through a switch. After the electric field was switched on and off 100,000 times, the contrast before and after the experiment changed by less than 1.0, which shows that the present invention has good stability and service life.
通过图1可以看出，本发明的实施例具有低于40V的驱动电压和75％以上的透过率。It can be seen from FIG. 1 that the embodiment of the present invention has a driving voltage lower than 40V and a transmittance of more than 75%.
用液晶综合参数测试仪测得实施例2的PDLC薄膜的电光曲线如图1所示，图中纵坐标为透过率，横坐标为施加电压。实施例二的PDLC薄膜聚合物网络的扫描电镜(SEM)图片如图2所示。The electro-optic curve of the PDLC film of Example 2 measured by a liquid crystal comprehensive parameter tester is shown in Figure 1, where the ordinate in the figure is the transmittance, and the abscissa is the applied voltage. The scanning electron microscope (SEM) picture of the PDLC thin film polymer network of Example 2 is shown in FIG. 2 .
测试结果如下表1所示：The test results are shown in Table 1 below:
表1Table 1
从表1的测试结果可以看出，本发明制备得到的非白色的聚合物分散液晶层或聚合物分散薄膜，可以同时达到驱动电压小于等于40V，开态透过率达75％以上。It can be seen from the test results in Table 1 that the non-white polymer-dispersed liquid crystal layer or polymer-dispersed film prepared by the present invention can simultaneously achieve a driving voltage of less than or equal to 40V, and an on-state transmittance of more than 75%.
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2008
- 2008-12-30 CN CN 200810242158 patent/CN101768449B/en not_active Expired - Fee Related
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