CN101430449B - Polymer-dispersed liquid crystal calender effect film and its manufacturing method and application - Google Patents
Polymer-dispersed liquid crystal calender effect film and its manufacturing method and application Download PDFInfo
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Abstract
Description
技术领域technical field
本发明涉及一种聚合物分散液晶压光效应膜,制备出弹性体膜实现即能通过施加电场使膜有散射或者透光性能,也能通过施加压力使膜有散射或者透光性能,进而获得更为奇特的调光功能薄膜,可以在光纤压力传感器,压力触点光阀以及智能触摸窗等领域得到特殊的应用。The invention relates to a polymer-dispersed liquid crystal calender effect film. The elastomer film is prepared to realize that the film can have scattering or light transmission properties by applying an electric field, and can also make the film have scattering or light transmission properties by applying pressure, thereby obtaining More exotic dimming functional films can be used in special applications in the fields of optical fiber pressure sensors, pressure contact light valves, and smart touch windows.
背景技术Background technique
聚合物分散液晶(Polymer Dispersed Liquid Crystal,简称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,液晶从聚合物中析出形成微滴,聚合物固化把液晶微滴包裹在其中的一种复合膜。不加电场时,由于聚合物的折射率与液晶材料折射率不匹配,造成光散射,复合膜对光是关态;当施加电场后,聚合物折射率与液晶材料折射率相匹配,造成光透射,复合膜对光是开态。PDLC膜是20世纪80年代发明的高科技产品,在调光玻璃,大屏幕显示,全息光栅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课题。Polymer Dispersed Liquid Crystal (Polymer Dispersed Liquid Crystal, referred to as PDLC) is a mixture of polymer, nematic liquid crystal and spacer in a certain ratio, sandwiched between two flexible transparent conductive films, and undergoes phase separation. , the liquid crystal precipitates from the polymer to form microdroplets, and the polymer solidifies a composite film in which the liquid crystal microdroplets are wrapped. When no electric field is applied, because the refractive index of the polymer does not match the refractive index of the liquid crystal material, resulting in light scattering, the composite film is off to light; when the electric field is applied, the refractive index of the polymer matches the refractive index of the liquid crystal material, resulting in light scattering. In transmission, the composite film is open to light. PDLC film is a high-tech product invented in the 1980s. It has application value in many fields such as dimming glass, large-screen display, and holographic grating. It is still a topic of concern to researchers of liquid crystal devices.
压电效应是众所周知的物理现象实用技术,依据电介质压电效应研制的一类传感器称为压电传感器。光纤传感器是现代传感技术的应用广泛的先进技术。胆甾相液晶在压力作用下螺距会变化引起布拉格反射光颜色变化,人们称之为压光效应。PDLC膜除具有奇特的电光特性外,还有拉伸或者剪切应力引起透光效应方面的应用研究报道,但是还没有压力引起透光效应,即压光效应的报道。本发明基于对PDLC具有压光效应的最新研究最新实验现象的认识,PDLC与压力作用下的透光现象结合起来,为设计新产品提供方案。The piezoelectric effect is a well-known physical phenomenon and a practical technology. A type of sensor developed based on the dielectric piezoelectric effect is called a piezoelectric sensor. Optical fiber sensor is a widely used advanced technology of modern sensing technology. Under the action of pressure, the pitch of cholesteric liquid crystal will change, causing the color of Bragg reflected light to change, which is called calendering effect. In addition to the unique electro-optic properties of PDLC films, there are also reports on the application of light transmission effects caused by tensile or shear stress, but there is no report on pressure-induced light transmission effects, that is, calendering effects. The present invention is based on the understanding of the latest research and latest experimental phenomenon that PDLC has a calendering effect. PDLC is combined with the light transmission phenomenon under pressure to provide a solution for designing new products.
发明内容Contents of the invention
本发明的目的在于提供一种聚合物分散液晶压光效应膜,采用高弹性聚合物,用简单的设计方案依靠压力变化实现PDLC散射与透光两种状态,进而获得一种PDLC的新方案,可以在建筑装修与珠宝柜台等领域得到特殊的应用,成为功能玻璃的新技术,新品种,新应用,为设计新的功能玻璃工作原理提供参考。特别是可以应用于光纤压力传感器,压力触点光阀以及智能触摸窗的应用制造。The purpose of the present invention is to provide a polymer dispersed liquid crystal calendering effect film, which adopts high elastic polymer, realizes two states of PDLC scattering and light transmission by means of pressure changes with a simple design scheme, and then obtains a new scheme of PDLC, It can be specially applied in the fields of architectural decoration and jewelry counters, and becomes a new technology, new variety, and new application of functional glass, providing a reference for the design of new functional glass working principles. In particular, it can be applied to the application and manufacture of optical fiber pressure sensors, pressure contact light valves and smart touch windows.
本发明提供的一种聚合物分散液晶压光效应膜,包括两张柔性透明导电薄膜,一层聚合物分散液晶层,聚合物分散液晶层夹在两张柔性透明导电薄膜之间,两张导电薄膜上刻蚀有电极;聚合物分散液晶层是由预聚物、向列相液晶材料及衬垫材料制成。具体制备步骤为:在常温下将预聚物、向列相液晶材料及衬垫材料混合后转印到两张柔性透明导电膜之间,挤压成复合膜,紫外光照射,使液晶从聚合物中析出,形成液晶微滴,两张柔性透明导电膜加工出电极引线,并在电极间施加直流电场,对聚合物分散液晶压光效应膜的垂直表面方向施加压力。A polymer dispersed liquid crystal calender effect film provided by the invention comprises two flexible transparent conductive films, a layer of polymer dispersed liquid crystal layer, the polymer dispersed liquid crystal layer is sandwiched between two flexible transparent conductive films, two conductive films Electrodes are etched on the film; the polymer dispersed liquid crystal layer is made of prepolymer, nematic liquid crystal material and pad material. The specific preparation steps are: mix the prepolymer, nematic liquid crystal material and liner material at room temperature, transfer between two flexible transparent conductive films, extrude into a composite film, and irradiate with ultraviolet light to make the liquid crystal from polymerization Liquid crystal droplets are formed, two flexible transparent conductive films are processed to form electrode leads, and a DC electric field is applied between the electrodes to exert pressure on the vertical surface direction of the polymer dispersed liquid crystal calender effect film.
预聚物与向列相液晶的质量比为1∶1-3,预聚物包括可聚合单体、链转移剂和光引发剂。所述的衬垫材料微球直径尺寸6-30μm,在聚合物分散液晶层中含量为10-30个/mm2。The mass ratio of the prepolymer to the nematic liquid crystal is 1:1-3, and the prepolymer includes a polymerizable monomer, a chain transfer agent and a photoinitiator. The microspheres of the spacer material have a diameter of 6-30 μm and a content of 10-30 microspheres/mm 2 in the polymer dispersed liquid crystal layer.
所述的聚合物分散液晶层中聚合物的折射率为np,液晶材料寻常光折射率为no,液晶非常光折射率为ne;三个折射率之间关系为np=(no+ne)/2,np取值1.5-1.65,no取值1.45-1.55,ne取值1.55-1.75。The refractive index of the polymer in the polymer-dispersed liquid crystal layer is np , the ordinary light refractive index of the liquid crystal material is no , and the extraordinary light refractive index of the liquid crystal is ne ; the relationship between the three refractive indices is np =(n o +n e )/2, the value of n p is 1.5-1.65, the value of n o is 1.45-1.55, and the value of n e is 1.55-1.75.
所述的预聚物原料的质量组成:可聚合单体丙氧基壬苯基丙烯酸酯15-25%,三羟甲基丙烷三丙烯酸酯65-75%,链转移剂癸二酸3-5%,光引发剂1173为3-5%。The mass composition of the prepolymer raw material: 15-25% of polymerizable monomer propoxynonyl phenyl acrylate, 65-75% of trimethylolpropane triacrylate, 3-5% of chain transfer agent sebacic acid %, photoinitiator 1173 is 3-5%.
所述的透明胶片可以是透明导电薄膜,也可以是普通不导电的透明胶片。The transparent film can be a transparent conductive film, or an ordinary non-conductive transparent film.
所述的聚合物分散液晶压光效应膜,施加电压时,液晶微滴中液晶分子指向电场方向,液晶微滴呈现为各向异性单轴晶体,PDLC膜处于透明开态。去掉电场液晶微滴中液晶分子指向矢散乱分布,即不是各向异性的单轴晶体,也不是各向同性的透明液体,而是浑浊液体,PDLC膜处于散射关态。In the polymer dispersed liquid crystal calender effect film, when a voltage is applied, the liquid crystal molecules in the liquid crystal microdroplets point to the direction of the electric field, the liquid crystal microdroplets appear as anisotropic uniaxial crystals, and the PDLC film is in a transparent open state. If the electric field is removed, the directors of the liquid crystal molecules in the liquid crystal microdroplets are scattered, that is, not an anisotropic uniaxial crystal, nor an isotropic transparent liquid, but a turbid liquid, and the PDLC film is in the scattering off state.
所述的聚合物分散液晶压光效应膜,垂直表面方向施加压力时,液晶微滴中液晶分子将沿薄膜表面排列,液晶微滴又呈现为各向异性单轴晶体,PDLC膜也能处于透明开态。The polymer-dispersed liquid crystal calender effect film, when pressure is applied in the direction perpendicular to the surface, the liquid crystal molecules in the liquid crystal droplets will be arranged along the surface of the film, and the liquid crystal droplets will appear as anisotropic uniaxial crystals, and the PDLC film can also be in a transparent state. Open state.
聚合物分散液晶压光效应膜的制造方法适用PDLC制造技术,是采用紫外光固化相分离技术。The manufacturing method of the polymer-dispersed liquid crystal calendering effect film is applicable to the PDLC manufacturing technology, which adopts the ultraviolet light curing phase separation technology.
本发明提供的聚合物分散液晶压光效应膜的制造方法包括的步骤:The manufacturing method of the polymer dispersed liquid crystal calendering effect film provided by the invention comprises the steps:
1)在常温下按计量将预聚物的可聚合单体、链转移剂和光引发剂与向列相液晶材料及衬垫料充分搅拌均匀混合;1) Fully stir and evenly mix the polymerizable monomer, chain transfer agent and photoinitiator of the prepolymer with the nematic liquid crystal material and the gasket at room temperature;
2)把混合好的预聚物与向列相液晶及衬垫料转印到两张柔性透明导电膜之间;2) transfer the mixed prepolymer, nematic liquid crystal and spacer between two flexible transparent conductive films;
3)用压合机把印刷了预聚物与液晶混合物的两张柔性透明导电膜挤压成复合膜;3) Extrude two flexible transparent conductive films printed with a mixture of prepolymer and liquid crystal into a composite film with a pressing machine;
4)用中等强度(约25mW)紫外光照射1-3分钟对复合膜进行相分离,使液晶从聚合物中充分析出,形成约2-4微米直径尺寸的液晶微滴。4) Phase-separate the composite film by irradiating with medium-intensity (about 25mW) ultraviolet light for 1-3 minutes, so that the liquid crystal is fully separated from the polymer to form liquid crystal droplets with a diameter of about 2-4 microns.
5)对两张柔性透明导电膜加工出电极引线,在电极间施加直流电场(如25伏),使复合膜(聚合物分散液晶压光效应膜)呈现透明开态;5) Process electrode leads on two flexible transparent conductive films, and apply a DC electric field (such as 25 volts) between the electrodes to make the composite film (polymer dispersed liquid crystal calender effect film) appear transparent and open;
6)去掉电场,聚合物分散液晶压光效应膜呈现散射关态;6) When the electric field is removed, the polymer dispersed liquid crystal calender effect film presents a scattering off state;
7)对聚合物分散液晶压光效应膜在垂直表面方向施加压力约105Pa,液晶微滴中液晶分子将沿薄膜表面排列,液晶微滴又呈现为各向异性单轴晶体,聚合物分散液晶膜处于透明开态。7) Apply a pressure of about 10 5 Pa to the polymer-dispersed liquid crystal calender effect film in the direction vertical to the surface. The liquid crystal film is in a transparent open state.
本发明提供的聚合物分散液晶压光效应膜可以应用于光纤压力传感器,压力触点光阀以及智能触摸窗的应用制造。The polymer-dispersed liquid crystal calender effect film provided by the invention can be applied to the application and manufacture of optical fiber pressure sensors, pressure contact light valves and intelligent touch windows.
本发明与已有技术相比,具有如下的优点:Compared with the prior art, the present invention has the following advantages:
已有的PDLC技术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,电子纸等领域有应用前景。已有的PDLC膜由于聚合物比较坚硬,用力按压也不出现透明漏光现象,而保持在散射状态。由于本发明把聚合物做得如同胶皮一般地比较有弹性,压力作用下观察到明显的从散射膜变成透光膜现象,所以是得到了兼有电光效应和压光效应的多功能膜材料。所以本发明是PDLC新技术方案,可以是PDLC调光玻璃的触摸窗或触点光阀等新产品;可以与光纤技术结合起来,制作液芯光纤压力传感器;或者配制出低折射率PDLC,作为光纤包皮设计新型光纤压力传感器。本发明也为其他的应用提供想象空间。The existing PDLC technology has been used more and more in the field of high-end building decoration as dimming glass, and has application prospects in large-screen display, holographic grating, electronic paper and other fields. The existing PDLC film remains in a scattering state because the polymer is relatively hard, and there is no transparent light leakage phenomenon when pressed hard. Because the present invention makes the polymer more elastic like rubber, and under pressure, it is observed that the phenomenon of changing from a scattering film to a light-transmitting film is obvious, so a multifunctional film material with both electro-optic effect and calender effect has been obtained. . Therefore, the present invention is a new technology solution of PDLC, which can be a new product such as a touch window or a contact light valve of PDLC dimming glass; it can be combined with optical fiber technology to make a liquid core optical fiber pressure sensor; or a low refractive index PDLC can be prepared as Fiber-optic foreskin design for novel fiber-optic pressure sensors. The present invention also provides room for imagination for other applications.
附图说明:Description of drawings:
图1为本发明的聚合物分散液晶压光效应膜结构示意图。Fig. 1 is a schematic diagram of the structure of the polymer-dispersed liquid crystal calender effect film of the present invention.
图2为本发明的聚合物分散液晶压光效应膜工作原理示意图。Fig. 2 is a schematic diagram of the working principle of the polymer-dispersed liquid crystal calender effect film of the present invention.
图3为本发明的聚合物分散液晶压光效应膜制造方法示意图。Fig. 3 is a schematic diagram of the manufacturing method of the polymer-dispersed liquid crystal calender effect film of the present invention.
具体实施方式:Detailed ways:
以下结合附图及实施例对本发明作进一步说明。聚合物分散液晶压光效应膜在超净化车间里进行生产,生产设备主要包括超纯去离子水清洗机,预聚物与液晶混合搅拌机,预聚物涂布机,压合机,平台密封紫外固化机,切片机等。The present invention will be further described below in conjunction with the accompanying drawings and embodiments. The polymer-dispersed liquid crystal calender effect film is produced in the ultra-purification workshop. The production equipment mainly includes ultra-pure deionized water cleaning machine, prepolymer and liquid crystal mixing mixer, prepolymer coating machine, pressing machine, platform sealing UV Curing machine, slicer, etc.
本发明使用的预聚物聚合单体是丙氧基壬苯基丙烯酸酯(20%),三羟甲基丙烷三丙烯酸酯(70%),链转移剂(5%),光引发剂1173(C10H12O2,2-羟基-2-甲基-1-苯丙酮)(5%)。本发明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产品。本发明使用的三羟甲基丙烷三丙烯酸酯是天津天骄化工产品。本发明使用的链转移剂癸二酸,由衢州化工厂生产。本发明使用的光引发剂1173是北京英力科技公司产品。所述的液晶材料是河北鹿泉新型电子材料厂酯类液晶系列产品HLC005,液晶寻常光折射率约为no=1.5,液晶非常光折射率为ne=1.7。所述的透明胶片薄膜可以是导电膜,也可以是不导电透明胶片,为湖南三才公司透明ITO导电膜产品。所述的预聚物与向列相液晶按质量比:1∶1-3;所述的衬垫料直径是约10微米塑料微球,可以是深圳纳微科技公司的产品,塑料微球含量为10-30个/mm2。The prepolymer polymerization monomer that the present invention uses is propoxy nonyl phenyl acrylate (20%), trimethylolpropane triacrylate (70%), chain transfer agent (5%), photoinitiator 1173 ( C 10 H 12 O 2 , 2-hydroxy-2-methyl-1-propiophenone) (5%). The propoxy nonyl phenyl acrylate used in the present invention is a product of Cytec Special Surface Technology Co., Ltd. of the United States. The trimethylolpropane triacrylate used in the present invention is a product of Tianjin Tianjiao Chemical Industry. The chain transfer agent sebacic acid used in the present invention is produced by Quzhou Chemical Factory. The photoinitiator 1173 used in the present invention is a product of Beijing Yingli Technology Co., Ltd. The liquid crystal material mentioned is HLC005 , an ester liquid crystal series product of Hebei Luquan New Electronic Material Factory. The transparent film film can be a conductive film or a non-conductive transparent film, which is a transparent ITO conductive film product of Hunan Sancai Company. The mass ratio of the prepolymer to the nematic liquid crystal is 1:1-3; the diameter of the spacer is plastic microspheres of about 10 microns, which can be products of Shenzhen Nawei Technology Co., Ltd., and the content of plastic microspheres is 10-30 pieces/mm 2 .
参见图1,本发明的聚合物分散液晶压光效应膜结构示意图。柔性透明胶片101,105上面有透明导电薄层电极102,104,中间夹着聚合物分散液晶层103。聚合物分散液晶层103厚度10μm,液晶微滴106平均直径约2-4μm,聚合物折射率选择约为np=1.6,液晶寻常光折射率约no=1.5,非常光折射率ne=1.7。Referring to FIG. 1 , it is a schematic diagram of the structure of the polymer-dispersed liquid crystal calender effect film of the present invention. The flexible
参见图2,在电极间施加约25伏电场,使液晶分子转向电场方向,膜呈现透明开态201。去掉电场,聚合物分散液晶压光效应膜呈现散射关态202。垂面施加压力时,液晶微滴变形,液晶分子沿面排列,液晶折射率取面平均折射率<n>=1.6,与聚合物折射率np相匹配,呈现透光开态效果203。去掉压力恢复到散射状态202。Referring to FIG. 2 , an electric field of about 25 volts is applied between the electrodes to make the liquid crystal molecules turn to the direction of the electric field, and the film assumes a transparent open state 201 . When the electric field is removed, the polymer-dispersed liquid crystal calender effect film exhibits a scattering off
参见图3,本发明的聚合物分散液晶压光效应膜制造方法示意图。Referring to FIG. 3 , it is a schematic diagram of the manufacturing method of the polymer-dispersed liquid crystal calender effect film of the present invention.
A、在常温下,预聚物(丙氧基壬苯基丙烯酸酯(20%),三羟甲基丙烷三丙烯酸酯(70%),链转移剂(5%),光引发剂1173(5%))与液晶材料及适量的10微米的衬垫料充分搅拌均匀混合,预聚物与向列相液晶按1∶1-3比例混合。A, at normal temperature, prepolymer (propoxynonyl phenyl acrylate (20%), trimethylolpropane triacrylate (70%), chain transfer agent (5%), photoinitiator 1173 (5%) %)) and the liquid crystal material and an appropriate amount of 10-micron spacer are thoroughly stirred and evenly mixed, and the prepolymer and the nematic liquid crystal are mixed in a ratio of 1:1-3.
B、外面两张柔性透明导电膜内侧刻蚀出电极102,104;B. The
C、把混合好的预聚物与向列相液晶及衬垫料转印涂布到301有共面电极的两张柔性透明导电膜302,303之间;C. transfer the mixed prepolymer, nematic liquid crystal and spacer to 301 between two flexible transparent
D、用压合机把涂布了预聚物与液晶混合物的两张柔性透明导电膜挤压成复合膜304;D. Extrude two flexible transparent conductive films coated with a prepolymer and a liquid crystal mixture into a
E、对复合膜进行相分离,使液晶从聚合物中充分析出,当形成平均直径约2-4微米的液晶微滴时进行固化(相分离及固化处理是紫外光固化技术)。E. Phase separation is carried out on the composite film, so that the liquid crystal is fully separated from the polymer, and solidified when forming liquid crystal droplets with an average diameter of about 2-4 microns (phase separation and curing treatment are ultraviolet curing technology).
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