聚合物分散液晶膜的制备及光学性能的研究
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摘要
液晶不仅作为显示材料已经被广泛应用于各种显示器件,而且液晶的新性能的研究对国民经济以及现代化的发展具有重要作用。液晶作为显示材料主要被应用于手机、电脑、笔记本、大屏幕显示等方面；而液晶高分子由于具有高模量,高弹性等优点而被应用于高性能纤维材料、防弹衣、显示等领域；液晶离聚物又以其独特性能而被广泛的研究。近几年来,作为新兴的液晶材料：液晶离聚物和聚合物分散液晶,引起广大研究者极大的研究兴趣。聚合物分散液晶(polymer dispersed liquid crystals, PDLCs)膜是一种新型的功能性液晶复合材料,在PDLC膜中,液晶微滴以纳米或微米数量级分散在固态聚合物基体中。由于聚合物具有高敏感性、宽动态范围和高分辨率、相对较快的响应时间,且能廉价地做成各种形状、各种厚度的薄膜,而得到广大研究者的青睐。
PDLC膜主要通过相分离法制备,即将预聚物与小分子液晶制备成均一混合物,通过引发预聚物聚合(缩聚反应,自由基聚合,光引发聚合等),随着聚合物分子量的增长,液晶在预聚物中的溶解度降低,导致液晶与聚合物两相分离,实现PDLC膜的制备。也可以通过聚合物与小分子液晶共溶于相同溶剂,再经溶剂挥发分离成聚合物与液晶两相,实现PDLC膜的制备。微胶囊法也是制备PDLC膜的一种有效手段,但程序过于复杂。
当在PDLC膜两端施加一定的电场时,液晶微滴中分子指向矢沿电场方向一致取向,若选取的液晶分子长轴折射率(no)与高分子折射率(np)匹配,则PDLC膜呈透射态；当外加电场消失,由于液晶分子与聚合物基体界面之间的锚定作用,液晶分子指向矢杂乱分布。此时,液晶微滴的有效折射率与基体折射率失配,则PDLC膜呈散射态。可以理解为,当聚合物与液晶界面强锚定时,液晶分子的垂面取向生成辐射分布,液晶分子的沿面取向生成双极分布,呈现散射态；当施加电场时液晶分子沿电场方向排列生成轴向排列,呈现透射态。
PDLC膜作为显示材料较之传统的Liquid Crystal Display(LCD)有着无可比拟的优势：PDLC显示材料具有不需偏光片、亮度高、视角宽、不需液晶取向层等优点。由于PDLC膜材料具有不需要偏振片、两基板间距离不需严格控制、基板内表面不需要取向处理等优点,故在制备柔软、高亮度、宽视角的大面积液晶显示方面具有广阔的应用前景。因此,PDLC材料的电控光学特性及其时间响应特性备受人们关注,国内外很多研究小组都对其进行了深入广泛的研究。目前,制作同时具有对比度高、阈值和饱和电压低、响应速度快、稳定性高的PDLC膜材料还很困难,这就限制了PDLC膜材料的应用。影响PDLC膜性能的主要因素有以下几个方面：(1)所采用的原材料的结构与性能；(2)PDLC薄膜内的相分离状态；(3)聚合物基体相的介电性能；(4) PDLC膜的制备条件等。
本文采用含有三官能团的丙烯酸酯交联剂和环氧树脂作为聚合物基体相的预聚物,三官能团的预聚物能够在紫外光引发下实现快速聚合,通过快速聚合制备了分散于聚合物基体相中的小粒径的液晶微滴。本文通过紫外光引发聚合致相分离法制备了4个系列PDLC膜,并通过手性分子,纳米石墨,可聚合极性小分子的掺杂,改善了PDLC膜的电光性能。本文主要研究工作如下：
(1)制备了具有手性的PDLC膜,分别研究了热场和电场作用下手性聚合物分散液晶的热光和电光性能的变化；热场和电场作用下PDLC膜的旋光性能变化与de Vries理论相一致；并通过偏光显微镜、扫描电镜和三维红外图像对PDLC膜内聚合物与液晶相态进行了研究。
(2)制备了纳米石墨掺杂下PDLC膜,通过测量PDLC膜的电光性能可知通过纳米石墨掺杂改善了聚合物基体相的介电性能,从而降低了PDLC膜的阈值电压和驱动电压。
(3)制备了丙烯酸单体掺杂的PDLC膜,通过实时透射率变化分析了不同浓度的丙烯酸单体对PDLC膜制备过程中的动力学影响。
(4)制备了不同的可聚合极性小分子掺杂的PDLC膜,通过实时透射率变化的观察获得了不同小分子作用下的聚合动力学；研究了不同单体掺杂对PDLC膜的电光性能影响。
总之,本文的研究不仅拘泥于研究制备条件对PDLC膜的影响,而且侧重于PDLC膜电光性能的改善,通过对聚合物基体相介电性能的改善和可聚合极性小分子的掺杂对PDLC膜的电光性能加以改善。本文对PDLC膜电光性能的改善提供了有效手段。
The liquid crystals are used to parts of a display apparatus widely as display materials. The study on new performance of liquid crystals propels the development of economy and modernization. The liquid crystals are used to mobile, computer, notebook PC and bigger display as display materials. The liquid crystal polymer is used to fibre materials, bullet-proof clothing and display because of the high modulus and highly elastic performance. The liquid crystal inomers are interested for the particular performance by pursuers. The liquid crystal inomer and PDLC are interested by pursuers as a novel kind of liquid crystals material lately. PDLC are a novel functional liquid crystal composites material. The liquid crystal droplets are dispersed in polymer matrix in nano-or micrometer. The novel liquid crystal materials are interested for the high sensitivity, widely dynamic, high resolving power, rapidly response time and easy molding of polymer.
The PDLC films are fabricated by phase separation. The prepolymer and liquid crystal are mixed in homogeneous mixture. When the prepolymer was polymerized by polycondensation, radical polymerization or light-initiated polymerization, the chains of polymer are lengthened and the solubility of liquid crystal is shrunk. The PDLC films are fabricated by phase separation of polymer and liquid crystal. The PDLC films are fabricated by solvent evaporation in mixture of polymer and liquid crystals which dissolved in same solvent. The microcapsule is an effective method to fabricate the PDLC films.
The director of liquid crystal droplets is orientated to direction of electric field when the electric field was applied to PDLC films. When the refractive index of liquid crystal equals to polymer, the PDLC film is transparent state. When the electric field is removed, the PDLC films is scattering state for the director of liquid crystal is clutter and the refractive index of liquid crystal not match to polymer. We can comprehend that the liquid crystal droplets are bipolar ellipsoid for the high anchoring energy between polymer and liquid crystals and presented scattering state. The director of liquid crystal was homogeneous orientated to electric field and presented transparent state.
The merit of PDLC films are none-polarizer, high brightness, wide angle and none-alignment layer as to traditional LCD. The PDLC films are potential used to bigger display for the novel merit. The electro-optic and response time properties of PDLC films are widely study by lots of team. At present, it is difficulty to fabricate high contrast, low threshold and saturation voltage, rapid responsiveness and high stability PDLC films. To influence the performance of PDLC films' factor are (1) the performance and structure of materials;(2) the morphology of PDLC films;(3) the dielectric of polymer matrix;(4) the condition of the fabrication of PDLC films.
In this paper, the polymer matrix is composed by tri-functional prepolymer and epoxy resins. The smaller liquid crystal droplets are obtained by rapid polymerization which initiated by ultraviolet lights in tri-functional prepolymer. We fabricate four series of PDLC films which composed by chiral liquid crystal, nano-graphites and polymerizable polar molecules respectively. The doped materials enhance the electro-optical performance of PDLC films. The main works in this paper are as following:
(1) Effect of thermal and electric field on optical performance of chiral PDLC film are studied. The changes of optic rotation which affect by thermal and electric field are equal to theory of de Vries. The morphology of chiral PDLC film is observed by POM, SEM and infrared images. The diameter of liquid crystal droplets is estimated by infrared images and POM photographs and obtains the same results in5μm.
(2) The nano-graphites doped PDLC films are fabricated. The doped nano-graphites enhance the dielectric of polymer and reduce the threshold and saturation voltage.
(3) We fabricate the acrylic acid doped PDLC films. The effect of doped acrylic acid on kinetic of polymerization is observed by change of real time transmittance. The doped acrylic acid improves the electro-optic of PDLC films according the reducing of threshold and saturation voltage.
(4) The kinetic of polymerization of polymerizable polar molecules doped PDLC films is studied by changing of real time transmittance. The effect of doped polymerizable polar molecules on electro-optic of PDLC films is studied.
In summery, the research of present study not only in the further investigation on the effect of polymerization condition on polymerization induced phase separation, but also in the improvement of electro-optical performance of PDLC films. The doped nano-graphites, pelymerizable polar molecules are effectively improving the performance of PDLC films.
PDLC膜主要通过相分离法制备,即将预聚物与小分子液晶制备成均一混合物,通过引发预聚物聚合(缩聚反应,自由基聚合,光引发聚合等),随着聚合物分子量的增长,液晶在预聚物中的溶解度降低,导致液晶与聚合物两相分离,实现PDLC膜的制备。也可以通过聚合物与小分子液晶共溶于相同溶剂,再经溶剂挥发分离成聚合物与液晶两相,实现PDLC膜的制备。微胶囊法也是制备PDLC膜的一种有效手段,但程序过于复杂。
当在PDLC膜两端施加一定的电场时,液晶微滴中分子指向矢沿电场方向一致取向,若选取的液晶分子长轴折射率(no)与高分子折射率(np)匹配,则PDLC膜呈透射态；当外加电场消失,由于液晶分子与聚合物基体界面之间的锚定作用,液晶分子指向矢杂乱分布。此时,液晶微滴的有效折射率与基体折射率失配,则PDLC膜呈散射态。可以理解为,当聚合物与液晶界面强锚定时,液晶分子的垂面取向生成辐射分布,液晶分子的沿面取向生成双极分布,呈现散射态；当施加电场时液晶分子沿电场方向排列生成轴向排列,呈现透射态。
PDLC膜作为显示材料较之传统的Liquid Crystal Display(LCD)有着无可比拟的优势：PDLC显示材料具有不需偏光片、亮度高、视角宽、不需液晶取向层等优点。由于PDLC膜材料具有不需要偏振片、两基板间距离不需严格控制、基板内表面不需要取向处理等优点,故在制备柔软、高亮度、宽视角的大面积液晶显示方面具有广阔的应用前景。因此,PDLC材料的电控光学特性及其时间响应特性备受人们关注,国内外很多研究小组都对其进行了深入广泛的研究。目前,制作同时具有对比度高、阈值和饱和电压低、响应速度快、稳定性高的PDLC膜材料还很困难,这就限制了PDLC膜材料的应用。影响PDLC膜性能的主要因素有以下几个方面：(1)所采用的原材料的结构与性能；(2)PDLC薄膜内的相分离状态；(3)聚合物基体相的介电性能；(4) PDLC膜的制备条件等。
本文采用含有三官能团的丙烯酸酯交联剂和环氧树脂作为聚合物基体相的预聚物,三官能团的预聚物能够在紫外光引发下实现快速聚合,通过快速聚合制备了分散于聚合物基体相中的小粒径的液晶微滴。本文通过紫外光引发聚合致相分离法制备了4个系列PDLC膜,并通过手性分子,纳米石墨,可聚合极性小分子的掺杂,改善了PDLC膜的电光性能。本文主要研究工作如下：
(1)制备了具有手性的PDLC膜,分别研究了热场和电场作用下手性聚合物分散液晶的热光和电光性能的变化；热场和电场作用下PDLC膜的旋光性能变化与de Vries理论相一致；并通过偏光显微镜、扫描电镜和三维红外图像对PDLC膜内聚合物与液晶相态进行了研究。
(2)制备了纳米石墨掺杂下PDLC膜,通过测量PDLC膜的电光性能可知通过纳米石墨掺杂改善了聚合物基体相的介电性能,从而降低了PDLC膜的阈值电压和驱动电压。
(3)制备了丙烯酸单体掺杂的PDLC膜,通过实时透射率变化分析了不同浓度的丙烯酸单体对PDLC膜制备过程中的动力学影响。
(4)制备了不同的可聚合极性小分子掺杂的PDLC膜,通过实时透射率变化的观察获得了不同小分子作用下的聚合动力学；研究了不同单体掺杂对PDLC膜的电光性能影响。
总之,本文的研究不仅拘泥于研究制备条件对PDLC膜的影响,而且侧重于PDLC膜电光性能的改善,通过对聚合物基体相介电性能的改善和可聚合极性小分子的掺杂对PDLC膜的电光性能加以改善。本文对PDLC膜电光性能的改善提供了有效手段。
The liquid crystals are used to parts of a display apparatus widely as display materials. The study on new performance of liquid crystals propels the development of economy and modernization. The liquid crystals are used to mobile, computer, notebook PC and bigger display as display materials. The liquid crystal polymer is used to fibre materials, bullet-proof clothing and display because of the high modulus and highly elastic performance. The liquid crystal inomers are interested for the particular performance by pursuers. The liquid crystal inomer and PDLC are interested by pursuers as a novel kind of liquid crystals material lately. PDLC are a novel functional liquid crystal composites material. The liquid crystal droplets are dispersed in polymer matrix in nano-or micrometer. The novel liquid crystal materials are interested for the high sensitivity, widely dynamic, high resolving power, rapidly response time and easy molding of polymer.
The PDLC films are fabricated by phase separation. The prepolymer and liquid crystal are mixed in homogeneous mixture. When the prepolymer was polymerized by polycondensation, radical polymerization or light-initiated polymerization, the chains of polymer are lengthened and the solubility of liquid crystal is shrunk. The PDLC films are fabricated by phase separation of polymer and liquid crystal. The PDLC films are fabricated by solvent evaporation in mixture of polymer and liquid crystals which dissolved in same solvent. The microcapsule is an effective method to fabricate the PDLC films.
The director of liquid crystal droplets is orientated to direction of electric field when the electric field was applied to PDLC films. When the refractive index of liquid crystal equals to polymer, the PDLC film is transparent state. When the electric field is removed, the PDLC films is scattering state for the director of liquid crystal is clutter and the refractive index of liquid crystal not match to polymer. We can comprehend that the liquid crystal droplets are bipolar ellipsoid for the high anchoring energy between polymer and liquid crystals and presented scattering state. The director of liquid crystal was homogeneous orientated to electric field and presented transparent state.
The merit of PDLC films are none-polarizer, high brightness, wide angle and none-alignment layer as to traditional LCD. The PDLC films are potential used to bigger display for the novel merit. The electro-optic and response time properties of PDLC films are widely study by lots of team. At present, it is difficulty to fabricate high contrast, low threshold and saturation voltage, rapid responsiveness and high stability PDLC films. To influence the performance of PDLC films' factor are (1) the performance and structure of materials;(2) the morphology of PDLC films;(3) the dielectric of polymer matrix;(4) the condition of the fabrication of PDLC films.
In this paper, the polymer matrix is composed by tri-functional prepolymer and epoxy resins. The smaller liquid crystal droplets are obtained by rapid polymerization which initiated by ultraviolet lights in tri-functional prepolymer. We fabricate four series of PDLC films which composed by chiral liquid crystal, nano-graphites and polymerizable polar molecules respectively. The doped materials enhance the electro-optical performance of PDLC films. The main works in this paper are as following:
(1) Effect of thermal and electric field on optical performance of chiral PDLC film are studied. The changes of optic rotation which affect by thermal and electric field are equal to theory of de Vries. The morphology of chiral PDLC film is observed by POM, SEM and infrared images. The diameter of liquid crystal droplets is estimated by infrared images and POM photographs and obtains the same results in5μm.
(2) The nano-graphites doped PDLC films are fabricated. The doped nano-graphites enhance the dielectric of polymer and reduce the threshold and saturation voltage.
(3) We fabricate the acrylic acid doped PDLC films. The effect of doped acrylic acid on kinetic of polymerization is observed by change of real time transmittance. The doped acrylic acid improves the electro-optic of PDLC films according the reducing of threshold and saturation voltage.
(4) The kinetic of polymerization of polymerizable polar molecules doped PDLC films is studied by changing of real time transmittance. The effect of doped polymerizable polar molecules on electro-optic of PDLC films is studied.
In summery, the research of present study not only in the further investigation on the effect of polymerization condition on polymerization induced phase separation, but also in the improvement of electro-optical performance of PDLC films. The doped nano-graphites, pelymerizable polar molecules are effectively improving the performance of PDLC films.
引文
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