高透明性聚醯亞胺混成複合材料合成與光電應用之研究

蔡家量

doi:10.6342/NTU201603072

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高透明性聚醯亚胺混成复合材料合成与光电应用之研究

Synthesis and Characterization of Highly Transparent Polyimide Hybrid Materials for Optoelectronic Applications

蔡家量 , 博士　　导师：刘贵生　　

英文 DOI： 10.6342/NTU201603072

聚醯亚胺；二氧化钛；二氧化锆；混掺材料；光学透明度；折射率；电阻式记忆体； Polyimide ； TiO2 ； ZrO2 ； Hybrid material ； Optical transparency ； Refractive index ； resistive memory

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摘要 │ 参考文献 (173) │ 国际计量

摘要〈TOP〉

本论文分成六个章节，第一章为总体序论。第二章由一新的简便合成方法来合成含有羟基可溶性Polyimidothioethers(PITEs)并由其制备polyimidothioethers-奈米晶二氧化钛（PITEs-TiO2）且具有高的二氧化钛含量（~50wt％）和厚度达15±3um的光学膜。此外，透明可绕的聚醯亚胺-奈米晶二氧化钛(PI/TiO2)的混合具有高的二氧化钛含量（~50wt％）和厚度达15±3um的光学膜由新的可溶性含有羟基之聚醯亚胺Polyimide(PI)所制备而成。羟基在PITEs和PI的骨干可以提供有机-无机键结点并且通过控制丁醇钛/羟基的莫耳比来制备获得均匀之混成溶液。由此方法可成功获得可绕有机无机混成膜，并拥有良好的表面平坦性，热尺寸稳定性，可调谐的折射率（1.63至1.80，在633nm波长下），和高的光学透明度。基於此系列之有机无机复合膜所制备三层抗反射涂层具有在可见光范围内小於0.5％的反射率，显示其潜在的光学应用性。
然而，在所获得之PI-TiO2的光学穿透度光谱中显示，因TiO2的能隙(3.2eV)使得在400 nm波长的穿透度有明显得减少，而导致复合膜有淡黄色的颜色。所以，在此有机-无机混掺系统中，选择之无机材料不仅需要能够提升折射率，更为重要的是能够保有原PI的光学透明度。因此，第三章成功制备出高热稳定性含二氧化锆的聚醯亚胺混成膜（PI/ZO2），且具有优良的光学透明性。所得到的ZrO2奈米粒子不仅可以良好地分散在聚醯亚胺基材中，此PI/ZO2复合薄膜也显示了优异的光学透明度，可调谐的折射率和阿贝数，分别高达1.804和32.18，这对於光学元件是至关重要的。此外，由於ZO2具有较大的能隙，故PI/ ZO2混合膜对比於相应的PI/ TiO2系统在可见光区域也表现出高阿贝数和透明性。因此，本研究表明，PI/ ZO2复合薄膜具有更优异的优点来应用於光学元件上。
第四章则由, 4’-bis(4-amino-3-hydroxyphenylthio)diphenylsulfide (3SOH-DA) 二胺和4,4’-(hexafluoroisopropylidene)diphthalic anhydride (6FDA)二酸酐合成出一种新颖的可溶液加工的具有羟基链侧基和含硫之poly(o-hydroxy-imide) 3SOH-6FPI并应用於记忆体元件上。为了提高元件的记忆行为，导入不同量的TiO2於3SOH-6FPI中并探讨TiO2的含量相应的元件记忆行为。混成膜中由不同TiO2含量0wt％至50wt％明显增其记忆时间，由DRAM，SRAM至WROM的可调控记忆时间之存储元件且具有高的开/关电流比（108）。另外，由电流-电压IV特性的结果显示，结晶相的TiO2拥有更高的电荷捕集能力，使元件在ON的状态有更长的停留时间。
在第五章中，更进一步设计及合成一系列含有具有羟基链侧基和含硫之聚醯亚胺3SOH-RPI，且由导入不同拉电子能力的二酸酐（CHDA < 6FDA < DSDA）到聚醯亚胺主链上，而得到相对应的记忆体储存行为（None, DRAM, SRAM）。且为了提高元件的记忆行为，导入不同含量的ZrO2於3SOH-RPI中并探讨ZrO2的含量相应的元件记忆行为。此外，也比较由含有不同HOMO和LUMO能阶的ZrO2和TiO2导入混掺系统中，来比较相同无机含量下，对元件记忆行为的影响。第六章节为结论。

并列摘要〈TOP〉

This study has been separated into six chapters. Chapter 1 is general introduction. In Chapter 2, a new facile synthetic route were developed to prepare flexible polyimidothioethers-nanocrystalline-titania (PITEs/TiO2) and polyimides–nanocrystalline-titania (PIs/TiO2) hybrid optical thin films with high titania content up to 50 wt% and thickness of 15 µm. The hydroxyl groups at the backbone of the PITEs and PIs could provide the organic-inorganic bonding sites and resulted in homogeneous hybrid solutions by controlling the mole ratio of titanium butoxide/hydroxyl group. The flexible hybrid films were successfully obtained and revealed good surface planarity, thermal dimensional stability, tunable refractive index (1.63 to 1.80 at 633 nm), and high optical transparency. In addition three-layer anti-reflection coating based on the hybrid films was prepared and showed a low reflectance 0.5% in the visible range indicated its potential on optical applications.
However, the optical transparency of the obtained PI/TiO2 hybrid films reduced dramatically at wavelength around 400 nm attributed to the low band gap of TiO2 (3.2 eV), resulting in pale yellow color of the hybrid films. Thus, by choosing species of inorganic materials in the hybrid system for enhancing the refractive index without optical transparency in visible light region is an important issue. Therefore, chapter 3 describes the novel thermally stable zirconia-containing polyimides (PI/ZrO2) with excellent optical properties have been prepared successfully. Thus, the zirconia nanoparticles were well dispersed in polyimide matrix. The obtained flexible PI/ZrO2 hybrid films revealed excellent optical transparency, tunable refractive index and Abbe number up to 1.804 and 32.18, respectively. In addition, the PI/ZrO2 hybrid films also exhibit higher Abbe number and transparency in visible light region than the corresponding PI/TiO2 system due to larger energy band gap of ZrO2. Thus, the study demonstrates the PI/ZrO2 film based on its advantages and potential is more superior for optical application.
In the other hand, chapter 4 introduce a novel solution-processable sulfur-containing poly(o-hydroxy-imide) 3SOH-6FPI with pendant hydroxyl groups and the corresponding polyimide 3SOH-6FPI/TiO2 hybrids were synthesized from the diamine 4,4’-bis(4-amino-3-hydroxyphenylthio)diphenylsulfide (3SOH-DA) and  4,4’-(hexafluoroisopropylidene)diphthalic anhydride (6FDA), for memory application. To enhance the memory behavior, different amounts of TiO2 were introduced into 3SOH-6FPI and investigated the corresponding tunable memory properties. The resulting hybrid films having different TiO2 concentration from 0 wt% to 50 wt% exhibited electrically programmable digital memory properties from DRAM, SRAM, to WROM with high ON/OFF current ratio (108). Furthermore, according to the results of the current-voltage I-V characteristics, the crystalline phase of titania reveals higher trapping ability to increase the retention time at the ON state. In order realize the switching mechanism of 3SOH-6FPI/TiO2 hybrids memory devices, molecular simulation and electrode effect were also discussed in this study. 
  Moreover, chapter 5 describes the series solution-processable sulfur-containing poly(o-hydroxy-imide)s 3SOH-RPI with pendant hydroxyl groups and the corresponding 3SOH-RPI/ZrO2 PI hybrids were synthesized from the diamine 3SOH-DA and dianhydrides of CHDA, 6FDA, and DSDA, respectively, for memory application. By introducing acceptors with different electron-withdrawing capability (CHDA < 6FDA < DSDA) into polyimide backbones, the obtained polymer memory devices show the memory behaviors of None, DRAM, and SRAM, respectively. In order to facilitate and enhance the memory effects, different amounts of ZrO2 were incorporated into 3SOH-RPI to investigate the corresponding memory properties. Moreover, in order to deeply confirm the memory switching mechanism of 3SOH-RPI/ZrO2 hybrids, the devices fabricated both from PI/ZrO2 and PI/TiO2 hybrid films were used to demonstrate the effect of LUMO energy level of ZrO2 and TiO2 on the memory characteristics and retention time in this study. Chapter 6 conclusions.

参考文献 ( 173 ) 〈TOP〉

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