SPLC杂化液晶及其衍生介孔材料的制备、结构表征与热致喷射效应
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摘要
上世纪八十年代中期,纳米材料成了材料科学和凝聚态物理研究领域的研究热点。到九十年代中期,在纳米结构单元基础上的自组装体系又成了纳米材料研究的最前沿。介孔材料(Mesoporous Materials)是这类纳米自组装材料中的重要一类。介孔材料具有许多优异的特点,比如制备方法多是对环境友好的软溶液法,材料的孔径在2～30nm 之间可调,并且孔径尺寸、形状和排列规整,还有就是介孔材料具有较高的表面积和孔体积(如SiO_2 基MCM-41:1050m~2/g 和0.93cm~3/g)。这些特点使得介孔材料在化学、物理、材料、生物、医学及信息等领域里都展示出广阔的应用前景。到目前为止,介孔材料的工业应用已在催化和吸附方面取得了成功。在其他的应用方面中,大面积功能介孔材料具有非常高的价值。美国新墨西哥大学的C.J. Brinker 研究组成功地采用了浸渍涂层工艺(一次浸渍所形成的膜的厚度约为0.5 微米),通过控制溶剂的蒸发制备了具有各种微观对称结构和宏观形貌的大面积介孔薄膜材料。
本研究工作采用SPLC(Silica-PE6400 Liquid Crystal)方法制备了厚度约1.2毫米的介孔薄膜和介孔块体产物PTO-1 等,并发现了此类较厚介孔产物的纳米新特性-“热致喷射效应”。此种介孔材料的新纳米效应在国内外均未见报导。
热致喷射效应的机理为一定温度时,介孔孔道内部结构导向剂(PE6400)胶束在孔内部高温高压水蒸汽的作用下,快速喷射出孔道的物理失重过程,而并非由PE6400 的氧化分解所引起。该效应的发生温度受介孔材料的孔径尺寸、分布和胶束-孔壁界面层作用力影响,可以明显低于(薄膜:低于40.3℃;PTO-1:低于23.3℃)或高于(改性PTO-1:高过62.6℃)宏观PE6400 的氧化分解温度(256.1℃);另一方面,介孔薄膜、PTO-1 和KH580 改性PTO-1 的热致喷射效应的温度跨度较PE6400 的分解温度跨度分别窄了106.5℃、98.8℃和96.6℃。
热致喷射效应是纳米效应的一种新的表现形式。其发生应当不仅仅局限于介孔材料,任何拥有纳米多孔结构的体系在适当的条件下都可能发生该效应,具有一定的普遍意义。热致喷射效应还具有重要的实用价值。它可以被用来作为一种通用的介孔材料孔径分布测试新方法;也可以用于研究客体分子的纳米效应(或行为);最后,还可以作为客体物质的一种存储-释放机制来使用。
另外,本文以普通工业表面活性剂PE6400(EO10PO30EO10)为新型结构导向剂,成功地制备了SPLC 杂化液晶及其衍生透明介孔薄膜、块状PTO-1 和有机改性PTO-1 等一系列大面积杂化介孔产物。详细研究了各反应组分和合成条件对结构规整程度的影响规律。该研究成果为利用工业表面活性剂生产大面积介孔器件材料
In the middle eighties of the twentieth century, nano-materials had become the most advanced researching field of materials science and solid-state physics. And when it reached the middle of nineties, the self-assembled system with nano-building-block became the focus of the research on nano-materials. Mesoporous material is an important kind of such self-assembled materials. Mesoporous materials possess many excellent characteristics such as environmental benign preparing method of soft solution, adjustable pore diameter between 2 nm to 30 nm and high surface area and porosity (for silica based MCM-41: 1050m~2/g and 0.93cm~3/g, respectively). Benefiting from these advantages, mesoporous materials were considered having great potentials in the fields of chemistry, physics, materials science, biology, medicine and information. Nowadays, mesoporous materials have been found to be successful in catalysis and absorption applications. In other application fields, large area functional mesoporous materials possess great potential. C.J. Brinker group from University of New Mexico has successfully prepared large area membrane materials possessing various micro-symmetric structures and macro-morphologies by dip coating process (membrane thickness of 0.5 micrometer each time) through controlling the solvent evaporation.
Mesoporous membrane and bulk mesoporous product PTO-1 with roughly 1.2 millimeter thickness was successfully prepared by using SPLC (Silica-PE6400 Liquid Crystal) method. A novel nano-effect from these mesoporous products, named “Thermal-Ejecting Effect”was firstly discovered and studied.
The formation mechanism for Thermal-Ejecting Effect is identified as the fast physical ejection of PE6400 micelles from inside pore channels by the driven of high temperature and pressure steam under certain temperature. This effect is not induced by PE6400 decomposing in oxygen atmosphere. The temperature of Thermal-Ejection Effect is dominated by pore size and its distribution and the interactions between PE6400 micelles and pore wall, which may be lower (for membrane: 40.3℃lower; for PTO-1: 23.3℃lower) or higher (for KH580 modified PTO-1: 62.6℃higher) than that of PE6400 decomposing (256.1℃). On the other hand, the temperature ranges for mesoporous membrane, PTO-1 and KH580 modified PTO-1 are 106.5℃, 98.8℃and 96.6℃narrower than that of PE6400 decomposing.
本研究工作采用SPLC(Silica-PE6400 Liquid Crystal)方法制备了厚度约1.2毫米的介孔薄膜和介孔块体产物PTO-1 等,并发现了此类较厚介孔产物的纳米新特性-“热致喷射效应”。此种介孔材料的新纳米效应在国内外均未见报导。
热致喷射效应的机理为一定温度时,介孔孔道内部结构导向剂(PE6400)胶束在孔内部高温高压水蒸汽的作用下,快速喷射出孔道的物理失重过程,而并非由PE6400 的氧化分解所引起。该效应的发生温度受介孔材料的孔径尺寸、分布和胶束-孔壁界面层作用力影响,可以明显低于(薄膜:低于40.3℃;PTO-1:低于23.3℃)或高于(改性PTO-1:高过62.6℃)宏观PE6400 的氧化分解温度(256.1℃);另一方面,介孔薄膜、PTO-1 和KH580 改性PTO-1 的热致喷射效应的温度跨度较PE6400 的分解温度跨度分别窄了106.5℃、98.8℃和96.6℃。
热致喷射效应是纳米效应的一种新的表现形式。其发生应当不仅仅局限于介孔材料,任何拥有纳米多孔结构的体系在适当的条件下都可能发生该效应,具有一定的普遍意义。热致喷射效应还具有重要的实用价值。它可以被用来作为一种通用的介孔材料孔径分布测试新方法;也可以用于研究客体分子的纳米效应(或行为);最后,还可以作为客体物质的一种存储-释放机制来使用。
另外,本文以普通工业表面活性剂PE6400(EO10PO30EO10)为新型结构导向剂,成功地制备了SPLC 杂化液晶及其衍生透明介孔薄膜、块状PTO-1 和有机改性PTO-1 等一系列大面积杂化介孔产物。详细研究了各反应组分和合成条件对结构规整程度的影响规律。该研究成果为利用工业表面活性剂生产大面积介孔器件材料
In the middle eighties of the twentieth century, nano-materials had become the most advanced researching field of materials science and solid-state physics. And when it reached the middle of nineties, the self-assembled system with nano-building-block became the focus of the research on nano-materials. Mesoporous material is an important kind of such self-assembled materials. Mesoporous materials possess many excellent characteristics such as environmental benign preparing method of soft solution, adjustable pore diameter between 2 nm to 30 nm and high surface area and porosity (for silica based MCM-41: 1050m~2/g and 0.93cm~3/g, respectively). Benefiting from these advantages, mesoporous materials were considered having great potentials in the fields of chemistry, physics, materials science, biology, medicine and information. Nowadays, mesoporous materials have been found to be successful in catalysis and absorption applications. In other application fields, large area functional mesoporous materials possess great potential. C.J. Brinker group from University of New Mexico has successfully prepared large area membrane materials possessing various micro-symmetric structures and macro-morphologies by dip coating process (membrane thickness of 0.5 micrometer each time) through controlling the solvent evaporation.
Mesoporous membrane and bulk mesoporous product PTO-1 with roughly 1.2 millimeter thickness was successfully prepared by using SPLC (Silica-PE6400 Liquid Crystal) method. A novel nano-effect from these mesoporous products, named “Thermal-Ejecting Effect”was firstly discovered and studied.
The formation mechanism for Thermal-Ejecting Effect is identified as the fast physical ejection of PE6400 micelles from inside pore channels by the driven of high temperature and pressure steam under certain temperature. This effect is not induced by PE6400 decomposing in oxygen atmosphere. The temperature of Thermal-Ejection Effect is dominated by pore size and its distribution and the interactions between PE6400 micelles and pore wall, which may be lower (for membrane: 40.3℃lower; for PTO-1: 23.3℃lower) or higher (for KH580 modified PTO-1: 62.6℃higher) than that of PE6400 decomposing (256.1℃). On the other hand, the temperature ranges for mesoporous membrane, PTO-1 and KH580 modified PTO-1 are 106.5℃, 98.8℃and 96.6℃narrower than that of PE6400 decomposing.
引文
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