胆酸类聚集体在材料合成中的模板调控作用研究
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摘要
生物矿化是研究生物矿物及其复杂多级结构形成过程的科学。化学工作者在这一领域的工作大致可以分为三个方向：(1)对生物材料的分析；(2)设计体外模型环境对生理条件进行模拟,如凝胶体系；(3)开发新的材料合成仿生方法,如模板法。
在本论文的工作中,我们首先利用仿生模板法合成了具有中空结构的二氧化硅微球,之后研究了无机晶体在水凝胶体系中的高度取向生长,最后在多孔聚合物基体上制备了导电聚合物杂化材料。分别概述如下：
(1)使用胆酸盐聚集体为模板,在温和的条件下(室温,水体系,一步反应)制备了具有中空结构的二氧化硅微球。运用扫描电子显微镜(SEM)和透射电子显微镜(TEM)对产品结构进行了表征。动态光散射(DLS)和相差显微镜(PCM)分析表明,胆酸与苄胺在水溶液中形成了粒径分散的囊泡状聚集体。红外光谱分析表明产品中存在胆酸盐分子,证实了模板作用的存在。分别以正丁胺和二乙胺为有机胺添加剂时,产品都是中空球与粉末结构的混合物,而添加三乙胺只得到粉末结构。3-三氨丙基三乙氧基硅烷(APES)作为共结构指示剂与胆酸、胆酸铵和胆酸钠分别形成聚集体,也可以作为模板合成中空结构硅球,但产物中存在部分实心球。结果表明,有机模板与无机前体间的氢键相互作用为形态转录能否实现的决定性因素。
(2)小分子水凝胶是近年来得到迅速拓展的一个研究领域。水凝胶是模仿生物矿化的重要体系,能够对矿物生长产生重要影响。我们在胆酸酯类小分子水凝胶中发现了KCl晶体高度取向生长以及形成的对称性枝晶图案。利用SEM及光电子能谱仪(EDS)对晶体形貌及成分进行了分析。研究表明,KCl初始浓度和凝胶密度不会改变枝晶取向性,而凝胶类型对晶体形态有较大影响。在L-胱氨酸衍生物小分子水凝胶中得到了宏观无序的KCl水草状枝蔓晶图案。对凝胶因子亲水部分在水溶液条件下对KCl晶体生长的影响进行了分析,发现了有机物对晶体特定晶面的特殊吸附作用。水凝胶体系不仅为晶体成核提供了位点,对成核晶面和晶体生长速度的取向性进行了选择和调控,还利用内部扩散受限而稳定的微环境,将晶体的局部对称性通过周期性生长转录给枝晶整体图案。
(3)导电聚合物材料由于自身的特性及其在高科技领域的潜在应用而吸引了人们的目光。聚苯胺(PANI)材料由于其独特的电学、热电和光学性质以及良好的环境稳定性,成为导电聚合物家族中优秀的一员。在多孔聚合物基体上制备PANI复合物,能够改善其机械稳定性和加工性能。我们采用水辅助法从CHCl3溶液中制备了具有蜂窝状有序多孔结构的聚碳酸酯(PC)薄膜,并以之为模板制备了PANI/PC复合薄膜材料。反应过程中首先通过氢键作用在PC膜表面对苯胺单体进行预吸附,再经过一步化学氧化聚合在原位合成了PANI层。运用SEM、FT-IR、热重分析(TGA)和四极探针法分别对得到的PANI/PC复合膜的表面和截面形态、分子间相互作用、热力学稳定性和导电能力进行了表征和分析,证实了复合膜具有蜂窝状有序多孔结构,PANI与PC层之间形成了氢键相互作用,PANI热稳定性得到提高并具有较好导电能力。
总之,具有预先形成的有序结构的有机基体,能够有效指导无机和有机材料的生长,这为制备新颖材料提供了新方法,也为对生物矿化过程的深入理解提供了更多信息。
Biomineralization is the study on the complex hierarchical structures of materials produced biologically, and the processes that lead to these biomaterials. In this field, the efforts of chemists can be roughly divided into three different areas:(1) the analysis of biological materials;(2) the design of new model systems to mimic physiological environment in vitro, such as hydrogel media; and (3) the development of new strategies of bioinspired material synthesis, like template methods.
In this work, we have synthesized hollow silica microspheres by a biomimetic template method at first, and then have studied the highly oriented growth of inorganic KCl crystals in hydrogel media; at last, we have prepared conductive polymer composite materials based on a porous polymer substrate. It can be summarized as follows:
(1) Hollow spherical silica has been successfully fabricated in mild conditions (room temperature, no organic solvent, one-step method) using cholic acid aggregates as templates in basic solutions. The structures of the synthesized silica materials were analyzed by Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The vesicle morphologies of the self-assembly aggregates of cholic acid in the presence of benzylamine were confirmed by Dynamic Light Scattering (DLS) and Phase Contrast Microscopy (PCM). The cholates were identified in FT-IR spectrum, confirmed the existence of organic templates. The mixture of hollow spherical and granular structure was obtained when n-butylamine or diethylamine was used as amine additives instead, while only granule in the case of diethylamine. The aggregates of 3-amino- propyltriethoxysiline (APES) with cholic acid, ammonium cholate and sodium cholate, have also been used as templates to prepare hollow silica spheres, where there were solid spheres existed in the products. The results were ascribed to the hydrogen bonding interactions between the organic templates and the inorganic precursors.
(2) Low-molecular-weight (LMW) hydrogel is one of the quickly expanded research fields in recent years. Hydrogel system is an important kind of artificial media for biomineralization simulation. We have observed the oriented growth of potassium chloride (KC1) crystals and the dendritic patterns with high symmetry grown from the novel kind of LMW hydrogels derived from cholic acid. It was characterized by SEM equipped with Electron Energy Disperse Spectroscopy (EDS). The orientation of the patterns can hardly be changed by the concentration of either solutes or hydrogel matrix. The type of the hydrogel had great influence on KCl crystal morphologies, since the seaweed-like patters disordered in macroscopy have been obtained from another kind of LMW hydrogel derived from L-cystine. Crystal habit modifications of KCl crystals in aqueous solutions added with the hydrophilic groups of the hydrogelators through the special adsorptions with the specific crystal faces were studied. The hydrogel media have not only provided the sites for nucleation, selected the orientations of nucleating faces and crystal growth rates, but also allowed the translation of local symmetries to the whole dendritic patterns through periodic growth under the mass diffusion limited but stable microenvironment.
(3) In the family of conductive polymer materials, which have attracted much attention because of their special features and potential applications in hi-tech aspects, polyaniline (PANI) is unique due to its electronic, thermoelectric and optical properties and good environmental stabilities. Preparation of PANI composites on porous polymer substrate could improve its mechanical stability and processibility. We have prepared conducting composite materials by the synthesis of PANI layers by a simple one-step chemical oxidative polymerization, based on the surface of a honeycomb ordered porous polycarbonate (PC) film prepared via water-assisted method from PC/CHCl3 solutions. Aniline monomers were pre-organized on the surfaces of the PC film through hydrogen bonding, and a PANI film was obtained by oxidation in situ. The surface and cross-section structures of the PANI/PC composite film were characterized by SEM, confirmed the role of the PC film as template. The results of thermogravimetric analysis (TGA) of the PANI/PC composite film showed higher thermal stability than PANI itself. The FT-IR spectrum confirmed the existence of hydrogen bonding interactions between PC and PANI. The electrical conductivity of the PANI/PC composite film was determined by the four-probe technique.
In conclusion, the organic matrix with pre-organized ordered morphologies can serve as templates to modulate the growth of inorganic and organic materials. It could provide new strategies for material preparation and more information for deeply understanding biomineralization.
在本论文的工作中,我们首先利用仿生模板法合成了具有中空结构的二氧化硅微球,之后研究了无机晶体在水凝胶体系中的高度取向生长,最后在多孔聚合物基体上制备了导电聚合物杂化材料。分别概述如下：
(1)使用胆酸盐聚集体为模板,在温和的条件下(室温,水体系,一步反应)制备了具有中空结构的二氧化硅微球。运用扫描电子显微镜(SEM)和透射电子显微镜(TEM)对产品结构进行了表征。动态光散射(DLS)和相差显微镜(PCM)分析表明,胆酸与苄胺在水溶液中形成了粒径分散的囊泡状聚集体。红外光谱分析表明产品中存在胆酸盐分子,证实了模板作用的存在。分别以正丁胺和二乙胺为有机胺添加剂时,产品都是中空球与粉末结构的混合物,而添加三乙胺只得到粉末结构。3-三氨丙基三乙氧基硅烷(APES)作为共结构指示剂与胆酸、胆酸铵和胆酸钠分别形成聚集体,也可以作为模板合成中空结构硅球,但产物中存在部分实心球。结果表明,有机模板与无机前体间的氢键相互作用为形态转录能否实现的决定性因素。
(2)小分子水凝胶是近年来得到迅速拓展的一个研究领域。水凝胶是模仿生物矿化的重要体系,能够对矿物生长产生重要影响。我们在胆酸酯类小分子水凝胶中发现了KCl晶体高度取向生长以及形成的对称性枝晶图案。利用SEM及光电子能谱仪(EDS)对晶体形貌及成分进行了分析。研究表明,KCl初始浓度和凝胶密度不会改变枝晶取向性,而凝胶类型对晶体形态有较大影响。在L-胱氨酸衍生物小分子水凝胶中得到了宏观无序的KCl水草状枝蔓晶图案。对凝胶因子亲水部分在水溶液条件下对KCl晶体生长的影响进行了分析,发现了有机物对晶体特定晶面的特殊吸附作用。水凝胶体系不仅为晶体成核提供了位点,对成核晶面和晶体生长速度的取向性进行了选择和调控,还利用内部扩散受限而稳定的微环境,将晶体的局部对称性通过周期性生长转录给枝晶整体图案。
(3)导电聚合物材料由于自身的特性及其在高科技领域的潜在应用而吸引了人们的目光。聚苯胺(PANI)材料由于其独特的电学、热电和光学性质以及良好的环境稳定性,成为导电聚合物家族中优秀的一员。在多孔聚合物基体上制备PANI复合物,能够改善其机械稳定性和加工性能。我们采用水辅助法从CHCl3溶液中制备了具有蜂窝状有序多孔结构的聚碳酸酯(PC)薄膜,并以之为模板制备了PANI/PC复合薄膜材料。反应过程中首先通过氢键作用在PC膜表面对苯胺单体进行预吸附,再经过一步化学氧化聚合在原位合成了PANI层。运用SEM、FT-IR、热重分析(TGA)和四极探针法分别对得到的PANI/PC复合膜的表面和截面形态、分子间相互作用、热力学稳定性和导电能力进行了表征和分析,证实了复合膜具有蜂窝状有序多孔结构,PANI与PC层之间形成了氢键相互作用,PANI热稳定性得到提高并具有较好导电能力。
总之,具有预先形成的有序结构的有机基体,能够有效指导无机和有机材料的生长,这为制备新颖材料提供了新方法,也为对生物矿化过程的深入理解提供了更多信息。
Biomineralization is the study on the complex hierarchical structures of materials produced biologically, and the processes that lead to these biomaterials. In this field, the efforts of chemists can be roughly divided into three different areas:(1) the analysis of biological materials;(2) the design of new model systems to mimic physiological environment in vitro, such as hydrogel media; and (3) the development of new strategies of bioinspired material synthesis, like template methods.
In this work, we have synthesized hollow silica microspheres by a biomimetic template method at first, and then have studied the highly oriented growth of inorganic KCl crystals in hydrogel media; at last, we have prepared conductive polymer composite materials based on a porous polymer substrate. It can be summarized as follows:
(1) Hollow spherical silica has been successfully fabricated in mild conditions (room temperature, no organic solvent, one-step method) using cholic acid aggregates as templates in basic solutions. The structures of the synthesized silica materials were analyzed by Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The vesicle morphologies of the self-assembly aggregates of cholic acid in the presence of benzylamine were confirmed by Dynamic Light Scattering (DLS) and Phase Contrast Microscopy (PCM). The cholates were identified in FT-IR spectrum, confirmed the existence of organic templates. The mixture of hollow spherical and granular structure was obtained when n-butylamine or diethylamine was used as amine additives instead, while only granule in the case of diethylamine. The aggregates of 3-amino- propyltriethoxysiline (APES) with cholic acid, ammonium cholate and sodium cholate, have also been used as templates to prepare hollow silica spheres, where there were solid spheres existed in the products. The results were ascribed to the hydrogen bonding interactions between the organic templates and the inorganic precursors.
(2) Low-molecular-weight (LMW) hydrogel is one of the quickly expanded research fields in recent years. Hydrogel system is an important kind of artificial media for biomineralization simulation. We have observed the oriented growth of potassium chloride (KC1) crystals and the dendritic patterns with high symmetry grown from the novel kind of LMW hydrogels derived from cholic acid. It was characterized by SEM equipped with Electron Energy Disperse Spectroscopy (EDS). The orientation of the patterns can hardly be changed by the concentration of either solutes or hydrogel matrix. The type of the hydrogel had great influence on KCl crystal morphologies, since the seaweed-like patters disordered in macroscopy have been obtained from another kind of LMW hydrogel derived from L-cystine. Crystal habit modifications of KCl crystals in aqueous solutions added with the hydrophilic groups of the hydrogelators through the special adsorptions with the specific crystal faces were studied. The hydrogel media have not only provided the sites for nucleation, selected the orientations of nucleating faces and crystal growth rates, but also allowed the translation of local symmetries to the whole dendritic patterns through periodic growth under the mass diffusion limited but stable microenvironment.
(3) In the family of conductive polymer materials, which have attracted much attention because of their special features and potential applications in hi-tech aspects, polyaniline (PANI) is unique due to its electronic, thermoelectric and optical properties and good environmental stabilities. Preparation of PANI composites on porous polymer substrate could improve its mechanical stability and processibility. We have prepared conducting composite materials by the synthesis of PANI layers by a simple one-step chemical oxidative polymerization, based on the surface of a honeycomb ordered porous polycarbonate (PC) film prepared via water-assisted method from PC/CHCl3 solutions. Aniline monomers were pre-organized on the surfaces of the PC film through hydrogen bonding, and a PANI film was obtained by oxidation in situ. The surface and cross-section structures of the PANI/PC composite film were characterized by SEM, confirmed the role of the PC film as template. The results of thermogravimetric analysis (TGA) of the PANI/PC composite film showed higher thermal stability than PANI itself. The FT-IR spectrum confirmed the existence of hydrogen bonding interactions between PC and PANI. The electrical conductivity of the PANI/PC composite film was determined by the four-probe technique.
In conclusion, the organic matrix with pre-organized ordered morphologies can serve as templates to modulate the growth of inorganic and organic materials. It could provide new strategies for material preparation and more information for deeply understanding biomineralization.
引文
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