基于磷酸钙的有机—无机复合材料
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摘要
生物材料的仿生制备是近年来材料学、化学、生物医学等重要领域的研究热点之一。在自然界中,通过精巧的有序结构设计,生命体可以将有机分子和无机矿物复合形成具有特殊力学或光学性能的功能材料。值得注意的是,在生物材料形成中,有机基质和无机矿物两相紧密结合并有序排列,而这种结构的有序性赋予了生物材料超乎寻常的性能。在人工合成仿生复合材料中,通过有机-无机自组装形式从下至上的合成途径被认为是最为接近生命体的合成路线,也是最有效率的合成路径之一。然而,自组装的方法需要有机分子之间,以及有机-无机相之间能够在分子及微纳尺度上紧密结合并排列组装。但是,如何在如此小尺度上引入有序的有机相和无机相的分布是目前难以逾越的挑战。在本工作中,我们仔细分析了生物材料形成中有机分子和无机相之间有序性排列需要的条件,并以此仿生设计了含有两亲分子和模型蛋白质的一个简单体系,在磷酸钙的过饱和溶液中实现了在纳米尺度上有序排列的有机-无机复合材料的制备,并且该材料具有类骨的力学特征。我们还研究了溶液组分对所形成的有机-无机复合材料的形貌和结构的影响,并进一步获得了由相同手性所构成的纳米螺旋材料聚集体。结合自然界中手性矿物材料的演变过程,我们利用有机分子手性和弹性自由能的关系,从物理化学的角度理解了手性材料的原因和手性繁殖扩增的过程。全文共分五章,每章内容介绍如下
第一章作为绪论简要地介绍了生物材料的典型特征。着重论述了生物材料中“组成-结构-功能”间的紧密联系并介绍了生物材料中的生物矿物沉积结晶的基本知识及最新的研究进展。随后综述了有机基质在生物材料的形成过程中的作用,特别是框架大分子和结晶调控分子的功能。接着通过仿生合成研究中的有机物和无机物如何能够进行有序复合的讨论提出了我们的仿生模型体系。
第二章中我们设计了简单而又有效的仿生体系,通过两亲分子琥珀辛酯磺酸钠(Bis(2-ethylhexyl) sulfosuccinate, AOT),牛血清蛋白(Bovine serum albumin,BSA)和无机磷酸钙(Calcium phosphate,CaP)的相互协同作用在溶液中自发形成了具有菱形晶体结构特征的有机-无机复合体。这种复合体在纳米层次上具有有机相-无机相层层交叠的结构,其模量和硬度十分接近于人体骨骼,是一种具有弹性特征的磷酸钙基类骨材料。
第三章我们研究了反应溶液中不同组分,包括AOT、BSA和钙磷离子浓度对所形成的有机-无机复合片的形貌的影响。改变AOT、BSA和钙磷离了浓度对复合片的长径比有较大的影响,但依然保持有机相-无机相层层交叠的精细结构。增加AOT的浓度使得复合片的长径比减小,而增加BSA和钙磷离子浓度的趋势与AOT则相反。
第四章中我们研究了这种类骨的有机-无机复合片的形成机理,认为它们是有机相-无机相共同复合生长而形成的介晶。从复合介晶表面台阶结构特征可知该复合晶体是通过类似于传统的晶体台阶生长的机制所得到的。由两个AOT双分子层与两个磷酸钙层组成的复合台阶通过台阶生长巧妙地将有机物AOT和无机相磷酸钙有序地安置在周期性结构中。BSA则可能通过各向异性的吸附作用来调节复合片的形貌。
第五章中我们通过降低了反应体系中AOT的浓度并成功合成了手性的有机-无机复合纳米螺旋,该复合纳米螺旋和前面所提的“类骨”晶体一样具有有机-无机复合交替结构。其中一个十分特别的现象是,具有相问手性特征的复合螺旋可以组成一个较大的同手性聚集体。我们发现且这种同手性聚集体是通过一个初始的螺旋作为“母体”不断地自我复制扩增而来,并提出了一个基于AOT手性和弹性自由能的关系式来解释这一个手性扩增的行为。这一发现揭示了有机-无机复合物可以通过自我繁殖将手性结构进行遗传扩增,这和自然界进化过程贝壳的手性选择性扩增情况十分类似。
第六章总结了我们在仿生合成有机-无机复合物中的体会,并对本工作中存在的不足进行了分析,提出改进的建议为后续的研究提供参考。
The synthesis of biomimetic materials has become the emerging areas in the fields of materials, chemistry and biomedicine et.al. With the excellent structure design procedure, the general organic component and inorganic phase can be well integrated to ensure amazing functions like mechanical, optic properties. It should be noted that the ordered arrangement of organic and inorganic component is the key fact to bring attractive functions to biomaterials. In the artificial design of biometic materials, the bottom-up strategy through the assembly of both organic and inorganic phase is considered as one of the most efficient ways which are close to the biological condition. However, the strict requirement of assembly needs the tight integration between organic molecule itself and organic-inorganic phase at nano or micro-scale. Accordingly, the essential issue that the ordered arrangement of organic phase and inorganic phase at such small scale is a great chellagen for fabrication of biomimetic materials. In this work, we investigate the biological conditions that give rise to the order of distinc organic and inorganic phase and design a simple model system containing amphiphilic molecules and model protein. After adding additional calcium ions and phosphate ions, organic-inorganic hybrid plates and helix spontennously generats in the solution via self-assembly process. Both organic and inorganic phase are tightly integrated at nanoscle with ordered arrangement.We note that thse hybrid plates have interesting mechanical properties as bone. We also invesitigate the influence of different concentrations of reaction components on the morphology of hybrid plates, and synthesize the homochial nano-helix clusters consisted with organic-inorganic hybrid helix with same chiratlity. A physicochemicalmodel based on the chirality of organic molecules and the elastic free energy is suggested to explain the formation of chiral helix and the proliferation of chirality. The thesis is composed of five chapters:
In chapter1, we briefly introduce the typical properties of biomaterials and their. We focus on the composition-structure-function relationship of biomaterials. Then, the fundamental mechanisms and the recent developments during the crystallization and growth model of biominerals are also described. We review the essencial role of organic molecules, especially matrix macromolecules and molecules in the crystallization process. Finally, we suggest the crucial relationship of organic molecules and inorganic phase in the assembly of high order structure and inspire us to design reasonable reaction system to achieve the goal.
In chapter2, we design a model system to mimic the special relationships of organic molecules and inorganic phase. Here a model amphiphilic molecules Bis(2-ethylhexyl) sulfosuccinate (AOT) and Bovine Serum Albumin (BSA) in a supersatuated calcium phosphate solution. Organic-inorganic hybrid plates can spontaneously form and own alternative stacking of ultrathin organic layers and inorganic layers.Interestingly, the modulus and hardness is close to the natural bone in human body, which can be considered as a calcium phosphate based bone-like materaisl.
In chapter3, we further investigate the role of different reaction components (AOT. BSA and calcium/phosphate ions) on the morphology of resulted hybrid plates, which can be considered as a kind of hybrid mesocrystal. We suggest the different concentration of AOT, BSA and calcium/phosphate ions have various effects on the morphology especially the aspect ratio of hybrid plates. However, the internal lamellar structure maintains inspite of the change of reaction components. The increase of AOT leads to smaller aspect ratio while the larger BSA concentrations give rise to elongated ones. Apart from the organic components, the aspect ratio can also increase with more calcium/phosphate ions in reaction solutions.
In chapter4we investigate the formation mechanism of these bone-like organic-inorganic hybrid mesocrystal. With the observation of the morphology of surface steps on the hybrid mesocrystal, we suggest that the classical step growth model of crystals dominate its formation process. The growth step is hybrid consisted by two AOT bilayers and two thin CaP layers. Through the movement of hybrid steps, the AOT molecules and CaP phase are carefully arranged into ordered structure while the anisotropic absorbtion behavior of BSA can control the morphology of steps and then the morphology of hybrid mesocrystal.
In chapter5, we obain chiral organic-inorganic hybrid helix by decreasing the concentration of AOT molecules with similar internal structure as above hybrid plates. Interestingly, the helix with same chirality can form homochiral clusters, and these homochiral clusters are proliferated from single chiral helix as matrix. We suggest that the chirality determined free elastic energy ensure the homichiral proliferation process. This means the biomimetic hybrid materials can spontenneously amplify their chiral strucrures to later generations. This is very similar as the chiral selection of mollusk shell and proliferation process.
In chapter6, we sumerize the key points for biomimetic fabrication of hybrid mateirals. Our investigation of hybrid crystal formation via co-assembly of organic and inorganic phase in a classical step growth of inorganic crystals offer a new strategy to orderly integrate organic-inorganic phase at nanoscale. In addition, we also indicate that materials-based spontenneous amplification can occure in our simple model system. This interesting phenomenon offers a novel insight in the synthesis of highly regulated or self-similar materials. Finally, we also describe the shortages of our work and unsolved issues for further investigation.
第一章作为绪论简要地介绍了生物材料的典型特征。着重论述了生物材料中“组成-结构-功能”间的紧密联系并介绍了生物材料中的生物矿物沉积结晶的基本知识及最新的研究进展。随后综述了有机基质在生物材料的形成过程中的作用,特别是框架大分子和结晶调控分子的功能。接着通过仿生合成研究中的有机物和无机物如何能够进行有序复合的讨论提出了我们的仿生模型体系。
第二章中我们设计了简单而又有效的仿生体系,通过两亲分子琥珀辛酯磺酸钠(Bis(2-ethylhexyl) sulfosuccinate, AOT),牛血清蛋白(Bovine serum albumin,BSA)和无机磷酸钙(Calcium phosphate,CaP)的相互协同作用在溶液中自发形成了具有菱形晶体结构特征的有机-无机复合体。这种复合体在纳米层次上具有有机相-无机相层层交叠的结构,其模量和硬度十分接近于人体骨骼,是一种具有弹性特征的磷酸钙基类骨材料。
第三章我们研究了反应溶液中不同组分,包括AOT、BSA和钙磷离子浓度对所形成的有机-无机复合片的形貌的影响。改变AOT、BSA和钙磷离了浓度对复合片的长径比有较大的影响,但依然保持有机相-无机相层层交叠的精细结构。增加AOT的浓度使得复合片的长径比减小,而增加BSA和钙磷离子浓度的趋势与AOT则相反。
第四章中我们研究了这种类骨的有机-无机复合片的形成机理,认为它们是有机相-无机相共同复合生长而形成的介晶。从复合介晶表面台阶结构特征可知该复合晶体是通过类似于传统的晶体台阶生长的机制所得到的。由两个AOT双分子层与两个磷酸钙层组成的复合台阶通过台阶生长巧妙地将有机物AOT和无机相磷酸钙有序地安置在周期性结构中。BSA则可能通过各向异性的吸附作用来调节复合片的形貌。
第五章中我们通过降低了反应体系中AOT的浓度并成功合成了手性的有机-无机复合纳米螺旋,该复合纳米螺旋和前面所提的“类骨”晶体一样具有有机-无机复合交替结构。其中一个十分特别的现象是,具有相问手性特征的复合螺旋可以组成一个较大的同手性聚集体。我们发现且这种同手性聚集体是通过一个初始的螺旋作为“母体”不断地自我复制扩增而来,并提出了一个基于AOT手性和弹性自由能的关系式来解释这一个手性扩增的行为。这一发现揭示了有机-无机复合物可以通过自我繁殖将手性结构进行遗传扩增,这和自然界进化过程贝壳的手性选择性扩增情况十分类似。
第六章总结了我们在仿生合成有机-无机复合物中的体会,并对本工作中存在的不足进行了分析,提出改进的建议为后续的研究提供参考。
The synthesis of biomimetic materials has become the emerging areas in the fields of materials, chemistry and biomedicine et.al. With the excellent structure design procedure, the general organic component and inorganic phase can be well integrated to ensure amazing functions like mechanical, optic properties. It should be noted that the ordered arrangement of organic and inorganic component is the key fact to bring attractive functions to biomaterials. In the artificial design of biometic materials, the bottom-up strategy through the assembly of both organic and inorganic phase is considered as one of the most efficient ways which are close to the biological condition. However, the strict requirement of assembly needs the tight integration between organic molecule itself and organic-inorganic phase at nano or micro-scale. Accordingly, the essential issue that the ordered arrangement of organic phase and inorganic phase at such small scale is a great chellagen for fabrication of biomimetic materials. In this work, we investigate the biological conditions that give rise to the order of distinc organic and inorganic phase and design a simple model system containing amphiphilic molecules and model protein. After adding additional calcium ions and phosphate ions, organic-inorganic hybrid plates and helix spontennously generats in the solution via self-assembly process. Both organic and inorganic phase are tightly integrated at nanoscle with ordered arrangement.We note that thse hybrid plates have interesting mechanical properties as bone. We also invesitigate the influence of different concentrations of reaction components on the morphology of hybrid plates, and synthesize the homochial nano-helix clusters consisted with organic-inorganic hybrid helix with same chiratlity. A physicochemicalmodel based on the chirality of organic molecules and the elastic free energy is suggested to explain the formation of chiral helix and the proliferation of chirality. The thesis is composed of five chapters:
In chapter1, we briefly introduce the typical properties of biomaterials and their. We focus on the composition-structure-function relationship of biomaterials. Then, the fundamental mechanisms and the recent developments during the crystallization and growth model of biominerals are also described. We review the essencial role of organic molecules, especially matrix macromolecules and molecules in the crystallization process. Finally, we suggest the crucial relationship of organic molecules and inorganic phase in the assembly of high order structure and inspire us to design reasonable reaction system to achieve the goal.
In chapter2, we design a model system to mimic the special relationships of organic molecules and inorganic phase. Here a model amphiphilic molecules Bis(2-ethylhexyl) sulfosuccinate (AOT) and Bovine Serum Albumin (BSA) in a supersatuated calcium phosphate solution. Organic-inorganic hybrid plates can spontaneously form and own alternative stacking of ultrathin organic layers and inorganic layers.Interestingly, the modulus and hardness is close to the natural bone in human body, which can be considered as a calcium phosphate based bone-like materaisl.
In chapter3, we further investigate the role of different reaction components (AOT. BSA and calcium/phosphate ions) on the morphology of resulted hybrid plates, which can be considered as a kind of hybrid mesocrystal. We suggest the different concentration of AOT, BSA and calcium/phosphate ions have various effects on the morphology especially the aspect ratio of hybrid plates. However, the internal lamellar structure maintains inspite of the change of reaction components. The increase of AOT leads to smaller aspect ratio while the larger BSA concentrations give rise to elongated ones. Apart from the organic components, the aspect ratio can also increase with more calcium/phosphate ions in reaction solutions.
In chapter4we investigate the formation mechanism of these bone-like organic-inorganic hybrid mesocrystal. With the observation of the morphology of surface steps on the hybrid mesocrystal, we suggest that the classical step growth model of crystals dominate its formation process. The growth step is hybrid consisted by two AOT bilayers and two thin CaP layers. Through the movement of hybrid steps, the AOT molecules and CaP phase are carefully arranged into ordered structure while the anisotropic absorbtion behavior of BSA can control the morphology of steps and then the morphology of hybrid mesocrystal.
In chapter5, we obain chiral organic-inorganic hybrid helix by decreasing the concentration of AOT molecules with similar internal structure as above hybrid plates. Interestingly, the helix with same chirality can form homochiral clusters, and these homochiral clusters are proliferated from single chiral helix as matrix. We suggest that the chirality determined free elastic energy ensure the homichiral proliferation process. This means the biomimetic hybrid materials can spontenneously amplify their chiral strucrures to later generations. This is very similar as the chiral selection of mollusk shell and proliferation process.
In chapter6, we sumerize the key points for biomimetic fabrication of hybrid mateirals. Our investigation of hybrid crystal formation via co-assembly of organic and inorganic phase in a classical step growth of inorganic crystals offer a new strategy to orderly integrate organic-inorganic phase at nanoscale. In addition, we also indicate that materials-based spontenneous amplification can occure in our simple model system. This interesting phenomenon offers a novel insight in the synthesis of highly regulated or self-similar materials. Finally, we also describe the shortages of our work and unsolved issues for further investigation.
引文
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