仿生物矿化模板法调控晶体生长机理与试验研究
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摘要
生物矿化是自然界生物体内普遍存在的一种现象，即在生物体内形成矿物质(生物矿物)的过程。在此过程中，晶体形貌、尺寸、晶体方向受到结晶时局部条件的控制，特别是在有机基质(分为不溶性有机基质和可溶性有机基质)和生物分子共同存在的情况下，可达到控制晶习和多晶类型的目的。可溶性有机基质可以吸附在特定的晶面上，从而改变不同晶面的相对生长速率，导致不同的晶体特性；不可溶性有机基质能作为生物矿化的惰性底质或矿物沉淀的局限空间，从而调控晶体的形态大小、空间排列、结晶取向和同质多晶类型。这些过程通常是在有机基质／无机界面发生的，有机基质为矿物以合适的方式成核和外延生长提供初始的结构信息。骨骼、牙齿、贝壳和珍珠等都是常见的生物矿物，它们是以生物大分子为有机基质，通过分子预组装、界面分子识别、生长调制和细胞加工等过程形成的高度有序的无机／有机复合材料。由于它们大小规整，结构、形态及结晶取向一致等特点使其具有优良的功能性，在实际应用中有广阔的应用前景，所以，模仿生物体内这些材料的矿化过程具有重要的意义。
近几年，利用模板法诱导晶体生长的方法模拟生物矿化研究已成为一个热门课题。虽然，模板法模拟生物矿化过程制备材料取得了很大的成功，但是这项研究还存在几点不足。首先，大多数的研究工作都是通过优化模板的结构和化学性质来调控晶体的结构、形貌和取向，但是对于用模板来控制特定晶型晶体生长的研究还很少。其次，实际应用的晶体材料大多需要厘米尺寸，但是由模板法调控生成的晶体，有很大一部分是毫米尺寸的，这就限制了晶体的实用性。另外，现今社会对有机材料的需求也日益增多，而由模板法调控生成的晶体大多数是无机晶体。
基于以上问题，本文从仿生学角度出发，将生物矿化的机理引入到材料合成领域，以不同介质为模板，去调控无机、有机晶体晶习、晶型的形成，并研究了各种模板对晶体结晶过程的调控作用及它们之间的识别和控制机制。同时通过控制晶体生长实验条件，在较短时间内生长出尺寸较大的晶体。总体上本文可以分为两部分：第一部分利用各种硬模板模拟不可溶性有机基质在生物矿化中的作用调控晶体生长；第二部分利用各种软模板模拟可溶性有机基质在生物矿化中的作用调控晶体生长。
第一部分主要研究内容如下：
1.以不同热力学状态的硬脂酸LB膜为模板诱导五水硫酸铜晶体生长。首先，利用变温红外光谱研究硬脂酸LB膜的热稳定性，结果显示LB膜中硬脂酸相变（固态-液态）发生在70-72℃。其次，深入探究了不同热力学状态LB膜对五水硫酸铜晶体生长、表面形貌、晶体结构和取向的影响。结果表明，即使在液态状态下，LB膜仍可调控诱导晶体生长，且不同热力学状态的LB膜由于表面结构的改变，结晶在LB膜上晶体的形貌和取向也随之发生改变。
2.以未经修饰的基片作为模板，通过缓慢分解(NH4)CO3的方法制备了CaCO3晶体，考察了不同基片对CaCO3结晶的影响。通过SEM、XRD、FTIR、接触角测试等方法对CaCO3晶体的形貌、晶型及所用基片进行表征。结果显示，当以金片为模板诱导碳酸钙晶体生长时,能制备出结晶度好、文石相含量高的针状碳酸钙；当以硅片为模板诱导碳酸钙晶体生长时,能制备出球霰石和方解石的共晶体。结合基片结构性质和碳酸钙晶体的XRD数据，探讨了基片诱导晶体生长的机理。实验结果表明对于金片，晶格立体匹配和金片的疏水特性是控制碳酸钙晶体生长的主要原因；而对于硅基片，电负性和羟基基团是控制碳酸钙晶体生长的主要原因。
3.以3-巯基丙基三甲氧基硅烷自组装膜作为仿生矿化模板成功制备出了大小均匀且沿（001）面单一取向，尺寸约为5mm的层状KCl晶体。通过与无模板诱导所得晶体的形貌和晶面取向进行比较，可知自组装膜头部基团与K+之间的静电作用以及自组装膜与（110）面之间较好的晶格匹配关系是KCl晶体取向生长的主要原因。同时，以改变模板放置方法的方式改变晶体生长的动力学因素即自发成核和诱导成核之间的关系，获得了不同形貌和结构特征的KCl晶体材料。
4.以黑色素自组装膜作为仿生矿化模板成功制备出了厘米级的甘氨酸晶体。首先，在碱性溶液中成功的将黑色素溶液组装在带有负电荷的基底（硅片和玻璃片）上，得到了均匀和形貌一致的黑色素薄膜。通过红外光谱和光电子能谱可知黑色素成分是通过N-O-Si形式与基底结合，且X-ray衍射结果显示组装在硅片上的自组装薄膜在两个方向上都是有序的结构，这对理解黑色素薄膜的微观结构是非常有用的一个贡献。然后用黑色素自组装膜作为仿生矿化模板成功制备出了与无模板诱导所得晶体的形貌和晶面取向有较大差别的晶体。结果表明，自组装膜头部基团与甘氨酸之间的静电作用以及自组装膜与α-甘氨酸（010）面之间较好的晶格匹配关系是晶体晶习改变的主要原因。
第二部分主要研究内容如下：
1.研究了各种羧酸类（甲酸、乙酸、丙酸）、丙酮、醇类（甲醇、乙醇、丙醇、丁醇）对谷氨酸溶液结晶晶型的影响。结果表明：当70°C的谷氨酸饱和溶液快速冷却搅拌到0°C时，有羧酸类物质为添加剂时，溶液易得到β型晶体;而当有酮类、醇类为添加剂时或无添加剂时，在相同条件下易得到α型晶体。
2.利用银溶胶为模板，在中性溶液中合成了γ-晶型的甘氨酸晶体。实验结果表明，甘氨酸结晶情况与银溶胶的浓度有关，银溶胶的加入有利于γ晶型甘氨酸的结晶。紫外光谱和拉曼光谱实验结果表明甘氨酸分子通过NH3+基团可以吸引带负电荷的银溶胶，破坏电离平衡，促进溶液中甘氨酸阴离子的产生，从而有效抑制α晶型的成核和生长，促进了γ-晶型晶核的生长。
Biological mineral is the step which minerals are becoming in organism, infact, they are very important components of organism and high-performancecomposite materials. The most immediately striking aspect of biomaterials is therange of exquisite and unique morphologies, which are frequently disparate fromtheir synthetic counterpart. Typical products of biomineralization are bones, teeth,shells, pearls, and so on. The general principles of biomineralization are introducedinto the synthesis process of inorganic materials. Simulating the biomineralizationprocess of the nucleation and growth of inorganic materials mediated by organicmatrixes and biomimetic synthesis of inorganic materials with higher performanceand more exquisite morphologies have become the focus of material science.
Biomineralization is mother natures approach to advanced materials synthesis,and it attempts to chemically control the growth of inorganic crystals in theorganicsubstrate by adapting or imitating biological mineralization strategies. Thekey to the successful synthesis of an inorganic-organic composite is an understandingof the parameters that control the nucleation and growth of inorganic crystals underthe substrate in aqueous solution. In this thesis, we try some new substrates to controlthe polymorphism and morphology of crystal.
1. We study the behavior of the CuSO4·5H2Ocrystals grown on the different state film. Theexperimental results demonstrated that the LB film in the liquid state has the ability of directingthe nucleation and grow of crystals. Moreover, the CuSO4·5H2O crystals grown on the liquid filmhave quite different orientation and morphology from those grown on the solid film.
2. Control of crystal polymorph and size is very important in many applicationfields. In the present study, Au and Si substrates were used as solid templates tocontrol the growth of calcium carbonate (CaCO3) crystals have been described. The obtained composite CaCO3were characterized by using X-ray powder diffraction(XRD) analysis, Scanning electron microscopy (SEM) and Fourier transforminfrared spectroscopy (FTIR) measurement.
3. The MPTS SAMS films is used as template to induce the nucleation andgrowth of KCl crystals. X-ray diffraction (XRD) patterns and optical microscopyimages show that the orientation and morphology of the crystals have successfullybeen controlled by changing the orientation and position of the self-assembly films inthe solutions.
4. In the present study, uniform and rather flat melanin films with the dendritesstructure obtained using self-assembly technique on Si substrate. The structure offilm was confirmed by Fourier-transformed infrared spectrometry (FTIR), X-raydiffraction (XRD) and Scanning Electron Microscopy (SEM). Experimental resultsshowed that the grown on the Si substrate, self-assembly film had oriented quality.Furthermore, according to the results，a model of the secondary structure in themelanin films was suggested. Then the SAMS films are used to serve as templates toinduce glycine crystal growth. The results of experiment proved that it is not onlythat morphology and orientation of crystal can be controlled by the optimization ofthe structure and chemistry of the SAMS film.
5.The control of crystal polymorphism of the trimorphic crystals of glutamicacid (Glu) grown in solutionsin the presence of formic acid、acetic acid，propionicacid，methanol，ethanol，propanol，butanol，acetone. The presence of acids insolutions induces-polymorphs of glutamic acid when the temperature of solutionsranges from70°C to0°C. At the same experiment conditions, the other additivesinduce α-polymorphs of glutamic acid.
6. We demonstrate that silver colloid can serve as additive and induced theγ-form polymorph of glycine crystals in the netural solution. The silver colloid couldquickly affect the packing arrangements of glycine molecules in aqueous solutionleading to the competitive nucleation of the two polymorphs.
近几年，利用模板法诱导晶体生长的方法模拟生物矿化研究已成为一个热门课题。虽然，模板法模拟生物矿化过程制备材料取得了很大的成功，但是这项研究还存在几点不足。首先，大多数的研究工作都是通过优化模板的结构和化学性质来调控晶体的结构、形貌和取向，但是对于用模板来控制特定晶型晶体生长的研究还很少。其次，实际应用的晶体材料大多需要厘米尺寸，但是由模板法调控生成的晶体，有很大一部分是毫米尺寸的，这就限制了晶体的实用性。另外，现今社会对有机材料的需求也日益增多，而由模板法调控生成的晶体大多数是无机晶体。
基于以上问题，本文从仿生学角度出发，将生物矿化的机理引入到材料合成领域，以不同介质为模板，去调控无机、有机晶体晶习、晶型的形成，并研究了各种模板对晶体结晶过程的调控作用及它们之间的识别和控制机制。同时通过控制晶体生长实验条件，在较短时间内生长出尺寸较大的晶体。总体上本文可以分为两部分：第一部分利用各种硬模板模拟不可溶性有机基质在生物矿化中的作用调控晶体生长；第二部分利用各种软模板模拟可溶性有机基质在生物矿化中的作用调控晶体生长。
第一部分主要研究内容如下：
1.以不同热力学状态的硬脂酸LB膜为模板诱导五水硫酸铜晶体生长。首先，利用变温红外光谱研究硬脂酸LB膜的热稳定性，结果显示LB膜中硬脂酸相变（固态-液态）发生在70-72℃。其次，深入探究了不同热力学状态LB膜对五水硫酸铜晶体生长、表面形貌、晶体结构和取向的影响。结果表明，即使在液态状态下，LB膜仍可调控诱导晶体生长，且不同热力学状态的LB膜由于表面结构的改变，结晶在LB膜上晶体的形貌和取向也随之发生改变。
2.以未经修饰的基片作为模板，通过缓慢分解(NH4)CO3的方法制备了CaCO3晶体，考察了不同基片对CaCO3结晶的影响。通过SEM、XRD、FTIR、接触角测试等方法对CaCO3晶体的形貌、晶型及所用基片进行表征。结果显示，当以金片为模板诱导碳酸钙晶体生长时,能制备出结晶度好、文石相含量高的针状碳酸钙；当以硅片为模板诱导碳酸钙晶体生长时,能制备出球霰石和方解石的共晶体。结合基片结构性质和碳酸钙晶体的XRD数据，探讨了基片诱导晶体生长的机理。实验结果表明对于金片，晶格立体匹配和金片的疏水特性是控制碳酸钙晶体生长的主要原因；而对于硅基片，电负性和羟基基团是控制碳酸钙晶体生长的主要原因。
3.以3-巯基丙基三甲氧基硅烷自组装膜作为仿生矿化模板成功制备出了大小均匀且沿（001）面单一取向，尺寸约为5mm的层状KCl晶体。通过与无模板诱导所得晶体的形貌和晶面取向进行比较，可知自组装膜头部基团与K+之间的静电作用以及自组装膜与（110）面之间较好的晶格匹配关系是KCl晶体取向生长的主要原因。同时，以改变模板放置方法的方式改变晶体生长的动力学因素即自发成核和诱导成核之间的关系，获得了不同形貌和结构特征的KCl晶体材料。
4.以黑色素自组装膜作为仿生矿化模板成功制备出了厘米级的甘氨酸晶体。首先，在碱性溶液中成功的将黑色素溶液组装在带有负电荷的基底（硅片和玻璃片）上，得到了均匀和形貌一致的黑色素薄膜。通过红外光谱和光电子能谱可知黑色素成分是通过N-O-Si形式与基底结合，且X-ray衍射结果显示组装在硅片上的自组装薄膜在两个方向上都是有序的结构，这对理解黑色素薄膜的微观结构是非常有用的一个贡献。然后用黑色素自组装膜作为仿生矿化模板成功制备出了与无模板诱导所得晶体的形貌和晶面取向有较大差别的晶体。结果表明，自组装膜头部基团与甘氨酸之间的静电作用以及自组装膜与α-甘氨酸（010）面之间较好的晶格匹配关系是晶体晶习改变的主要原因。
第二部分主要研究内容如下：
1.研究了各种羧酸类（甲酸、乙酸、丙酸）、丙酮、醇类（甲醇、乙醇、丙醇、丁醇）对谷氨酸溶液结晶晶型的影响。结果表明：当70°C的谷氨酸饱和溶液快速冷却搅拌到0°C时，有羧酸类物质为添加剂时，溶液易得到β型晶体;而当有酮类、醇类为添加剂时或无添加剂时，在相同条件下易得到α型晶体。
2.利用银溶胶为模板，在中性溶液中合成了γ-晶型的甘氨酸晶体。实验结果表明，甘氨酸结晶情况与银溶胶的浓度有关，银溶胶的加入有利于γ晶型甘氨酸的结晶。紫外光谱和拉曼光谱实验结果表明甘氨酸分子通过NH3+基团可以吸引带负电荷的银溶胶，破坏电离平衡，促进溶液中甘氨酸阴离子的产生，从而有效抑制α晶型的成核和生长，促进了γ-晶型晶核的生长。
Biological mineral is the step which minerals are becoming in organism, infact, they are very important components of organism and high-performancecomposite materials. The most immediately striking aspect of biomaterials is therange of exquisite and unique morphologies, which are frequently disparate fromtheir synthetic counterpart. Typical products of biomineralization are bones, teeth,shells, pearls, and so on. The general principles of biomineralization are introducedinto the synthesis process of inorganic materials. Simulating the biomineralizationprocess of the nucleation and growth of inorganic materials mediated by organicmatrixes and biomimetic synthesis of inorganic materials with higher performanceand more exquisite morphologies have become the focus of material science.
Biomineralization is mother natures approach to advanced materials synthesis,and it attempts to chemically control the growth of inorganic crystals in theorganicsubstrate by adapting or imitating biological mineralization strategies. Thekey to the successful synthesis of an inorganic-organic composite is an understandingof the parameters that control the nucleation and growth of inorganic crystals underthe substrate in aqueous solution. In this thesis, we try some new substrates to controlthe polymorphism and morphology of crystal.
1. We study the behavior of the CuSO4·5H2Ocrystals grown on the different state film. Theexperimental results demonstrated that the LB film in the liquid state has the ability of directingthe nucleation and grow of crystals. Moreover, the CuSO4·5H2O crystals grown on the liquid filmhave quite different orientation and morphology from those grown on the solid film.
2. Control of crystal polymorph and size is very important in many applicationfields. In the present study, Au and Si substrates were used as solid templates tocontrol the growth of calcium carbonate (CaCO3) crystals have been described. The obtained composite CaCO3were characterized by using X-ray powder diffraction(XRD) analysis, Scanning electron microscopy (SEM) and Fourier transforminfrared spectroscopy (FTIR) measurement.
3. The MPTS SAMS films is used as template to induce the nucleation andgrowth of KCl crystals. X-ray diffraction (XRD) patterns and optical microscopyimages show that the orientation and morphology of the crystals have successfullybeen controlled by changing the orientation and position of the self-assembly films inthe solutions.
4. In the present study, uniform and rather flat melanin films with the dendritesstructure obtained using self-assembly technique on Si substrate. The structure offilm was confirmed by Fourier-transformed infrared spectrometry (FTIR), X-raydiffraction (XRD) and Scanning Electron Microscopy (SEM). Experimental resultsshowed that the grown on the Si substrate, self-assembly film had oriented quality.Furthermore, according to the results，a model of the secondary structure in themelanin films was suggested. Then the SAMS films are used to serve as templates toinduce glycine crystal growth. The results of experiment proved that it is not onlythat morphology and orientation of crystal can be controlled by the optimization ofthe structure and chemistry of the SAMS film.
5.The control of crystal polymorphism of the trimorphic crystals of glutamicacid (Glu) grown in solutionsin the presence of formic acid、acetic acid，propionicacid，methanol，ethanol，propanol，butanol，acetone. The presence of acids insolutions induces-polymorphs of glutamic acid when the temperature of solutionsranges from70°C to0°C. At the same experiment conditions, the other additivesinduce α-polymorphs of glutamic acid.
6. We demonstrate that silver colloid can serve as additive and induced theγ-form polymorph of glycine crystals in the netural solution. The silver colloid couldquickly affect the packing arrangements of glycine molecules in aqueous solutionleading to the competitive nucleation of the two polymorphs.
引文
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