二氧化硅基质复合材料及荧光共轭聚合物制备与表征
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摘要
纳米材料由于独特的物理、化学性能受到了广泛的关注。纳米材料形貌对其性能有重要影响，因此发展新的材料制备方法已经成为近年的研究热点之一。本论文针对目前银纳米材料、量子点复合材料制备过程复杂、条件要求苛刻等问题以及目前所制备共轭有机聚合物溶解性、荧光性能差、制备过程复杂等问题，开展了以下三方面的研究工作，具体内容如下：
1．通过原位还原结合溶胶-凝胶法制备了纳米银掺杂二氧化硅材料；本部分研究内容中包括了:（a）通过溶胶-凝胶法首次制备了修饰银纳米颗粒的二氧化硅微管并对其形成机理进行了初步探索、考察了制备过程中主要因素对所制备材料形貌影响，并通过扫描电子显微镜、高分辨场致发射透射电子显微镜以及红外光谱、紫外-可见光谱对材料的形貌以及基本性质进行了研究；（b）首次通过非水相溶胶-凝胶法制备了圆柱形的纳米银掺杂二氧化硅微棒、纳米银掺杂的二氧化硅纳米带以及六棱柱形的纳米银掺杂二氧化硅微棒。详细研究了硝酸银与（3-巯丙基）三乙氧基硅烷之间的反应，考察了两者之间的配比、溶剂、温度等主要因素对所制备材料形貌的影响。通过扫描电子显微镜、高分辨场致发射透射电子显微镜以及紫外-可见光谱以及红外光谱等对所制备材料的形貌以及基本性质进行了研究。
2．通过溶胶-凝胶结合原位生长量子点技术在室温条件下制备了硫化镉、硫化铅量子点掺杂二氧化硅材料，并考察了醋酸镉、醋酸铅、（3-巯丙基）三乙氧基硅烷等试剂用量以及之间的比例对材料形貌以及性能的影响。通过扫描电子显微镜、高分辨场致发射电子显微镜以及紫外-可见、荧光光谱对材料的形貌以及发光性能进行了研究。结果表明：制备方法、试剂用量以及比例都对材料的发光性能产生影响，通过控制制备过程主要因素可以制备出理想发光性能量子点掺杂二氧化硅复合材料。
3.利用化学氧化聚合反应在室温条件下通过简单的一步法，在没有加入任何辅助模板的条件下，制备了“菊花状”、以及“树枝状”共轭聚合物材料；在模板辅助下制备了“方形管状”共轭聚合物材料。并详细研究了以间氨基苯甲酸为功能单体制备荧光共轭聚合物过程中，引发剂的种类与用量，功能单体的浓度，甲基橙，蛋白质等对聚合物形貌的影响。并通过扫描电子显微镜、红外光谱等技术对材料的形貌与组成进行了表征。通过荧光光谱研究了所制备材料的荧光性能。研究表明：所制备的荧光共轭聚合物不仅能够溶解于常见有机溶剂而且显示了优异的荧光性能。
Nanomaterials have attracted widely interest due to unique physical andchemical properties. The morphology of nanomaterials plays an important role tomaterials properties. Thus the development of the novel preparation approach tomaterials has become an important field. Most of the present preparation approachinvolved in complex preparation process, high temperature and high pressure and soon. In the present research, we have developed series of simple preparation approachto inorganic and organic optical materials. The whole work can be divided into threeparts. More details are shown as following:
1. In the first research work, silver nanoparticles doped silica compositematerials are prepared by the combination of in situ reduction and sol-gel techniques.First, we prepared silicon dioxide nanotubes with silver nanoparticle in inner wall bytwo steps sol-gel approach at room temperature. The possible formation mechanismwas suggested. The influence of the preparation condition on the materialsmorphology was investigated. The obtained materials were characterized by SEM andFETEM. The properties and composition of the synthesized materials were alsoinvestigated by Uv-Vis and FTIR, respectively. Secondly, silver nanoparticles dopedsilica hybrid materials were fabricated by “one-pot” sol-gel technique in nonaqueoussolutions at room temperature. The columniform shaped micro-rods, nanobelt andhexagon shaped micro-rods were obtained by controlling the preparation conditions.The main factors that affect the morphology of hybrid materials were investigated indetail. The materials were further characterized by SEM and FETEM and theproperties were checked by Uv-Vis. The results indicated that different morphologysilver nanoparticles doped hybrid materials could be obtained by adjusting thereaction conditions.
2. In the second research work, CdS and pbS quantum dots doped silica hybridmaterials were obtained by sol-gel technique at room temperature. The morphologychange was studied by adjusting the preparation conditions. The morphologies of synthesized materials were further characterized by SEM and TEM, respectively. Thefluorescence properties were also checked by fluorescence spectrometry. The resultsindicated that the obtained materials showed excellent fluorescence properties.
3. Chrysanthemum, square tube and dendritic conjugated polymers wereprepared by a simple one-pot approach in the absence of any template. The effect ofmain factors such as initiator type and amount, the concentration of functionalmonomer, methyl orange and protein on morphology was investigated in detail.. Themorphology of the materials was checked by SEM and TEM, respectively.Fluorescence properties of prepared materials were also investigated in differentorganic solvents by fluorescence spectrometry. All results indicated the synthesizedmaterials show a potential in fluorescence sensor.
1．通过原位还原结合溶胶-凝胶法制备了纳米银掺杂二氧化硅材料；本部分研究内容中包括了:（a）通过溶胶-凝胶法首次制备了修饰银纳米颗粒的二氧化硅微管并对其形成机理进行了初步探索、考察了制备过程中主要因素对所制备材料形貌影响，并通过扫描电子显微镜、高分辨场致发射透射电子显微镜以及红外光谱、紫外-可见光谱对材料的形貌以及基本性质进行了研究；（b）首次通过非水相溶胶-凝胶法制备了圆柱形的纳米银掺杂二氧化硅微棒、纳米银掺杂的二氧化硅纳米带以及六棱柱形的纳米银掺杂二氧化硅微棒。详细研究了硝酸银与（3-巯丙基）三乙氧基硅烷之间的反应，考察了两者之间的配比、溶剂、温度等主要因素对所制备材料形貌的影响。通过扫描电子显微镜、高分辨场致发射透射电子显微镜以及紫外-可见光谱以及红外光谱等对所制备材料的形貌以及基本性质进行了研究。
2．通过溶胶-凝胶结合原位生长量子点技术在室温条件下制备了硫化镉、硫化铅量子点掺杂二氧化硅材料，并考察了醋酸镉、醋酸铅、（3-巯丙基）三乙氧基硅烷等试剂用量以及之间的比例对材料形貌以及性能的影响。通过扫描电子显微镜、高分辨场致发射电子显微镜以及紫外-可见、荧光光谱对材料的形貌以及发光性能进行了研究。结果表明：制备方法、试剂用量以及比例都对材料的发光性能产生影响，通过控制制备过程主要因素可以制备出理想发光性能量子点掺杂二氧化硅复合材料。
3.利用化学氧化聚合反应在室温条件下通过简单的一步法，在没有加入任何辅助模板的条件下，制备了“菊花状”、以及“树枝状”共轭聚合物材料；在模板辅助下制备了“方形管状”共轭聚合物材料。并详细研究了以间氨基苯甲酸为功能单体制备荧光共轭聚合物过程中，引发剂的种类与用量，功能单体的浓度，甲基橙，蛋白质等对聚合物形貌的影响。并通过扫描电子显微镜、红外光谱等技术对材料的形貌与组成进行了表征。通过荧光光谱研究了所制备材料的荧光性能。研究表明：所制备的荧光共轭聚合物不仅能够溶解于常见有机溶剂而且显示了优异的荧光性能。
Nanomaterials have attracted widely interest due to unique physical andchemical properties. The morphology of nanomaterials plays an important role tomaterials properties. Thus the development of the novel preparation approach tomaterials has become an important field. Most of the present preparation approachinvolved in complex preparation process, high temperature and high pressure and soon. In the present research, we have developed series of simple preparation approachto inorganic and organic optical materials. The whole work can be divided into threeparts. More details are shown as following:
1. In the first research work, silver nanoparticles doped silica compositematerials are prepared by the combination of in situ reduction and sol-gel techniques.First, we prepared silicon dioxide nanotubes with silver nanoparticle in inner wall bytwo steps sol-gel approach at room temperature. The possible formation mechanismwas suggested. The influence of the preparation condition on the materialsmorphology was investigated. The obtained materials were characterized by SEM andFETEM. The properties and composition of the synthesized materials were alsoinvestigated by Uv-Vis and FTIR, respectively. Secondly, silver nanoparticles dopedsilica hybrid materials were fabricated by “one-pot” sol-gel technique in nonaqueoussolutions at room temperature. The columniform shaped micro-rods, nanobelt andhexagon shaped micro-rods were obtained by controlling the preparation conditions.The main factors that affect the morphology of hybrid materials were investigated indetail. The materials were further characterized by SEM and FETEM and theproperties were checked by Uv-Vis. The results indicated that different morphologysilver nanoparticles doped hybrid materials could be obtained by adjusting thereaction conditions.
2. In the second research work, CdS and pbS quantum dots doped silica hybridmaterials were obtained by sol-gel technique at room temperature. The morphologychange was studied by adjusting the preparation conditions. The morphologies of synthesized materials were further characterized by SEM and TEM, respectively. Thefluorescence properties were also checked by fluorescence spectrometry. The resultsindicated that the obtained materials showed excellent fluorescence properties.
3. Chrysanthemum, square tube and dendritic conjugated polymers wereprepared by a simple one-pot approach in the absence of any template. The effect ofmain factors such as initiator type and amount, the concentration of functionalmonomer, methyl orange and protein on morphology was investigated in detail.. Themorphology of the materials was checked by SEM and TEM, respectively.Fluorescence properties of prepared materials were also investigated in differentorganic solvents by fluorescence spectrometry. All results indicated the synthesizedmaterials show a potential in fluorescence sensor.
引文
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