核壳复合结构材料及空心结构材料的制备研究
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摘要
近年来,随着材料合成技术和材料制备方法的进一步深入发展,一些特殊功能结构材料(如核壳复合结构材料、空心结构材料)越来越得到人们的关注。核壳复合结构材料具有可设计性的特点,利用多种层次复合以及非线性复合效应等创造出全新性能的先进复合颗粒。同时,将核壳结构材料的内核去除而得到的具有空心结构的一类功能材料,也存在极大地研究价值。目前,溶胶-凝胶法是制备这些特殊粒子最常用、也是技术比较成熟的一种方法。
为了改善氢氧化镁与硅烷偶联剂之间的结合作用,本文采用溶胶-凝胶法以自制六方片状结构的氢氧化镁颗粒为模板,制备氢氧化镁/二氧化硅复合材料。实验中考察了不同pH值、反应温度、不同硅源等因素对制备复合粒子的影响。通过SEM、TEM、EDS、FT-IR等手段对粒子的形貌、化学组成、界面化学状态等进行了分析和表征,并对复合粒子的形成机理进行了分析,结果表明:以硅酸钠为硅源,pH为9.00,90℃的条件下可以制备出较好的Mg(OH)_2/SiO_2核壳复合结构粒子。二氧化硅和氢氧化镁颗粒界面处存在化学作用,二氧化硅对复合材料的比表面积的贡献率为120m2/g。经硅烷偶联剂改性后的复合粒子与改性后的氢氧化镁单相粒子相比具有活化指数高、分散性好、比表面积大的特点,且硅烷偶联剂与二氧化硅之间存在化学键合作用。以硅溶胶为硅源同样可以合成出Mg(OH)_2/SiO_2核壳复合结构粒子,温度升高有助于二氧化硅在氢氧化镁表面的包覆。本论文还对包覆机制进行理论解释以及实验验证,提出了吸附、聚合-异相成核、生长-凝胶成膜的包覆理论机制。
对以硅酸钠为硅源,溶胶-凝胶法制备Mg(OH)_2/SiO_2复合粒子的小试最佳条件进行了中试工艺初步探索,采用SEM、BET、FT-IR手段对Mg(OH)_2/SiO_2复合颗粒进行了分析表征,结果表明:二氧化硅在氢氧化镁表面是以薄膜的形式存在,复合粒子中氢氧化镁与二氧化硅之间存在化学作用。Mg(OH)_2/SiO_2复合粒子的中试制备工艺的初步探索为该复合粒子的工业化制备奠定了一定的基础。
在本实验室前期工作的基础上,本论文还对以针状纳米碳酸钙、氢氧化镁为模板,采用溶胶-凝胶法制备氧化铝空心结构的制备进行了探讨。实验结果表明:由于纳米碳酸钙和硝酸铝之间不存在较强的结合力,所以在本文的工艺和实验条件下,以纳米碳酸钙为模板制备氧化铝空心管的方法是不可行的。以偏铝酸钠为铝源制备出了残缺管状结构,说明偏铝酸钠与碳酸钙之间存在一定结合力。以偏铝酸钠为铝源选用水热法所制得产品较为理想,但需对其工艺条件进行进一步改进研究,从而制得空心管状氧化铝颗粒。以硝酸铝为铝源,水热六方片状氢氧化镁为模板采用水热法制备出了片状中空结构的γ-氧化铝颗粒,由于包覆层厚度的原因只有部分颗粒呈现完整空心结构。以硝酸铝为铝源,尝试反胶束方法制备出了均匀的棒状γ-氧化铝颗粒。
In recent years, with the development of technology of materials and Compositions, there has been great interest in concerning the synthesis of hollow structured materials with specific structures and different compositions. Composites with core-shell structure not only can combine the advantages of all ingredients, so their properties are better than any ingredient. And the control of their properties is easy because of the core-shell structure. So it has widely applications in many fields and has become a vital part in material research fields. Hollow materials are formed by removal of the core by a solvent or heating. Hollow materials have widely potential applications as delivery vehicles for the controlled release of drugs, dyes due to their special hollow structure. At present, the sol-gel method is the most widely way used to prepare these special particles.
In order to improve the integration between magnesium hydroxide and the silane coupling agent, a sol-gel approach was used to prepare the Mg(OH)_2/SiO_2 core-shell composite particles . The influence of pH, temperature, different silicon sources and other factors on the preparation of the composite particles were studied. The measurement of SEM, TEM, EDS, FT-IR were used to characterize the chemical composition, morphology, size and superficial crystal structure of the particles. The results show that, good Mg(OH)_2/SiO_2 particles with core-shell structure can be prepared under the conditions of sodium silicate as silica source, pH 9 and 90℃. There are chemical bonds between Mg(OH)2 and SiO2, a thin film of SiO2 with porous structure were coated on the surface of Mg(OH)2, the contribution rate of BET of the composite caused by SiO2 was 120m2/g.
The composite particles modified by the silane coupling agent have a feature of actived index,high specific surface area and good dispersion. Aslo there are chemical bonds between the silane coupling agent and SiO2. Under the condition of silica gel as silica source, Mg(OH)_2/SiO_2 core-shell composite can also be synthesized. High temperatures is preferred. After explained the coating theory and did experimental verification, a theory of adsorption process,“Sol- heterogeneous nucleation- growth-Gel film”was proposed.
The pilot experiments on the synthesiz of Mg(OH)_2/SiO_2 core-shell composite is also made. SEM, EDS, FT-IR, BET were used to characterize the chemical composition, morphology, size and superficial crystal structure of the particles. The results show that, there are chemical bonds between Mg(OH)2 and SiO2, a thin film of SiO2 of porous structure was coated on the surface of Mg(OH)2. It is important to make pilot experiments for the further scale-up of this process.
On the basis of previous experimental work, alumina hollow structure was prepared with sol-gel method by the use of needle-shaped nano-calcium carbonate and magnesium hydroxide as template. Because it does not exist strong bonding force between alumina nitrate and calcium carbonate, the preparation of alumina tube with alumina nitrate using nano-calcium carbonate as template is not feasible in experimental conditions. The experiments also were done with sodium aluminate as Al source using nano-calcium carbonate as template, and the results showed that there had incomplete tubular structures got in the product, which indicated that there are strong bonding force between sodium aluminate and nano-calcium carbonate. Using the hydrothermal method, we get better products with using sodium aluminate as the source and nano-calcium carbonate as template. And it is necessary to do further experiments to optimize the operation conditions. Using aluminum nitrate as the aluminum source, and magnesium hydroxide as a template by hydrothermal method, hollow sheet structure ofγ-alumina particles was obtained. Using aluminum nitrate as the aluminum source, uniformγ-alumina rod was obtained with the reverse micelles method.
为了改善氢氧化镁与硅烷偶联剂之间的结合作用,本文采用溶胶-凝胶法以自制六方片状结构的氢氧化镁颗粒为模板,制备氢氧化镁/二氧化硅复合材料。实验中考察了不同pH值、反应温度、不同硅源等因素对制备复合粒子的影响。通过SEM、TEM、EDS、FT-IR等手段对粒子的形貌、化学组成、界面化学状态等进行了分析和表征,并对复合粒子的形成机理进行了分析,结果表明:以硅酸钠为硅源,pH为9.00,90℃的条件下可以制备出较好的Mg(OH)_2/SiO_2核壳复合结构粒子。二氧化硅和氢氧化镁颗粒界面处存在化学作用,二氧化硅对复合材料的比表面积的贡献率为120m2/g。经硅烷偶联剂改性后的复合粒子与改性后的氢氧化镁单相粒子相比具有活化指数高、分散性好、比表面积大的特点,且硅烷偶联剂与二氧化硅之间存在化学键合作用。以硅溶胶为硅源同样可以合成出Mg(OH)_2/SiO_2核壳复合结构粒子,温度升高有助于二氧化硅在氢氧化镁表面的包覆。本论文还对包覆机制进行理论解释以及实验验证,提出了吸附、聚合-异相成核、生长-凝胶成膜的包覆理论机制。
对以硅酸钠为硅源,溶胶-凝胶法制备Mg(OH)_2/SiO_2复合粒子的小试最佳条件进行了中试工艺初步探索,采用SEM、BET、FT-IR手段对Mg(OH)_2/SiO_2复合颗粒进行了分析表征,结果表明:二氧化硅在氢氧化镁表面是以薄膜的形式存在,复合粒子中氢氧化镁与二氧化硅之间存在化学作用。Mg(OH)_2/SiO_2复合粒子的中试制备工艺的初步探索为该复合粒子的工业化制备奠定了一定的基础。
在本实验室前期工作的基础上,本论文还对以针状纳米碳酸钙、氢氧化镁为模板,采用溶胶-凝胶法制备氧化铝空心结构的制备进行了探讨。实验结果表明:由于纳米碳酸钙和硝酸铝之间不存在较强的结合力,所以在本文的工艺和实验条件下,以纳米碳酸钙为模板制备氧化铝空心管的方法是不可行的。以偏铝酸钠为铝源制备出了残缺管状结构,说明偏铝酸钠与碳酸钙之间存在一定结合力。以偏铝酸钠为铝源选用水热法所制得产品较为理想,但需对其工艺条件进行进一步改进研究,从而制得空心管状氧化铝颗粒。以硝酸铝为铝源,水热六方片状氢氧化镁为模板采用水热法制备出了片状中空结构的γ-氧化铝颗粒,由于包覆层厚度的原因只有部分颗粒呈现完整空心结构。以硝酸铝为铝源,尝试反胶束方法制备出了均匀的棒状γ-氧化铝颗粒。
In recent years, with the development of technology of materials and Compositions, there has been great interest in concerning the synthesis of hollow structured materials with specific structures and different compositions. Composites with core-shell structure not only can combine the advantages of all ingredients, so their properties are better than any ingredient. And the control of their properties is easy because of the core-shell structure. So it has widely applications in many fields and has become a vital part in material research fields. Hollow materials are formed by removal of the core by a solvent or heating. Hollow materials have widely potential applications as delivery vehicles for the controlled release of drugs, dyes due to their special hollow structure. At present, the sol-gel method is the most widely way used to prepare these special particles.
In order to improve the integration between magnesium hydroxide and the silane coupling agent, a sol-gel approach was used to prepare the Mg(OH)_2/SiO_2 core-shell composite particles . The influence of pH, temperature, different silicon sources and other factors on the preparation of the composite particles were studied. The measurement of SEM, TEM, EDS, FT-IR were used to characterize the chemical composition, morphology, size and superficial crystal structure of the particles. The results show that, good Mg(OH)_2/SiO_2 particles with core-shell structure can be prepared under the conditions of sodium silicate as silica source, pH 9 and 90℃. There are chemical bonds between Mg(OH)2 and SiO2, a thin film of SiO2 with porous structure were coated on the surface of Mg(OH)2, the contribution rate of BET of the composite caused by SiO2 was 120m2/g.
The composite particles modified by the silane coupling agent have a feature of actived index,high specific surface area and good dispersion. Aslo there are chemical bonds between the silane coupling agent and SiO2. Under the condition of silica gel as silica source, Mg(OH)_2/SiO_2 core-shell composite can also be synthesized. High temperatures is preferred. After explained the coating theory and did experimental verification, a theory of adsorption process,“Sol- heterogeneous nucleation- growth-Gel film”was proposed.
The pilot experiments on the synthesiz of Mg(OH)_2/SiO_2 core-shell composite is also made. SEM, EDS, FT-IR, BET were used to characterize the chemical composition, morphology, size and superficial crystal structure of the particles. The results show that, there are chemical bonds between Mg(OH)2 and SiO2, a thin film of SiO2 of porous structure was coated on the surface of Mg(OH)2. It is important to make pilot experiments for the further scale-up of this process.
On the basis of previous experimental work, alumina hollow structure was prepared with sol-gel method by the use of needle-shaped nano-calcium carbonate and magnesium hydroxide as template. Because it does not exist strong bonding force between alumina nitrate and calcium carbonate, the preparation of alumina tube with alumina nitrate using nano-calcium carbonate as template is not feasible in experimental conditions. The experiments also were done with sodium aluminate as Al source using nano-calcium carbonate as template, and the results showed that there had incomplete tubular structures got in the product, which indicated that there are strong bonding force between sodium aluminate and nano-calcium carbonate. Using the hydrothermal method, we get better products with using sodium aluminate as the source and nano-calcium carbonate as template. And it is necessary to do further experiments to optimize the operation conditions. Using aluminum nitrate as the aluminum source, and magnesium hydroxide as a template by hydrothermal method, hollow sheet structure ofγ-alumina particles was obtained. Using aluminum nitrate as the aluminum source, uniformγ-alumina rod was obtained with the reverse micelles method.
引文
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