纳米及介孔金属氧化物材料新合成方法探索研究
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摘要
纳米结构材料,是指三维空间尺度至少有一维处于纳米量级(1-100 nm)的材料,包括纳米尺寸材料和纳米孔材料。当纳米结构材料的尺寸小到纳米量级时,则会表现出独特的物理化学性质,在催化,吸附、分离、传感、药物负载、光电等众多领域有着广泛的应用前景。本论文分别以Fe3O4纳米粒子、介孔-大孔TiO2、有序介孔金属氧化物(Fe2O3、Cr2O3、In2O3、CeO2、Co3O4、NiO、ITO和Mn3O4)为研究对象,探索其新颖的合成方法、最优的调控路线和调控机制,实现对尺寸、结构、形貌、晶型及物性的有效调变,对深入研究材料制备、结构与性能的关系具有重要的意义。具体研究内容如下：
首次分别以p-环糊精或蔗糖为绿色双功能促进剂,以廉价的三价氯化铁为铁源,成功的制备出粒子尺寸小于20nm的超顺磁性磁铁矿。磁铁矿纳米粒子的尺寸可随p-环糊精或蔗糖浓度的变化而变化。并对整个反应过程的机理进行了详细的研究。p-环糊精或蔗糖一方面起到绿色还原剂前驱体的作用,温和还原三价铁制备磁铁矿,且防止制备得到的磁铁矿再次被氧化。从而使整个制备过程无需纯化或保护流程,易于实现。另一方面,p-环糊精或蔗糖又有包覆剂前体的作用,修饰所制备的磁铁矿的表面,控制其生长,从而制得尺寸可调且超顺磁性的纳米粒子。制备得到的磁铁矿纳米粒子的饱和磁化强度随粒子尺寸的改变而在一定范围内变化。
首次采用简单易得的细胞作为生物模板,通过生物灵感法成功制备出介孔-大孔多级孔TiO2材料。且其大孔形貌可随细胞组装体形貌的改变而变化,分别为具有球状大孔、杆状大孔及蠕虫状大孔的介孔-大孔TiO2材料。并对其光催化性能进行了详细的研究,结果表明将介孔的高比表面积、多的活性位点与大孔的通透、易传质性质相结合,有利于催化性能的提高,且相对纳米粒子更有助于回收利用。
用纳米浇铸法制备有序介孔金属氧化物材料,首次发现影响其介孔有序性形貌和结晶度的热处理调变方法及其“迁移机理”。从而可以在大范围内调变以金属硝酸盐为前驱体纳米浇铸法制备的金属氧化物材料的介孔有序性和结晶度。适用的金属氧化物包括：Fe2O3、Cr2O3、In2O3、CeO2、C03O4、NiO和Mn3O4。并深入研究了该简单易行方法背后的“迁移”机理,从而可以对金属氧化物材料的介孔有序性和结晶度进行连续调变。其金属氧化物的形貌和结晶度可以从高结晶的有序介孔微米级大颗粒调变到低结晶甚至无定形的纳米粒子。同时,有序介孔Fe203的热处理温度从600℃降到仅为150℃。
首次采用后掺杂纳米浇铸法制备高度有序介孔氧化铟锡(ITO)材料。并运用“迁移机理”,调变ITO材料的形貌和结晶度从高结晶的有序介孔ITO大颗粒(微米级)到低结晶的ITO纳米粒子。并考察纳米浇铸法后掺杂Sn含量、热处理气氛、热处理温度等因素对其结构、形貌、透光及导电性质的影响。
"Nanostructured Materials", also called "Nanomaterials", are materials with one or more dimensions in the 1-100 nm range, including nanosized materials and nanoporous materials. These materials, notable for their extremely small feature size, have special physic-chemical properties and have the potential for wide-ranging applications, such as catalysis, adsorption, separation, sensor, drug delivery and photoelectricity. In this work, magnetite nanoparticles, meso-macroporous TiO2, and ordered mesoporous metal oxides (including Fe2O3, Cr2O3,In2O3, CeO2,Co3O4, NiO, ITO and Mn3O4) have been synthesized in novel ways. The sizes, morphology,phase and properties of these materials have been controlled and adjusted using feasible methods. Especially, the actual mechanism, which affects the synthesis, has been studied in detail. The main contents of this dissertation are following:
Novel and facileβ-cyclodextrin-assisted (β-CD-assisted) or sucrose-assisted methods have been employed to prepare superparamagnetic Fe3O4 nanoparticles from a'single iron precursor of FeCl3. Various characterization involving X-raydiffraction (XRD), standard and high-resolution transmission electron microscopy (TEM and HRTEM), electron diffraction (ED), and Raman spectroscopy has integrally testified the formation of pure magnetite nanoparticles with homogeneous morphology. The size of nanoparticles can be adjusted by varying the concentration ofβ-CD or sucrose. The success is ascribed to in situ formation of reducing agent originating from the self-decomposition of P-CD or sucrose under the reaction conditions, which partly reduces Fe3+ ions into Fe2+ ions for final formation of Fe3O4. Another function ofβ-CD or sucrose is also discussed:that they also act as the coating agent to prevent particle growth and agglomeration, which allows the formation of nanoscale and superparamagnetic magnetite with different particle sizes. The saturation magnetization of the as-obtained magnetite is measured and is strongly related to the particle size.
Cell-assemblies with different cell shapes have been used as macrotemplates in the bioinspired synthesis of hierarchical meso-macroporous titania with tunable macroporous morphology. The porous materials exhibit relatively homogeneous and uniform macropores with spheroidal, baculiform, and wormlike porous shapes, respectively. The photocatalytic performance of the meso-macroporous titania has also been evaluated by degrading methylene blue (MB) under UV irradiation, which indicates that an optimal catalyst should combine large pores (enabling high substance flow rates) with smaller pores (ensuring high substrate-substance contact) in a connected network.
During the synthesis of mesoprous metal oxides using nanocasting method from metal nitrate precursors, a simple and general "thermal treatment" strategy to control the morphology of mesoporous periodicity and crystallinity in a large range has been found. The mechanism behind the phenomenon is discussed in detail and explained clearly as "migration mechanism". The preparation of mesoporous hematite will be first demonstrated as an example, followed by all the other metal oxide examples (including Cr2O3, In2O3, CeO2, Co3O4, NiO and Mn3O4). The morphology and crystallinity can be controlled from ordered mesoporous particles in micrometer dimension with high crystallinity to nanoparticles with low crystallinity in succession. The thermal treatment temperature for Fe2O3 can be decreased from 600℃to only 150℃.
Ordered mesoporous indium tin oxide (ITO) materials have been synthesized using nanocasting method with post-doping strategy. The mesoporous morphology and crystallinity can be controlled easily using "migration mechanism" from ordered mesoporous particles in micrometer dimension with high crystallinity to nanoparticles with low crystallinity in succession. The structure, morphology, transparent and conducting properties of the ITO materials have been discussed in detail with different tin contents, thermal treatment atmosphere and temperatures.
首次分别以p-环糊精或蔗糖为绿色双功能促进剂,以廉价的三价氯化铁为铁源,成功的制备出粒子尺寸小于20nm的超顺磁性磁铁矿。磁铁矿纳米粒子的尺寸可随p-环糊精或蔗糖浓度的变化而变化。并对整个反应过程的机理进行了详细的研究。p-环糊精或蔗糖一方面起到绿色还原剂前驱体的作用,温和还原三价铁制备磁铁矿,且防止制备得到的磁铁矿再次被氧化。从而使整个制备过程无需纯化或保护流程,易于实现。另一方面,p-环糊精或蔗糖又有包覆剂前体的作用,修饰所制备的磁铁矿的表面,控制其生长,从而制得尺寸可调且超顺磁性的纳米粒子。制备得到的磁铁矿纳米粒子的饱和磁化强度随粒子尺寸的改变而在一定范围内变化。
首次采用简单易得的细胞作为生物模板,通过生物灵感法成功制备出介孔-大孔多级孔TiO2材料。且其大孔形貌可随细胞组装体形貌的改变而变化,分别为具有球状大孔、杆状大孔及蠕虫状大孔的介孔-大孔TiO2材料。并对其光催化性能进行了详细的研究,结果表明将介孔的高比表面积、多的活性位点与大孔的通透、易传质性质相结合,有利于催化性能的提高,且相对纳米粒子更有助于回收利用。
用纳米浇铸法制备有序介孔金属氧化物材料,首次发现影响其介孔有序性形貌和结晶度的热处理调变方法及其“迁移机理”。从而可以在大范围内调变以金属硝酸盐为前驱体纳米浇铸法制备的金属氧化物材料的介孔有序性和结晶度。适用的金属氧化物包括：Fe2O3、Cr2O3、In2O3、CeO2、C03O4、NiO和Mn3O4。并深入研究了该简单易行方法背后的“迁移”机理,从而可以对金属氧化物材料的介孔有序性和结晶度进行连续调变。其金属氧化物的形貌和结晶度可以从高结晶的有序介孔微米级大颗粒调变到低结晶甚至无定形的纳米粒子。同时,有序介孔Fe203的热处理温度从600℃降到仅为150℃。
首次采用后掺杂纳米浇铸法制备高度有序介孔氧化铟锡(ITO)材料。并运用“迁移机理”,调变ITO材料的形貌和结晶度从高结晶的有序介孔ITO大颗粒(微米级)到低结晶的ITO纳米粒子。并考察纳米浇铸法后掺杂Sn含量、热处理气氛、热处理温度等因素对其结构、形貌、透光及导电性质的影响。
"Nanostructured Materials", also called "Nanomaterials", are materials with one or more dimensions in the 1-100 nm range, including nanosized materials and nanoporous materials. These materials, notable for their extremely small feature size, have special physic-chemical properties and have the potential for wide-ranging applications, such as catalysis, adsorption, separation, sensor, drug delivery and photoelectricity. In this work, magnetite nanoparticles, meso-macroporous TiO2, and ordered mesoporous metal oxides (including Fe2O3, Cr2O3,In2O3, CeO2,Co3O4, NiO, ITO and Mn3O4) have been synthesized in novel ways. The sizes, morphology,phase and properties of these materials have been controlled and adjusted using feasible methods. Especially, the actual mechanism, which affects the synthesis, has been studied in detail. The main contents of this dissertation are following:
Novel and facileβ-cyclodextrin-assisted (β-CD-assisted) or sucrose-assisted methods have been employed to prepare superparamagnetic Fe3O4 nanoparticles from a'single iron precursor of FeCl3. Various characterization involving X-raydiffraction (XRD), standard and high-resolution transmission electron microscopy (TEM and HRTEM), electron diffraction (ED), and Raman spectroscopy has integrally testified the formation of pure magnetite nanoparticles with homogeneous morphology. The size of nanoparticles can be adjusted by varying the concentration ofβ-CD or sucrose. The success is ascribed to in situ formation of reducing agent originating from the self-decomposition of P-CD or sucrose under the reaction conditions, which partly reduces Fe3+ ions into Fe2+ ions for final formation of Fe3O4. Another function ofβ-CD or sucrose is also discussed:that they also act as the coating agent to prevent particle growth and agglomeration, which allows the formation of nanoscale and superparamagnetic magnetite with different particle sizes. The saturation magnetization of the as-obtained magnetite is measured and is strongly related to the particle size.
Cell-assemblies with different cell shapes have been used as macrotemplates in the bioinspired synthesis of hierarchical meso-macroporous titania with tunable macroporous morphology. The porous materials exhibit relatively homogeneous and uniform macropores with spheroidal, baculiform, and wormlike porous shapes, respectively. The photocatalytic performance of the meso-macroporous titania has also been evaluated by degrading methylene blue (MB) under UV irradiation, which indicates that an optimal catalyst should combine large pores (enabling high substance flow rates) with smaller pores (ensuring high substrate-substance contact) in a connected network.
During the synthesis of mesoprous metal oxides using nanocasting method from metal nitrate precursors, a simple and general "thermal treatment" strategy to control the morphology of mesoporous periodicity and crystallinity in a large range has been found. The mechanism behind the phenomenon is discussed in detail and explained clearly as "migration mechanism". The preparation of mesoporous hematite will be first demonstrated as an example, followed by all the other metal oxide examples (including Cr2O3, In2O3, CeO2, Co3O4, NiO and Mn3O4). The morphology and crystallinity can be controlled from ordered mesoporous particles in micrometer dimension with high crystallinity to nanoparticles with low crystallinity in succession. The thermal treatment temperature for Fe2O3 can be decreased from 600℃to only 150℃.
Ordered mesoporous indium tin oxide (ITO) materials have been synthesized using nanocasting method with post-doping strategy. The mesoporous morphology and crystallinity can be controlled easily using "migration mechanism" from ordered mesoporous particles in micrometer dimension with high crystallinity to nanoparticles with low crystallinity in succession. The structure, morphology, transparent and conducting properties of the ITO materials have been discussed in detail with different tin contents, thermal treatment atmosphere and temperatures.
引文
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