水滑石向复合金属氧化物的转晶机制及相关产物性能研究
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摘要
由层状双羟基复合金属氧化物材料(layered double hydroxides,简称LDHs,又叫类水滑石)在高温氧化条件下转化所得复合金属氧化物材料(Mixed Metal Oxides,简称MMO)在催化、磁学、光学等领域有着广泛的应用前景。在由LDHs向MMO转化过程中,材料的微观结构、物相组成及宏观形貌等发生一系列规律变化；同时,材料的最终性能也是与上述结构及物相变化密切相关的。本论文围绕LDHs材料高温转晶机制及所形成MMO材料的相界面处相互耦合作用导致性能的(?)系列变化开展基础研究。针对目前该领域中的科学问题,首先选取ZnAl-LDHs为前驱体,系统研究了其在高温转晶过程中的微观结构及物相变化,并提出相关LDHs向MMO的转晶机制。在此基础上,分别研究了MMO材料中不同物相界面处的耦合作用对最终性能的影响。此外,针对LDHs材料在光催化领域的争议,探讨了其去除有机染料分子中的真实原因。本研究工作可望为深入理解LDHs高温转晶过程及基于实际需要对MMO材料进行构筑并对最终性能进行调控奠定一定理论和实验基础。
本论文的创新点和研究结果如下：
首先,针对LDHs在高温氧化条件下的转晶机制这一关键科学问题,以ZnAl-LDHs为前驱体,采用包括高分辨投射电镜在内的多种表征手段对其向最终ZnO/ZnAl2O4纳米复合材料的转化过程进行研究。结果证实,ZnAl-LDHs分别经历了水滑石结构破坏与ZnO成核、ZnO的取向生长与ZnO/ZnAl2O4复合材料形成的三个阶段。在此基础上,提出了相关的LDHs向MMO的转晶机制,同时,该机制被证明具有良好的普适性。
其次,基于LDHs向MMO转化过程中的结构特征,研究了ZnO/ZnAl2O4复合纳米材料的光催化性能。经高温转化后,在ZnAl2O4和ZnO相界面处形成了纳米异质结的结构；因此两种半导体物相间存在较强耦合作用,有利于分离光生电子—空穴对,从而与单相ZnO材料相比,所得ZnO/ZnAl2O4复合纳米材料具有更高的光催化活性。
第三,针对纳米磁性粒子存在的“超顺磁限制”问题,以NiFe-LDHs为前体,在高温条件下利用LDHs的拓扑效应制备得到NiO/NiFe2O4纳米复合材料。NiO和NiFe2O4相界面处较强的铁磁/反铁磁相互耦合作用有效提高了NiFe2O4纳米粒子的磁热稳定性。与相同粒径的NiFe2O4粒子相比,NiO/NiFe2O4纳米复合材料中的NiFe2O4的截止温度(TB)提高了200K以上。
本论文最后针对LDHs材料在去除有机染料分子领域的广泛应用,深入探讨了该反应本质。选取代表性MgAl-LDHs和ZnCr-LDHs为研究对象,基于一系列光照/暗处条件的去除不同染料分子实验及密度泛函计算结果,讨论了MgAl-LDHs和ZnCr-LDHs去除有机染料分子及ZnCr-LDHs不具备光催化活性的真实原因。
The mixted metal oxides (MMO) material, derived from Layered double hydroxides (LDHs) precursor after thermal treatment under high temperature, has potentially been used in many fields such as catalysis, magnetic, opticals and so on. The properties preformed by the MMO material are closely related with the microstructure, the composition and the morphology transformation from LDHs precursor. In the present thesis, we discuss the transformation mechanism of LDHs precursors under high temperature, and then focous on the relationship between the properties and the coupling interaction on the interface of different phases of the MMO material. Firstly, ZnAl-LDHs were chosed and studied the microstructure as well as composition transformation during the transformation process, and the transformation mechanism was proposed based on the experimental results. Then coupling effects on the properties of the MMO material, including the photocatalytic and magnetic properties were studied respectively. Moreover, considering the controversy about LDHs material in the photocatalytic field, we discuss the real cause of the removal of organic dye molecules using pristine LDHs materal. We believe that our work can be regarded as theorical and experimental basis for the understanding of the transformation mechanism from LDHs precursors to MMO material, and it also can provide some information for the structural design as well as the property regulation of the MMO material according to the actural requirments.
The innovation of this thesis and results are as follows:
Fristly, aiming at the point about the transformation mechanism under high temperature, the ZnAl-LDHs precursors were firstly chosed, and the transformation process to the ZnO/ZnAl2O4 nanocomposites were studied based on the various characterization methods including high resolution transmission electron microscope (HRTEM). The final results indicated that, the ZnAl-LDHs underwent three stages under different thermal treatment condition, includingⅰ) the destruction of the LDHs precursors and the formation of ZnO crystal nucleus;ⅱ) the orientional growth of ZnO andⅲ) the formation of ZnO/ZnAl2O4 nanocomposites. The transformation mechanism was proposed and it also has been proved to show good university.
Secondly, based on the structural feature of the ZnO/ZnAl2O4 nanocomposites derived from ZnAl-LDHs precursors, the photocatalytic properties of the ZnO/ZnAl2O4 were discussed. After the thermal treatment, the nanoheterjunction structure was formed on the interface between the ZnO and ZnAl2O4 phases, and the strong coupling interaction between the two semiconductors made for the separation of photo-induced electron-hole pairs. Therefore, compared with single phase ZnO or similar ZnO/ZnAl2O4 fabricated by other physiochemical methods, the ZnO/ZnAl2O4 derived from ZnAL-LDHs precursors showed higher photocatalytic activity.
Thirdly, in order to beat "superparamagnetic limit" of ferromagnetic nanoparticles, the NiO/NiFe2O4 nanocomposites were fabricated from NiFe-LDHs precursors after the topotactic transformation under high temperature. The strong ferromagnetic (FM)-antiferromagnetic (AFM) coupling interaction between the NiO and NiFe2O4 phases leads to the obvious improvement of the magnetic stability of the NiFe2O4 nanoparticles. The blocking temperature of NiFe2O4 nanoparticles in NiO/NiFe2O4 nanocomposite film increased more than 200 K than that for pure NiFe2O4 nanoparticles with similar size.
Finally, considering the extensive use of LDHs in the field of removal of organic dye molecules in the solution, the reaction essence was discussed. Representative MgAl-LDHs and ZnCr-LDHs were chosed; then series of experiments under/without visible light irradiation and density functional computation have been done. The real reason for the removal of different organic dye molecoules from the solution with the MgAl-LDHs and ZnCr-LDHs were discussed.
本论文的创新点和研究结果如下：
首先,针对LDHs在高温氧化条件下的转晶机制这一关键科学问题,以ZnAl-LDHs为前驱体,采用包括高分辨投射电镜在内的多种表征手段对其向最终ZnO/ZnAl2O4纳米复合材料的转化过程进行研究。结果证实,ZnAl-LDHs分别经历了水滑石结构破坏与ZnO成核、ZnO的取向生长与ZnO/ZnAl2O4复合材料形成的三个阶段。在此基础上,提出了相关的LDHs向MMO的转晶机制,同时,该机制被证明具有良好的普适性。
其次,基于LDHs向MMO转化过程中的结构特征,研究了ZnO/ZnAl2O4复合纳米材料的光催化性能。经高温转化后,在ZnAl2O4和ZnO相界面处形成了纳米异质结的结构；因此两种半导体物相间存在较强耦合作用,有利于分离光生电子—空穴对,从而与单相ZnO材料相比,所得ZnO/ZnAl2O4复合纳米材料具有更高的光催化活性。
第三,针对纳米磁性粒子存在的“超顺磁限制”问题,以NiFe-LDHs为前体,在高温条件下利用LDHs的拓扑效应制备得到NiO/NiFe2O4纳米复合材料。NiO和NiFe2O4相界面处较强的铁磁/反铁磁相互耦合作用有效提高了NiFe2O4纳米粒子的磁热稳定性。与相同粒径的NiFe2O4粒子相比,NiO/NiFe2O4纳米复合材料中的NiFe2O4的截止温度(TB)提高了200K以上。
本论文最后针对LDHs材料在去除有机染料分子领域的广泛应用,深入探讨了该反应本质。选取代表性MgAl-LDHs和ZnCr-LDHs为研究对象,基于一系列光照/暗处条件的去除不同染料分子实验及密度泛函计算结果,讨论了MgAl-LDHs和ZnCr-LDHs去除有机染料分子及ZnCr-LDHs不具备光催化活性的真实原因。
The mixted metal oxides (MMO) material, derived from Layered double hydroxides (LDHs) precursor after thermal treatment under high temperature, has potentially been used in many fields such as catalysis, magnetic, opticals and so on. The properties preformed by the MMO material are closely related with the microstructure, the composition and the morphology transformation from LDHs precursor. In the present thesis, we discuss the transformation mechanism of LDHs precursors under high temperature, and then focous on the relationship between the properties and the coupling interaction on the interface of different phases of the MMO material. Firstly, ZnAl-LDHs were chosed and studied the microstructure as well as composition transformation during the transformation process, and the transformation mechanism was proposed based on the experimental results. Then coupling effects on the properties of the MMO material, including the photocatalytic and magnetic properties were studied respectively. Moreover, considering the controversy about LDHs material in the photocatalytic field, we discuss the real cause of the removal of organic dye molecules using pristine LDHs materal. We believe that our work can be regarded as theorical and experimental basis for the understanding of the transformation mechanism from LDHs precursors to MMO material, and it also can provide some information for the structural design as well as the property regulation of the MMO material according to the actural requirments.
The innovation of this thesis and results are as follows:
Fristly, aiming at the point about the transformation mechanism under high temperature, the ZnAl-LDHs precursors were firstly chosed, and the transformation process to the ZnO/ZnAl2O4 nanocomposites were studied based on the various characterization methods including high resolution transmission electron microscope (HRTEM). The final results indicated that, the ZnAl-LDHs underwent three stages under different thermal treatment condition, includingⅰ) the destruction of the LDHs precursors and the formation of ZnO crystal nucleus;ⅱ) the orientional growth of ZnO andⅲ) the formation of ZnO/ZnAl2O4 nanocomposites. The transformation mechanism was proposed and it also has been proved to show good university.
Secondly, based on the structural feature of the ZnO/ZnAl2O4 nanocomposites derived from ZnAl-LDHs precursors, the photocatalytic properties of the ZnO/ZnAl2O4 were discussed. After the thermal treatment, the nanoheterjunction structure was formed on the interface between the ZnO and ZnAl2O4 phases, and the strong coupling interaction between the two semiconductors made for the separation of photo-induced electron-hole pairs. Therefore, compared with single phase ZnO or similar ZnO/ZnAl2O4 fabricated by other physiochemical methods, the ZnO/ZnAl2O4 derived from ZnAL-LDHs precursors showed higher photocatalytic activity.
Thirdly, in order to beat "superparamagnetic limit" of ferromagnetic nanoparticles, the NiO/NiFe2O4 nanocomposites were fabricated from NiFe-LDHs precursors after the topotactic transformation under high temperature. The strong ferromagnetic (FM)-antiferromagnetic (AFM) coupling interaction between the NiO and NiFe2O4 phases leads to the obvious improvement of the magnetic stability of the NiFe2O4 nanoparticles. The blocking temperature of NiFe2O4 nanoparticles in NiO/NiFe2O4 nanocomposite film increased more than 200 K than that for pure NiFe2O4 nanoparticles with similar size.
Finally, considering the extensive use of LDHs in the field of removal of organic dye molecules in the solution, the reaction essence was discussed. Representative MgAl-LDHs and ZnCr-LDHs were chosed; then series of experiments under/without visible light irradiation and density functional computation have been done. The real reason for the removal of different organic dye molecoules from the solution with the MgAl-LDHs and ZnCr-LDHs were discussed.
引文
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