几种一维无机纳米材料的液相合成及机理研究
摘要
合成一维无机纳米材料,探索其合成方法与调控机制,实现对尺寸、维度及物性的有效调控,对深入研究材料结构与性能的关系具有重要的意义。本论文旨在探索合成一维无机纳米材料液相控制合成新思路,通过设计合理的反应路线、控制实验参数,在水热和声化学方法制备纳米材料的基础上合成Ni(SO_4)_(0.3)(OH)_(1.4)、NiO、CdCO_3、CdO、CaSn(OH)_6、CaCO_3等多种功能纳米材料的一维纳米结构,包括纳米片、纳米线和纳米带,以及单晶纳米管等,并深入研究了它们的生长机理和相关性质。具体归纳如下:
(1)以低成本无机小分子-氨水分子为配位剂,与Ni~(2+)离子配合形成[Ni(NH_3)_6]~(2+)配合离子,以无水乙醇/水为溶剂限制配合离子的水解速度,采用一个简单、无模板的水热方法合成了(Ni(SO_4)_(0.3)(OH)_(1.4))纳米带,并实现了控制纳米材料形貌的目的。另外,经过不同温度的热处理,获得了多种形貌的晶体NiO和无定形硫酸镍混合物纳米结构,例如:纳米带、多孔纳米带和纳米颗粒。详细的机理研究表明,硫酸根基团对于纳米带的形成起着重要的作用。该方法简单、成本低廉、产率高,易于大规模生产。初步研究还表明,该方法可成功推广至合成其他过渡金属状化合物,显示了该方法可普遍用于合成其它无机层状化合物。
(2)在低温、无模板的条件下,利用液相法得到了形貌可控的CdCO_3纳米晶,通过实验参数的调整可得到纳米线、纳米带和纳米片等形貌,尤其还获得了一维分等级复杂结构的CdCO_3纳米晶体。机理研究表明,溶液中单体的净扩散流量对于晶体的生长性质和形貌控制有至关重要的影响。在我们的实验中,通过调控氨水的浓度、温度等反应条件可以方便地控制溶液中单体的净扩散流量,从而实现了对于CdCO_3纳米晶体的生长模式和形貌的控制。
另外,通过对CdCO_3纳米晶进行适当的热处理,本工作还首次得到了多种形貌的多孔CdO纳米单晶材料,为制备Ⅱ-Ⅵ族一维纳米半导体单晶材料提供了一种简单且具有规模化生产前景的新途径。
(3)采用声化学方法,在不使用任何模板的条件下,通过简单的超声处理我们首次得到了CaSn(OH)_6纳米管单晶和多种形貌的CaCO_3单晶一维纳米结构,如:纳米线,纳米片,以及少见的六方纳米盘。在合成过程中我们发现:这些纳米线和纳米管的形成和晶化过程明显地受到合成环境中所包含的异类无机阴离子以及溶液pH值的影响。通过研究介稳的随时间变化的中间状态,探索了晶化控制的影响因素以及晶化与空间限域之间的复杂的相互作用,从而对纳米管和纳米线的形成机制进行了合理理解,并且这种新颖的简单的纳米管合成方法及其生长机理为其他纳米管材料的合成提供了一定的指导作用。利用同样的方法,我们还成功合成了SrSn(OH)_6、BaSn(OH)_6、SrCO_3和BaCO_3纳米线或纳米棒。
In this dissertation, based on the hydrothermal and sonochemical methods, new wet chemical synthesis routes were explored to prepare one-dimensional (1D) nanomaterials. 1D nanostructures including nanowires, nanobelts, nanotubes and nanoplates of various hydroxides and carbonates materials, such as nickel hydroxyl sulfate (Ni(SO_4)_(0.3)(OH)_(1.4)), cadmium carbonate (CdCO_3), alkaline stannates and carbonates were synthesized by designing possible chemical reactions and controlling the experimental parameters. Porous 1D nanostructures of their corresponding metal oxides were also obtained through heat treatments. At the same time, their growth mechanisms were also studied. The experimental details are summarized as follows:
(1) Nanobelts of nickel hydroxyl sulfate have been prepared on a large scale via a simple template-free hydrothermal reaction on the basis of a complex [Ni(NH_3)_6]~(2+) formed with Ni~(2+) and ammonia in an ethanol-water solution. Furthermore, nanostructures of mixture of crystralline NiO and amorphous nickel sulfate with various morphologies, such as nanobelts, porous nanobelts, and nanoparticles, were obtained by thermal treatment of the as-synthesized Ni(SO_4)_(0.3)(OH)_(1.4) nanobelts at different temperatures. Based on the temporal-dependent SEM and XRD evidences, we could find that that the sulfate group inserting should be responsible to the shape transformation from layer structure to nanobelts. As a matter of fact, our experiments may provides a general, simple, and effective method to control the shape of single-metal layered hydroxy salts in aqueous solution, and are also suitable to the synthesis of other hydroxide double salts (HDSs) and layered double hydroxides (LDHs) which contain i.e.Cd~(2+), Zn~(2+), Cu~(2+), Co~(2+) and Co~(3+) ions.
(2) Low-dimensional single crystalline CdCO_3 nanostructures such as nanowires, nanobelts, nanorolls and 1D hierarchical structures have been successfully synthesized through a convenient, low-temperature hydrothermal method. The influences of ammonia concentration, reaction time and temperature on the morphologies of CdCO_3 were investigated. In addition, these low-dimensional nanostructures could be transformed into oriented CdO nanoporous structures through heat treatment process, and the corresponding shapes can be preserved completely.
(3) We have used the sonochemical approach to firstly synthesize CaSn(OH)_6 single crystal nanotubes, and various single crystals anisotropic shapes of CaCO_3 such as nanowires, nanosheets and unusually obtained nanoplates without using any template at room temperature. The complex interplay between crystallization processes and self-assembly resulting from spatial constrains had been investigated through studying the structural evolution of metastable intermediates synthesized. crystallization pathway involved in nanotubes and nanowires formation under the condition of sonication. Moreover, this approach is suitable to the anisotropic single crystals synthesis of other alkaline earth stannates and carbonates such as SrSn(OH)_6, BaSn(OH)_6, SrCO_3 and BaCO_3. It also gives a new demonstration of sonochemical effects on the crystallization and assembly of block building in the mesoscale.
(1)以低成本无机小分子-氨水分子为配位剂,与Ni~(2+)离子配合形成[Ni(NH_3)_6]~(2+)配合离子,以无水乙醇/水为溶剂限制配合离子的水解速度,采用一个简单、无模板的水热方法合成了(Ni(SO_4)_(0.3)(OH)_(1.4))纳米带,并实现了控制纳米材料形貌的目的。另外,经过不同温度的热处理,获得了多种形貌的晶体NiO和无定形硫酸镍混合物纳米结构,例如:纳米带、多孔纳米带和纳米颗粒。详细的机理研究表明,硫酸根基团对于纳米带的形成起着重要的作用。该方法简单、成本低廉、产率高,易于大规模生产。初步研究还表明,该方法可成功推广至合成其他过渡金属状化合物,显示了该方法可普遍用于合成其它无机层状化合物。
(2)在低温、无模板的条件下,利用液相法得到了形貌可控的CdCO_3纳米晶,通过实验参数的调整可得到纳米线、纳米带和纳米片等形貌,尤其还获得了一维分等级复杂结构的CdCO_3纳米晶体。机理研究表明,溶液中单体的净扩散流量对于晶体的生长性质和形貌控制有至关重要的影响。在我们的实验中,通过调控氨水的浓度、温度等反应条件可以方便地控制溶液中单体的净扩散流量,从而实现了对于CdCO_3纳米晶体的生长模式和形貌的控制。
另外,通过对CdCO_3纳米晶进行适当的热处理,本工作还首次得到了多种形貌的多孔CdO纳米单晶材料,为制备Ⅱ-Ⅵ族一维纳米半导体单晶材料提供了一种简单且具有规模化生产前景的新途径。
(3)采用声化学方法,在不使用任何模板的条件下,通过简单的超声处理我们首次得到了CaSn(OH)_6纳米管单晶和多种形貌的CaCO_3单晶一维纳米结构,如:纳米线,纳米片,以及少见的六方纳米盘。在合成过程中我们发现:这些纳米线和纳米管的形成和晶化过程明显地受到合成环境中所包含的异类无机阴离子以及溶液pH值的影响。通过研究介稳的随时间变化的中间状态,探索了晶化控制的影响因素以及晶化与空间限域之间的复杂的相互作用,从而对纳米管和纳米线的形成机制进行了合理理解,并且这种新颖的简单的纳米管合成方法及其生长机理为其他纳米管材料的合成提供了一定的指导作用。利用同样的方法,我们还成功合成了SrSn(OH)_6、BaSn(OH)_6、SrCO_3和BaCO_3纳米线或纳米棒。
In this dissertation, based on the hydrothermal and sonochemical methods, new wet chemical synthesis routes were explored to prepare one-dimensional (1D) nanomaterials. 1D nanostructures including nanowires, nanobelts, nanotubes and nanoplates of various hydroxides and carbonates materials, such as nickel hydroxyl sulfate (Ni(SO_4)_(0.3)(OH)_(1.4)), cadmium carbonate (CdCO_3), alkaline stannates and carbonates were synthesized by designing possible chemical reactions and controlling the experimental parameters. Porous 1D nanostructures of their corresponding metal oxides were also obtained through heat treatments. At the same time, their growth mechanisms were also studied. The experimental details are summarized as follows:
(1) Nanobelts of nickel hydroxyl sulfate have been prepared on a large scale via a simple template-free hydrothermal reaction on the basis of a complex [Ni(NH_3)_6]~(2+) formed with Ni~(2+) and ammonia in an ethanol-water solution. Furthermore, nanostructures of mixture of crystralline NiO and amorphous nickel sulfate with various morphologies, such as nanobelts, porous nanobelts, and nanoparticles, were obtained by thermal treatment of the as-synthesized Ni(SO_4)_(0.3)(OH)_(1.4) nanobelts at different temperatures. Based on the temporal-dependent SEM and XRD evidences, we could find that that the sulfate group inserting should be responsible to the shape transformation from layer structure to nanobelts. As a matter of fact, our experiments may provides a general, simple, and effective method to control the shape of single-metal layered hydroxy salts in aqueous solution, and are also suitable to the synthesis of other hydroxide double salts (HDSs) and layered double hydroxides (LDHs) which contain i.e.Cd~(2+), Zn~(2+), Cu~(2+), Co~(2+) and Co~(3+) ions.
(2) Low-dimensional single crystalline CdCO_3 nanostructures such as nanowires, nanobelts, nanorolls and 1D hierarchical structures have been successfully synthesized through a convenient, low-temperature hydrothermal method. The influences of ammonia concentration, reaction time and temperature on the morphologies of CdCO_3 were investigated. In addition, these low-dimensional nanostructures could be transformed into oriented CdO nanoporous structures through heat treatment process, and the corresponding shapes can be preserved completely.
(3) We have used the sonochemical approach to firstly synthesize CaSn(OH)_6 single crystal nanotubes, and various single crystals anisotropic shapes of CaCO_3 such as nanowires, nanosheets and unusually obtained nanoplates without using any template at room temperature. The complex interplay between crystallization processes and self-assembly resulting from spatial constrains had been investigated through studying the structural evolution of metastable intermediates synthesized. crystallization pathway involved in nanotubes and nanowires formation under the condition of sonication. Moreover, this approach is suitable to the anisotropic single crystals synthesis of other alkaline earth stannates and carbonates such as SrSn(OH)_6, BaSn(OH)_6, SrCO_3 and BaCO_3. It also gives a new demonstration of sonochemical effects on the crystallization and assembly of block building in the mesoscale.
引文
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