一维硅纳米材料及镍硅异质结纳米线的制备和表征
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摘要
一维纳米结构的硅材料是一类新型的半导体光电材料,由于它具有体硅材料稳定的半导体性,能和当代成熟的微电子技术相兼容,有望将来能够在纳米器件中得到广泛的应用。本文对硅的一维纳米结构材料进行了制备、表征及性能测试的研究。
首先,采用高压裂解法对小直径自主生长的硅纳米线合成进行了研究,实验中制备了直径小于10nm、硅晶核仅为5nm左右小尺寸硅纳米线,受量子效应的影响,样品拉曼特征峰发生了明显的红移,这种小直径纳米线极具研究价值,因为它更能反映纳米线所特有的性能。在高压裂解条件下,加入少量去离子水并在保温过程中释放少量的保护气体,首创性地成功制备了自主生长的硅纳米针状结构。
其次,采用热蒸发法研究了超长硅纳米线的制备,实验中制备的硅纳米线长度可达150μm,这种超长的硅纳米线在纳米电子器件应用中更具有优势,能够有效提高器件的集成度。文中还对硅氧化合物的半空心结构以及金刚石结构单晶硅纳米管的合成进行了研究。硅纳米管的成功制备是继模板法和水热发之后,又一重大实验突破。
硅纳米线在合成过程中是团聚在一起的,并且还伴随着大量的纳米颗粒生成,本文中采用十二烷基硫酸钠、乳化剂OP、二甲基甲酰胺等溶剂为表面分散剂在超声震荡条件下实现了对团聚纳米线的分散,结合离心技术,在不同的离心转速下实现了硅纳米线的分离.
最后,研究了硅纳米线表面镀镍工艺以及镍硅异质结纳米线的特性,即在除氧化层后的硅纳米线表面采用磁控溅射的方法对其镀镍,不同条件下的退火处理,分别得到了Ni/Ni_xSi_y/Si异质结纳米线和NiSi_2纳米线。通过对纳米线高分辨图像(HRTEM)的分析,研究了纳米线异质结的退火行为,应用FIB等实验设备对单根异质结纳米线进行操控和测试,研究了异质结纳米线的电学性能,为将来纳米线在互连及器件化应用中奠定了基础。
One dimension silicon nanomaterials are new kinds of optoelectronic materials. Since silicon nanomaterials are stabile with semiconductor property and compatible with modern silicon technology, they are promising in nanodevices. The synthesis, characterization and test of the one dimension silicon nanomaterials were studied in this paper.
At first, The self-assembled silicon nanowires ( SiNWs) with small diameter were studied. The SiNWs were synthesized by decomposition of silicon monoxide under high pressure. Their diameters were no more than 10nm and the silicon cores were about 5nm. Influenced by the quantum effect, Raman spectrum of the SiNWs was found to be downshifted. The research of the small size SiNWs was valuable for nanodevices. The silicon nanoneedles (SiNNs) were firstly reported by us with the similar growth method. SiNNs were synthesized with a small quantity of deionized water as the reaction medium. During the nanoneedles growth, some protection gas was released.
Secondly, synthesis of very long SiNWs was studied by thermal decomposition method. The SiNWs with the length more than 150μm were prepared in this work. They were promising for nanodevices, since the integrated level of device based on those nanowires would be effectively improved. The synthesis of half hollow silica nanomaterials and single crystal silicon nanotube (SiNTs) were also studied in this paper.
The as-grown SiNWs were agglomerated with lots of nanoparticles. By using ultrasonic agitation, the agglomerated SiNWs were dispersed in traditional organic solvents incorporated with various surfactants or surfactantmixtures, such as sodium dodecyl sulfate, emulsifier-OP, N,N-dimethylformamide. The SiNWs with different length and nanoparticles were separated by centrifugal machine.
In the end, the properties of nickel silicide heterostructure nanowires were studied. When the nickel implanted SiNWs were annealed at different temperature, Ni/Ni_xSi_y/Si core-shell heterostructure nanowires and NiSi_2 nanowires were formed. The formation and annealing behavior of the heterostructure nanowires were researched with the help of HRTEM images. Single heterostructure nanowire was manipulated in the FIB system and the I-V curve was tested in micro-current detection station. The research of the heterostructure nanowires was useful for the application of interconnection and nanodevices.
首先,采用高压裂解法对小直径自主生长的硅纳米线合成进行了研究,实验中制备了直径小于10nm、硅晶核仅为5nm左右小尺寸硅纳米线,受量子效应的影响,样品拉曼特征峰发生了明显的红移,这种小直径纳米线极具研究价值,因为它更能反映纳米线所特有的性能。在高压裂解条件下,加入少量去离子水并在保温过程中释放少量的保护气体,首创性地成功制备了自主生长的硅纳米针状结构。
其次,采用热蒸发法研究了超长硅纳米线的制备,实验中制备的硅纳米线长度可达150μm,这种超长的硅纳米线在纳米电子器件应用中更具有优势,能够有效提高器件的集成度。文中还对硅氧化合物的半空心结构以及金刚石结构单晶硅纳米管的合成进行了研究。硅纳米管的成功制备是继模板法和水热发之后,又一重大实验突破。
硅纳米线在合成过程中是团聚在一起的,并且还伴随着大量的纳米颗粒生成,本文中采用十二烷基硫酸钠、乳化剂OP、二甲基甲酰胺等溶剂为表面分散剂在超声震荡条件下实现了对团聚纳米线的分散,结合离心技术,在不同的离心转速下实现了硅纳米线的分离.
最后,研究了硅纳米线表面镀镍工艺以及镍硅异质结纳米线的特性,即在除氧化层后的硅纳米线表面采用磁控溅射的方法对其镀镍,不同条件下的退火处理,分别得到了Ni/Ni_xSi_y/Si异质结纳米线和NiSi_2纳米线。通过对纳米线高分辨图像(HRTEM)的分析,研究了纳米线异质结的退火行为,应用FIB等实验设备对单根异质结纳米线进行操控和测试,研究了异质结纳米线的电学性能,为将来纳米线在互连及器件化应用中奠定了基础。
One dimension silicon nanomaterials are new kinds of optoelectronic materials. Since silicon nanomaterials are stabile with semiconductor property and compatible with modern silicon technology, they are promising in nanodevices. The synthesis, characterization and test of the one dimension silicon nanomaterials were studied in this paper.
At first, The self-assembled silicon nanowires ( SiNWs) with small diameter were studied. The SiNWs were synthesized by decomposition of silicon monoxide under high pressure. Their diameters were no more than 10nm and the silicon cores were about 5nm. Influenced by the quantum effect, Raman spectrum of the SiNWs was found to be downshifted. The research of the small size SiNWs was valuable for nanodevices. The silicon nanoneedles (SiNNs) were firstly reported by us with the similar growth method. SiNNs were synthesized with a small quantity of deionized water as the reaction medium. During the nanoneedles growth, some protection gas was released.
Secondly, synthesis of very long SiNWs was studied by thermal decomposition method. The SiNWs with the length more than 150μm were prepared in this work. They were promising for nanodevices, since the integrated level of device based on those nanowires would be effectively improved. The synthesis of half hollow silica nanomaterials and single crystal silicon nanotube (SiNTs) were also studied in this paper.
The as-grown SiNWs were agglomerated with lots of nanoparticles. By using ultrasonic agitation, the agglomerated SiNWs were dispersed in traditional organic solvents incorporated with various surfactants or surfactantmixtures, such as sodium dodecyl sulfate, emulsifier-OP, N,N-dimethylformamide. The SiNWs with different length and nanoparticles were separated by centrifugal machine.
In the end, the properties of nickel silicide heterostructure nanowires were studied. When the nickel implanted SiNWs were annealed at different temperature, Ni/Ni_xSi_y/Si core-shell heterostructure nanowires and NiSi_2 nanowires were formed. The formation and annealing behavior of the heterostructure nanowires were researched with the help of HRTEM images. Single heterostructure nanowire was manipulated in the FIB system and the I-V curve was tested in micro-current detection station. The research of the heterostructure nanowires was useful for the application of interconnection and nanodevices.
引文
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