方形硅纳米孔洞的制备及应用研究
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摘要
硅纳米材料特别是一维纳米硅材料由于其在尺寸上的特点,表现出与体材料不同的量子限域效应、小尺寸效应、宏观量子隧道效应和表面效应等特点,并表现出奇特的力学、光学、电学、磁学、热学和化学等性能,已经成为国际半导体材料和纳米领域研究的热点。
集成电路及光伏器件等基本上都是以硅作为衬底的。因此把硅纳米线、硅纳米孔洞、多孔硅及硅纳米管等一维纳米结构与硅片结合起来,将对硅纳米材料的广泛应用产生深远的影响。
本文在不采用任何模板和特别技术下,采用金属辅助化学腐蚀法,同时结合硅的各向异性腐蚀制备出了大面积具有同一尺寸的方形硅纳米孔洞结构,对影响方形硅纳米孔洞生长的因素进行了初步探索。
由于金属银纳米颗粒对硅的腐蚀有重要的辅助催化作用,且分散的金属银纳米颗粒更有利于硅纳米孔洞的生长,所以重点进行了银纳米颗粒形貌的控制研究。通过改变银膜厚度、升温和降温速度、保温时间和保护气氛等退火条件,研究了不同的工艺参数对银纳米颗粒形成的影响,最后得到分散性较好的银纳米颗粒的合成条件为：银膜厚度为8～10nm,以氩气为保护气体,升温速度为100℃/min,降温速度为20℃/min,在退火温度为300℃下对样品进行退火。
通过改变刻蚀溶液的浓度、反应温度、反应时间等刻蚀条件,研究了不同工艺参数对方形硅纳米孔洞形成的影响。结合金属催化机制和硅的各向异性腐蚀机理解释了方形硅纳米孔洞形成原因。获得了制备方形硅纳米孔洞结构的优化条件：氢氟酸的浓度为2～5Mol/L,双氧水的浓度为0.3～0.4Mol/L,反应温度为50-55℃。
进行了方形硅纳米孔洞的应用研究。用拉曼光谱仪探测吸附有腺嘌呤分子的方形硅纳米孔洞／银基底的拉曼谱,结果显示方形硅纳米孔洞／银基底具有良好的灵敏性。利用分光光度计测量了具有方形纳米孔结构的硅衬底的积分反射谱,结果显示出其具有优良的减反射性,在250-800nm波段的反射率低至2%。
Silicon nano-materials, especially one-dimensional silicon material because of its characteristics of size show quantum confinement effect, the small size effect, macroscopic quantum tunneling effect and surface effect and other characteristics different with bulk materials, and showed unusual mechanical, optical, electrical, magnetic, thermal and chemical properties, has become researching focus of international semiconductor materials and nano-materials.
Basically, such as integrated circuits and photovoltaic devices are based on silicon substrate, so silicon nanowires, silicon nanoholes, porous silicon and silicon nanotubes and other one-dimensional silicon nanostructures would be connected with bulk silicon substrate, which is important for extensive use of silicon nanomaterials.
This paper does not use any template and special technical, large-area and uniform size square silicon nanoholes are produced by combining metal-assisted catalyzed etching with anisotropic etching of silicon. The factors affected the growth of square silicon nanoholes were explored.
Because Ag nanoparticles has an important auxiliary catalytics on the corrosion of silicon, and dispersed silver nanoparticles is more conducive to the growth of silicon nanoholes, so we concentrated on controlling of the morphology of silver nanoparticles. We changed annealing conditions such as the silver film thickness, heating rate and cooling rate, holding time and protective atmosphere, and studied the influence of different process parameters on the formation of silver nanoparticles. The optimum conditions of synthesis for meeting requirements of Ag nanoparticles is:The thickness of Ag film is 8～10nm, Argon as a shielding gas, heating rate is 100℃/ min, cooling rate is 20℃/min, the annealing temperature is 300℃.
We changed etching conditions such as the etching solution concentration, reaction temperature and reaction time, and discussed the influence of different process parameters on the formation of square silicon nanoholes. We explain the the formation of square silicon nanoholes with metal catalytic mechanism and the mechanism of anisotropic etching of silicon. After continuous exploration the best conditions of fabricating square silicon nanoholes is:The concentration of hydrofluoric acid is controlled in 2～5 Mol/L, concentration of hydrogen peroxide is 0.3～0.4 Mol/L, reaction temperature is 50～55℃.
The application of square silicon nanoholes is studied. We fabricated square silicon nanoholes/Ag as SERS substrate by immersion plating siliveron square silicon nanoholes. The enhanced Raman spectrum of adenine molecules adsorbed on square silicon nanoholes/Ag substrate is detected by Raman spectroscopy. The results showed that silver/square holes in nano-silicon substrate has a good sensitivity and has potential applications in the field of molecular detection; The integral reflection spectrum of square silicon nanoholes is measured by spectrophotometer. The results show that it has good reflection of the reduction, the low reflectance is about 2% in 250-800nm.
集成电路及光伏器件等基本上都是以硅作为衬底的。因此把硅纳米线、硅纳米孔洞、多孔硅及硅纳米管等一维纳米结构与硅片结合起来,将对硅纳米材料的广泛应用产生深远的影响。
本文在不采用任何模板和特别技术下,采用金属辅助化学腐蚀法,同时结合硅的各向异性腐蚀制备出了大面积具有同一尺寸的方形硅纳米孔洞结构,对影响方形硅纳米孔洞生长的因素进行了初步探索。
由于金属银纳米颗粒对硅的腐蚀有重要的辅助催化作用,且分散的金属银纳米颗粒更有利于硅纳米孔洞的生长,所以重点进行了银纳米颗粒形貌的控制研究。通过改变银膜厚度、升温和降温速度、保温时间和保护气氛等退火条件,研究了不同的工艺参数对银纳米颗粒形成的影响,最后得到分散性较好的银纳米颗粒的合成条件为：银膜厚度为8～10nm,以氩气为保护气体,升温速度为100℃/min,降温速度为20℃/min,在退火温度为300℃下对样品进行退火。
通过改变刻蚀溶液的浓度、反应温度、反应时间等刻蚀条件,研究了不同工艺参数对方形硅纳米孔洞形成的影响。结合金属催化机制和硅的各向异性腐蚀机理解释了方形硅纳米孔洞形成原因。获得了制备方形硅纳米孔洞结构的优化条件：氢氟酸的浓度为2～5Mol/L,双氧水的浓度为0.3～0.4Mol/L,反应温度为50-55℃。
进行了方形硅纳米孔洞的应用研究。用拉曼光谱仪探测吸附有腺嘌呤分子的方形硅纳米孔洞／银基底的拉曼谱,结果显示方形硅纳米孔洞／银基底具有良好的灵敏性。利用分光光度计测量了具有方形纳米孔结构的硅衬底的积分反射谱,结果显示出其具有优良的减反射性,在250-800nm波段的反射率低至2%。
Silicon nano-materials, especially one-dimensional silicon material because of its characteristics of size show quantum confinement effect, the small size effect, macroscopic quantum tunneling effect and surface effect and other characteristics different with bulk materials, and showed unusual mechanical, optical, electrical, magnetic, thermal and chemical properties, has become researching focus of international semiconductor materials and nano-materials.
Basically, such as integrated circuits and photovoltaic devices are based on silicon substrate, so silicon nanowires, silicon nanoholes, porous silicon and silicon nanotubes and other one-dimensional silicon nanostructures would be connected with bulk silicon substrate, which is important for extensive use of silicon nanomaterials.
This paper does not use any template and special technical, large-area and uniform size square silicon nanoholes are produced by combining metal-assisted catalyzed etching with anisotropic etching of silicon. The factors affected the growth of square silicon nanoholes were explored.
Because Ag nanoparticles has an important auxiliary catalytics on the corrosion of silicon, and dispersed silver nanoparticles is more conducive to the growth of silicon nanoholes, so we concentrated on controlling of the morphology of silver nanoparticles. We changed annealing conditions such as the silver film thickness, heating rate and cooling rate, holding time and protective atmosphere, and studied the influence of different process parameters on the formation of silver nanoparticles. The optimum conditions of synthesis for meeting requirements of Ag nanoparticles is:The thickness of Ag film is 8～10nm, Argon as a shielding gas, heating rate is 100℃/ min, cooling rate is 20℃/min, the annealing temperature is 300℃.
We changed etching conditions such as the etching solution concentration, reaction temperature and reaction time, and discussed the influence of different process parameters on the formation of square silicon nanoholes. We explain the the formation of square silicon nanoholes with metal catalytic mechanism and the mechanism of anisotropic etching of silicon. After continuous exploration the best conditions of fabricating square silicon nanoholes is:The concentration of hydrofluoric acid is controlled in 2～5 Mol/L, concentration of hydrogen peroxide is 0.3～0.4 Mol/L, reaction temperature is 50～55℃.
The application of square silicon nanoholes is studied. We fabricated square silicon nanoholes/Ag as SERS substrate by immersion plating siliveron square silicon nanoholes. The enhanced Raman spectrum of adenine molecules adsorbed on square silicon nanoholes/Ag substrate is detected by Raman spectroscopy. The results showed that silver/square holes in nano-silicon substrate has a good sensitivity and has potential applications in the field of molecular detection; The integral reflection spectrum of square silicon nanoholes is measured by spectrophotometer. The results show that it has good reflection of the reduction, the low reflectance is about 2% in 250-800nm.
引文
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