硅纳米洞/线的制备及应用于SERS基底的研究
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摘要
一维硅纳米材料由于其进入纳米尺度后具有了纳米材料的独特效应,并且表现出好的热、光、电学等优异特性,它所具有的独特的半导体性质使其成为微纳电子器件潜在材料之一,受到学术界越来越多的关注。
本论文采用金属辅助化学刻蚀法制备硅纳米孔洞和硅纳米线,并以硅纳米线为衬底制备了金属以及金属复合结构／硅纳米线阵列,并探究了其对R6G的SERS效应。本论文的主要研究结果如下：
一、硅纳米孔洞的制备及工艺参数的影响。探究了镀银时间和硝酸银浓度,以及真空退火对银纳米颗粒的影响；银颗粒的形貌和与刻蚀后的硅纳米孔洞的关系；重力、离心力都对刻蚀方向没有影响；H202浓度的增大和离心力都可分别加速刻蚀反应速度；在小体积状态下,刻蚀速率会随着刻蚀液体积的增加而增加,并且当刻蚀液的体积达到10m1后,刻蚀结构由纳米孔洞变成了“孔+线”纳米结构。
二、硅纳米线的制备及工艺参数的影响。通过改变硅片的电阻率,刻蚀时间以及氢氟酸浓度得出了最优化的制备参数：镀银溶液为4.6Mol/L的HF和0.01Mol/L的AgNO3混合液；镀银时间为1.2min,刻蚀溶液为10%.15%HF和1%H2O2混合溶液,温度70℃,刻蚀时间为40min；发现硅片的电阻率、刻蚀时间、HF浓度分别与硅纳米线的长度成正相关。
三、硅纳米线阵列结构和金属以及金属复合结构的复合材料的SERS效应。研究了金属以及金属复合结构／硅纳米线阵列(Ag/SiNWs、Au/SiNWs、 Ag-Au/SiNWs)作为活性基底对R6G的SERS效应,发现SiNWs对R6G没有SERS效应或者效应很弱；而SiNWs上附着的银或金纳米颗粒或者Ag-Au核壳结构能显著地提高拉曼信号,在他们各自的最佳状态下Ag-Au/SiNWs的SERS信号最强,Ag/SiNWs的SERS信号次之,Au/SiNWs的SERS信号最差。
One-dimensional silicon nanometre materials have received intensive interests because of the unique effect of nanometer materials after its entering nanoscale and exhibiting excellent properties, such as thermal, optical and electrical properties, their unique properties of semiconductor that make them one of the potential materials for micro-nano electronic devices.
This thesis mainly prepared silicon nanoholes and silicon nanowires by metal assisted chemical etching method, and metal or metal composite structure/silicon nanowire arrays by using silicon nanowires as substrate, and we also explored their SERS effect for R6G. The main research results are as follows:
First, the preparation of silicon nanoholes and the influence of process parameters. The effects of the silver plating time, the concentration of silver nitrate and vacuum annealing on morphologies of the silver nanoparticles, and the relationship with the morphology of silver nanoparticles and the etched silicon nanoholes are discussed. There is no effect on etching direction by gravity and centrifugal force; the etching reaction can be accelerated by the increase of H2O2concentration and centrifugal force respectively. In the condition of small volume, etching rate will be increased with the increase of etching fluid volume, and after the volume of the etching solution reaching10ml, the pores turn into the nanostructure composed of nanowires and nanopores.
Second, the preparation of silicon nanowires and the influence of process parameters. The optimal parameters of preparing silicon nanowires was obtained by changing the resistivity of silicon wafer, etching time and concentration of hydrofluoric acid:silver plating solution is the mixture solution of4.6Mol/L HF and0.01Mol/L AgNO3; the time of silver plating is1-2min, the etching solution is the mixed solution of10%-15%HF and1%H2O2, the etching temperature is70℃, the etching time is40min. The positive relationship between the resistivity of silicon, etching time, HF concentration and the length of the nanowires is also found respectively.
Third, the SERS effect of the composite material between silicon nanowire array structure and the structure of the metal or metal composite material. Their (Ag/SiNWs, Au/SiNWs, Ag-Au/SiNWs) SERS effects for R6G were studied, the SERS effect of the SiNWs may be very weak and is not found; the SERS signal can be significantly enhanced by the Ag, Au or Ag-Au core-shell structure adhering to the SiNWs in their own best condition. The SERS signal of Ag-Au/SiNWs is the strongest, the SERS signal of Ag/SiNWs takes second place, the SERS signal of Au/SiNWs is the worst.
本论文采用金属辅助化学刻蚀法制备硅纳米孔洞和硅纳米线,并以硅纳米线为衬底制备了金属以及金属复合结构／硅纳米线阵列,并探究了其对R6G的SERS效应。本论文的主要研究结果如下：
一、硅纳米孔洞的制备及工艺参数的影响。探究了镀银时间和硝酸银浓度,以及真空退火对银纳米颗粒的影响；银颗粒的形貌和与刻蚀后的硅纳米孔洞的关系；重力、离心力都对刻蚀方向没有影响；H202浓度的增大和离心力都可分别加速刻蚀反应速度；在小体积状态下,刻蚀速率会随着刻蚀液体积的增加而增加,并且当刻蚀液的体积达到10m1后,刻蚀结构由纳米孔洞变成了“孔+线”纳米结构。
二、硅纳米线的制备及工艺参数的影响。通过改变硅片的电阻率,刻蚀时间以及氢氟酸浓度得出了最优化的制备参数：镀银溶液为4.6Mol/L的HF和0.01Mol/L的AgNO3混合液；镀银时间为1.2min,刻蚀溶液为10%.15%HF和1%H2O2混合溶液,温度70℃,刻蚀时间为40min；发现硅片的电阻率、刻蚀时间、HF浓度分别与硅纳米线的长度成正相关。
三、硅纳米线阵列结构和金属以及金属复合结构的复合材料的SERS效应。研究了金属以及金属复合结构／硅纳米线阵列(Ag/SiNWs、Au/SiNWs、 Ag-Au/SiNWs)作为活性基底对R6G的SERS效应,发现SiNWs对R6G没有SERS效应或者效应很弱；而SiNWs上附着的银或金纳米颗粒或者Ag-Au核壳结构能显著地提高拉曼信号,在他们各自的最佳状态下Ag-Au/SiNWs的SERS信号最强,Ag/SiNWs的SERS信号次之,Au/SiNWs的SERS信号最差。
One-dimensional silicon nanometre materials have received intensive interests because of the unique effect of nanometer materials after its entering nanoscale and exhibiting excellent properties, such as thermal, optical and electrical properties, their unique properties of semiconductor that make them one of the potential materials for micro-nano electronic devices.
This thesis mainly prepared silicon nanoholes and silicon nanowires by metal assisted chemical etching method, and metal or metal composite structure/silicon nanowire arrays by using silicon nanowires as substrate, and we also explored their SERS effect for R6G. The main research results are as follows:
First, the preparation of silicon nanoholes and the influence of process parameters. The effects of the silver plating time, the concentration of silver nitrate and vacuum annealing on morphologies of the silver nanoparticles, and the relationship with the morphology of silver nanoparticles and the etched silicon nanoholes are discussed. There is no effect on etching direction by gravity and centrifugal force; the etching reaction can be accelerated by the increase of H2O2concentration and centrifugal force respectively. In the condition of small volume, etching rate will be increased with the increase of etching fluid volume, and after the volume of the etching solution reaching10ml, the pores turn into the nanostructure composed of nanowires and nanopores.
Second, the preparation of silicon nanowires and the influence of process parameters. The optimal parameters of preparing silicon nanowires was obtained by changing the resistivity of silicon wafer, etching time and concentration of hydrofluoric acid:silver plating solution is the mixture solution of4.6Mol/L HF and0.01Mol/L AgNO3; the time of silver plating is1-2min, the etching solution is the mixed solution of10%-15%HF and1%H2O2, the etching temperature is70℃, the etching time is40min. The positive relationship between the resistivity of silicon, etching time, HF concentration and the length of the nanowires is also found respectively.
Third, the SERS effect of the composite material between silicon nanowire array structure and the structure of the metal or metal composite material. Their (Ag/SiNWs, Au/SiNWs, Ag-Au/SiNWs) SERS effects for R6G were studied, the SERS effect of the SiNWs may be very weak and is not found; the SERS signal can be significantly enhanced by the Ag, Au or Ag-Au core-shell structure adhering to the SiNWs in their own best condition. The SERS signal of Ag-Au/SiNWs is the strongest, the SERS signal of Ag/SiNWs takes second place, the SERS signal of Au/SiNWs is the worst.
引文
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