一维硅基纳米材料的水热制备与表征
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摘要
由于与现有硅技术有良好的兼容性,一维硅基纳米材料有潜力成为硅纳米器件的基材,硅纳米管作为重要的硅基纳米材料之一,引起了人们极大的研究兴趣。由于硅为sp3杂化,易形成实心结构,故在实验上难以合成。因此,硅纳米管的研究在国际上都尚处于起步阶段。另外,硅纳米线、碳化硅纳米管/棒等一维硅基纳米材料由于独特的结构和优异性能,也成为了研究热点之一。本论文以一氧化硅和碳化硅为基础硅源,在自组生长硅纳米管、硅纳米线、碳化硅纳米管及碳化硅纳米棒的水热制备与表征、生长机理及光致发光PL性能等方面展开了较深入的研究,研究具有基础性和前瞻性,兼具重要的理论意义和潜在应用前景。
以一氧化硅为原料,未使用金属催化剂及模板,采用水热法于470℃、6.8MPa制备出了自组生长硅纳米管。研究表明硅纳米管的生长头部为闭合结构,由内部数纳米的中空结构,中部为壁厚不大于5nm的晶体硅管壁结构以及厚度低于2nm的无定形二氧化硅外层所组成。采用5wt%的HF酸对自组生长硅纳米管的稳定性研究表明HF酸可以去除硅纳米管的氧化物外层,只剩下晶体硅纳米管,说明自组生长硅纳米管是一种稳定结构,因而使其应用成为可能。采用硅纳米管Si-H自组生长模型解释了硅纳米管的形成与生长,研究表明硅纳米管的稳定性与其生长过程密切相关。样品的Raman及IR结果进一步证明所得纳米管是一种晶体硅纳米管,外层主要为二氧化硅。PL结果表明样品在436nm处具有较强的PL性能,发射范围400-500nm,发射峰不对称,并出现了不均匀宽化。
对不同水热条件一维硅纳米材料的系统研究表明470℃、6.8-8MPa是目前制备自组生长硅纳米管较合适的水热条件。470℃时,随着压力和保温时间的增加,硅纳米管的直径从小于20nm增加到了约100nm,压力增至9.5MPa以上时,所得一维硅纳米材料为实心结构。以硅及二氧化硅为硅源,所得样品只含有近圆形或不规则纳米颗粒,而以硅粉为硅源可制备出长数微米、直径约100nm的硅纳米链。
水热条件下在硅片上可沉积出中间为硅核、外层包覆无定形二氧化硅的核壳结构硅纳米线,直径数百纳米、长度大于10μm。硅纳米线的Raman结果表明在519cm-1处有一Raman特征峰,并出现了不对称宽化,PL测试表明在754.1nm处有强烈的PL特征峰。采用氧化物辅助生长机理解释了沉积于硅片上硅纳米线的形成与生长,进一步研究表明470℃、9-14MPa及保温48h是目前较优的工艺参数。以硅及二氧化硅为硅源的研究表明只能在硅片上沉积出不同尺寸的球状及不规则颗粒,说明一氧化硅是水热条件下在硅片上沉积硅纳米线的较合适的硅源。
以碳化硅与二氧化硅为原料,在470℃、8MPa时制备出了直径约10nm、长
One-dimensional silicon-based nanoscale materials have the potential to become the important basic material in silicon nanoscale devices owing to the excellent compatibility with the present silicon technology. Silicon nanotube (SiNT) is a kind of important silicon-based nanoscale materials and has attracted great interest. Solid silicon nanowires (SiNWs) can form easily due to sp3 hybridization in silicon. So SiNTs are difficult to synthesize in the experiments. Therefore, the research on SiNTs is still in primary stage in the world. In addition, one-dimensional silicon-based nanoscale materials such as SiNWs, silicon carbide nanotubes (SiCNTs) and nanorods (SiCNRs) are also the present research focuses because of their inimitable structures and outstanding properties. Silicon monoxide and silicon carbide are the basic silicon starting materials. The hydrothermal preparation and characterization, growth mechanism and photoluminescence (PL) properties of the self-assembled SiNTs, SiNWs, SiCNTs and SiCNRs have been studied in detail in the paper. The research is fundamental and pioneering, and is of great significance on theory and application potential.
Self-assembled SiNTs have been prepared from silicon monoxide by the hydrothermal method with the temperature of 470℃, pressure of 6.8MPa without metallic-catalysts and templates. The research results demonstrate that the SiNTs have close caps at the tips. The structures of SiNTs are hollow inner pores with a size of several nanometers in the middle, crystalline silicon wall layers with the thickness of less than 5nm and amorphous silica outer layers with the thickness of less than 2nm. The research result on the stability of self-asembled SiNTs with 5wt% HF acid shows that silicon oxide outer layers can be removed and pure crystalline SiNTs survive after etching the SiNTs for enough time which implys that the self-assembled SiNTs are stable. Therefore, it’s possible to research the application of self-assembled SiNTs. A hypothetical SiNT Si-H self-assembled growth model is proposed to explain the formation and growth process of the SiNTs and the stability of the SiNTs is closely relative to the growth process. The Raman and Infra-red (IR) spectra of the SiNT sample further show that the obtained nanotubes are a kind of crystalline SiNTs with silica outer layers. PL result of the SiNT sample demonstrates that PL peak center at 436nm is strong and asymmetrically broad. And the range of PL emission peak is
以一氧化硅为原料,未使用金属催化剂及模板,采用水热法于470℃、6.8MPa制备出了自组生长硅纳米管。研究表明硅纳米管的生长头部为闭合结构,由内部数纳米的中空结构,中部为壁厚不大于5nm的晶体硅管壁结构以及厚度低于2nm的无定形二氧化硅外层所组成。采用5wt%的HF酸对自组生长硅纳米管的稳定性研究表明HF酸可以去除硅纳米管的氧化物外层,只剩下晶体硅纳米管,说明自组生长硅纳米管是一种稳定结构,因而使其应用成为可能。采用硅纳米管Si-H自组生长模型解释了硅纳米管的形成与生长,研究表明硅纳米管的稳定性与其生长过程密切相关。样品的Raman及IR结果进一步证明所得纳米管是一种晶体硅纳米管,外层主要为二氧化硅。PL结果表明样品在436nm处具有较强的PL性能,发射范围400-500nm,发射峰不对称,并出现了不均匀宽化。
对不同水热条件一维硅纳米材料的系统研究表明470℃、6.8-8MPa是目前制备自组生长硅纳米管较合适的水热条件。470℃时,随着压力和保温时间的增加,硅纳米管的直径从小于20nm增加到了约100nm,压力增至9.5MPa以上时,所得一维硅纳米材料为实心结构。以硅及二氧化硅为硅源,所得样品只含有近圆形或不规则纳米颗粒,而以硅粉为硅源可制备出长数微米、直径约100nm的硅纳米链。
水热条件下在硅片上可沉积出中间为硅核、外层包覆无定形二氧化硅的核壳结构硅纳米线,直径数百纳米、长度大于10μm。硅纳米线的Raman结果表明在519cm-1处有一Raman特征峰,并出现了不对称宽化,PL测试表明在754.1nm处有强烈的PL特征峰。采用氧化物辅助生长机理解释了沉积于硅片上硅纳米线的形成与生长,进一步研究表明470℃、9-14MPa及保温48h是目前较优的工艺参数。以硅及二氧化硅为硅源的研究表明只能在硅片上沉积出不同尺寸的球状及不规则颗粒,说明一氧化硅是水热条件下在硅片上沉积硅纳米线的较合适的硅源。
以碳化硅与二氧化硅为原料,在470℃、8MPa时制备出了直径约10nm、长
One-dimensional silicon-based nanoscale materials have the potential to become the important basic material in silicon nanoscale devices owing to the excellent compatibility with the present silicon technology. Silicon nanotube (SiNT) is a kind of important silicon-based nanoscale materials and has attracted great interest. Solid silicon nanowires (SiNWs) can form easily due to sp3 hybridization in silicon. So SiNTs are difficult to synthesize in the experiments. Therefore, the research on SiNTs is still in primary stage in the world. In addition, one-dimensional silicon-based nanoscale materials such as SiNWs, silicon carbide nanotubes (SiCNTs) and nanorods (SiCNRs) are also the present research focuses because of their inimitable structures and outstanding properties. Silicon monoxide and silicon carbide are the basic silicon starting materials. The hydrothermal preparation and characterization, growth mechanism and photoluminescence (PL) properties of the self-assembled SiNTs, SiNWs, SiCNTs and SiCNRs have been studied in detail in the paper. The research is fundamental and pioneering, and is of great significance on theory and application potential.
Self-assembled SiNTs have been prepared from silicon monoxide by the hydrothermal method with the temperature of 470℃, pressure of 6.8MPa without metallic-catalysts and templates. The research results demonstrate that the SiNTs have close caps at the tips. The structures of SiNTs are hollow inner pores with a size of several nanometers in the middle, crystalline silicon wall layers with the thickness of less than 5nm and amorphous silica outer layers with the thickness of less than 2nm. The research result on the stability of self-asembled SiNTs with 5wt% HF acid shows that silicon oxide outer layers can be removed and pure crystalline SiNTs survive after etching the SiNTs for enough time which implys that the self-assembled SiNTs are stable. Therefore, it’s possible to research the application of self-assembled SiNTs. A hypothetical SiNT Si-H self-assembled growth model is proposed to explain the formation and growth process of the SiNTs and the stability of the SiNTs is closely relative to the growth process. The Raman and Infra-red (IR) spectra of the SiNT sample further show that the obtained nanotubes are a kind of crystalline SiNTs with silica outer layers. PL result of the SiNT sample demonstrates that PL peak center at 436nm is strong and asymmetrically broad. And the range of PL emission peak is
引文
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