ZnE（E=S,Se,Te）和Mn掺杂AIN纳米结构的制备及表征
摘要
宽带隙半导体纳米材料由于其特殊的理化性质和重要的应用前景引起广泛的关注,其可控制备一直是纳米科学研究的热点。ZnE (E=S,Se,Te)作为重要的宽禁带、直接带隙的II-VI族半导体,具有优异的光电化学性能,在激光器和太阳能电池方面有很多潜在的应用价值。稀磁半导体兼备磁性和半导体特性,在光、电、磁功能集成等新型器件方面具有重要的应用。宽带隙半导体AlN具有良好的光学性质和广泛的潜在用途,基于A1N纳米结构的稀磁半导体具有相当重要的研究意义。
本论文的主要内容归纳如下:
1.以ZnO为锌源,Na_2S_2O_3·5H_2O为硫源,通过乙醇胺(EA)辅助的溶剂热法一步合成了直径约为6 nm的纤锌矿型ZnS细纳米棒。合成的ZnS为单晶,沿[001]方向择优生长。根据实验结果,提出了ZnS纳米棒可能的形成机制:EA辅助形核与一维生长。
2.以乙酸锌为锌源,Na_2EO_3 (E=Se,Te)或E粉为E源,采用溶剂热技术在乙醇胺(EA)体系中一步合成ZnE纳米材料。测试结果表明以Na_2EO_3为E源,产物为立方相闪锌矿结构的ZnE纳米颗粒;以E粉为源,产物为ZnE纳米片,厚度约60 nm。分析表明合适配位能力溶剂EA对ZnE纳米结构的形成至关重要,E源的选取则对ZnE的物相和形貌有很大影响。
3.采用无催化化学气相沉积法,以高纯Al粉、无水AlCl_3、高纯Mn粉、MnCl_2和NH3气为源,在陶瓷和硅衬底上得到Mn掺杂AlN单晶纳米棒、纳米带和超长纳米线等。EDS和XPS测试证实了Mn成功掺入AlN纳米结构中。采用超导量子磁通计(SQUID)在5 K和300 K都观察到Mn掺杂AlN单晶纳米棒的铁磁有序。
4.采用无催化化学气相沉积法,以无水AlCl_3、无水MnCl_2和NH_3气为源,在硅片和石墨片衬底上成功制备了Mn掺杂AlN纳米棒阵列和纳米晶薄膜。分析结果显示,合成的纳米棒阵列和纳米晶薄膜为纤锌矿结构的AlN,沿[001]方向生长。采用SQUID纳米棒阵列的磁性测试显示其具有室温铁磁性。
Wide band gap semiconductor nanomaterials have drawn universal attention due to their unique physicochemical properties and important applications, while controlled synthesis of nanomaterials is still the research hotspot in nanoscience. As wide and direct band gap II-VI semiconductor, ZnE (E=S, Se, Te) materials show great potential applications in laser and solar cell with the excellent optoelectronic and chemical performance. Diluted magnetic semiconductors (DMSs), combining the properties of both magnetic materials and semiconductors, have many potential applications for optical, electronic and magnetic devices. With a series of excellent optical properties and wide potential use, AlN nanostructure-based DMSs have important value in scientific research.
The main work completed in this thesis can be summarized as following:
1. This paper describes a novel ethanol amine (EA)-directed solvothermal approach for one-step synthesis of wurtzite-structured ZnS thin nanorods with mean diameters of about 6 nm adopting ZnO and Na_2S_2O_3·5H_2O as starting reagents. The as-prepared ZnS nanorods are well-crystallized single crystals with growth direction along [001] of wurtzite. The possible growth mechanism of the as prepared ZnS nanorods involving EA-mediated nucleation and one-dimensional (1D) growth has been discussed referring to the experimental results.
2. Sphalerite or wurtzite ZnE (E=Se, Te) nanomaterials were synthesized by one-step solvothermal technique by using EA as solvent, zinc acetate as zinc source and Na_2EO_3 or E powder as E source. The test results show that sphalerite ZnE nanoparticles were obtained by adopting Na_2EO_3 as E source, and ZnE nanoplates with thickness of 60 nm by employing E powder as E source. Analysis indicates that EA solvent with appropriate coordination ability has played an important role in the formation of ZnE nanostructures, while the structure and morphology of ZnE nanomaterials are determined by the choice of E source.
3. Mn-doped AlN single-crystalline nanorods, nanobelts and ultralong nanowires were grown on alumina and silicon substrates by doping Mn using a chemical catalyst-free vapor deposition method employing Al powder, anhydrous AlCl3, Mn powder, MnCl2 and NH3 as sources. Energy dispersive spectroscopy (EDS) and X-ray photoemission spectroscopy (XPS) demonstrate that Mn is successfully doped into the nanostructures. Ferromagnetic ordering of the AlN:Mn nanorods was observed both at 5 K and 300 K by a superconducting quantum interference device magnetometer (SQUID).
4. Mn-doped AlN nanorod arrays and nanocrystalline films were synthesized on silicon plates and graphite sheets by adopting anhydrous AlCl_3, anhydrous MnCl_2 and NH3 as sources via a catalyst-free chemical vapor deposition method. Analysis shows that the as-prepared nanorods and nanocrystalline grow on the substrates with the alignment along [001] orientation of hexagonal AlN and ferromagnetic ordering of the Mn-doped AlN nanorod arrays was observed at 300 K by a SQUID.
本论文的主要内容归纳如下:
1.以ZnO为锌源,Na_2S_2O_3·5H_2O为硫源,通过乙醇胺(EA)辅助的溶剂热法一步合成了直径约为6 nm的纤锌矿型ZnS细纳米棒。合成的ZnS为单晶,沿[001]方向择优生长。根据实验结果,提出了ZnS纳米棒可能的形成机制:EA辅助形核与一维生长。
2.以乙酸锌为锌源,Na_2EO_3 (E=Se,Te)或E粉为E源,采用溶剂热技术在乙醇胺(EA)体系中一步合成ZnE纳米材料。测试结果表明以Na_2EO_3为E源,产物为立方相闪锌矿结构的ZnE纳米颗粒;以E粉为源,产物为ZnE纳米片,厚度约60 nm。分析表明合适配位能力溶剂EA对ZnE纳米结构的形成至关重要,E源的选取则对ZnE的物相和形貌有很大影响。
3.采用无催化化学气相沉积法,以高纯Al粉、无水AlCl_3、高纯Mn粉、MnCl_2和NH3气为源,在陶瓷和硅衬底上得到Mn掺杂AlN单晶纳米棒、纳米带和超长纳米线等。EDS和XPS测试证实了Mn成功掺入AlN纳米结构中。采用超导量子磁通计(SQUID)在5 K和300 K都观察到Mn掺杂AlN单晶纳米棒的铁磁有序。
4.采用无催化化学气相沉积法,以无水AlCl_3、无水MnCl_2和NH_3气为源,在硅片和石墨片衬底上成功制备了Mn掺杂AlN纳米棒阵列和纳米晶薄膜。分析结果显示,合成的纳米棒阵列和纳米晶薄膜为纤锌矿结构的AlN,沿[001]方向生长。采用SQUID纳米棒阵列的磁性测试显示其具有室温铁磁性。
Wide band gap semiconductor nanomaterials have drawn universal attention due to their unique physicochemical properties and important applications, while controlled synthesis of nanomaterials is still the research hotspot in nanoscience. As wide and direct band gap II-VI semiconductor, ZnE (E=S, Se, Te) materials show great potential applications in laser and solar cell with the excellent optoelectronic and chemical performance. Diluted magnetic semiconductors (DMSs), combining the properties of both magnetic materials and semiconductors, have many potential applications for optical, electronic and magnetic devices. With a series of excellent optical properties and wide potential use, AlN nanostructure-based DMSs have important value in scientific research.
The main work completed in this thesis can be summarized as following:
1. This paper describes a novel ethanol amine (EA)-directed solvothermal approach for one-step synthesis of wurtzite-structured ZnS thin nanorods with mean diameters of about 6 nm adopting ZnO and Na_2S_2O_3·5H_2O as starting reagents. The as-prepared ZnS nanorods are well-crystallized single crystals with growth direction along [001] of wurtzite. The possible growth mechanism of the as prepared ZnS nanorods involving EA-mediated nucleation and one-dimensional (1D) growth has been discussed referring to the experimental results.
2. Sphalerite or wurtzite ZnE (E=Se, Te) nanomaterials were synthesized by one-step solvothermal technique by using EA as solvent, zinc acetate as zinc source and Na_2EO_3 or E powder as E source. The test results show that sphalerite ZnE nanoparticles were obtained by adopting Na_2EO_3 as E source, and ZnE nanoplates with thickness of 60 nm by employing E powder as E source. Analysis indicates that EA solvent with appropriate coordination ability has played an important role in the formation of ZnE nanostructures, while the structure and morphology of ZnE nanomaterials are determined by the choice of E source.
3. Mn-doped AlN single-crystalline nanorods, nanobelts and ultralong nanowires were grown on alumina and silicon substrates by doping Mn using a chemical catalyst-free vapor deposition method employing Al powder, anhydrous AlCl3, Mn powder, MnCl2 and NH3 as sources. Energy dispersive spectroscopy (EDS) and X-ray photoemission spectroscopy (XPS) demonstrate that Mn is successfully doped into the nanostructures. Ferromagnetic ordering of the AlN:Mn nanorods was observed both at 5 K and 300 K by a superconducting quantum interference device magnetometer (SQUID).
4. Mn-doped AlN nanorod arrays and nanocrystalline films were synthesized on silicon plates and graphite sheets by adopting anhydrous AlCl_3, anhydrous MnCl_2 and NH3 as sources via a catalyst-free chemical vapor deposition method. Analysis shows that the as-prepared nanorods and nanocrystalline grow on the substrates with the alignment along [001] orientation of hexagonal AlN and ferromagnetic ordering of the Mn-doped AlN nanorod arrays was observed at 300 K by a SQUID.
引文
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