硫属化合物和氧化物纳米材料的化学液相合成与机理研究
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摘要
本论文以液相化学合成为基础,重点探索了用室温水相化学合成,水热以及溶剂热合成制备了CuS,NiTe_2,Cu_2O,CuO纳米材料。室温下采用水相合成方法可控制备CuS纳米管和纳米空心球:水热条件下制备具有正六边形形貌的NiTe_2单晶纳米片;采用乙二醇还原法合成Cu_2O纳米线阵列;在水热条件下经过氧化路径合成出CuO分级微米球结构。此外,对所制备的纳米材料进行了详细的形貌表征和结构研究,进而探讨不同反应条件对产物的相成分和形貌的影响。在此基础上,提出纳米材料相应的形成机理。主要内容归纳如下:
1.室温下,以CuCl_2,硫脲(Tu)和NaHCO_3作为反应物,通过调节Tu/CuCl_2的摩尔比选择性地合成了CuS纳米管和纳米空心球,其直径约为100-200nm,结构观察表明这些CuS纳米管和纳米空心球都是由大量尺寸约为5-10 nm的CuS小颗粒组成。对CuS形貌的影响因素进行了系统的探讨,并对CuS不同形貌的形成过程提出了两种可能的生长路径。当Tu/CuCl_2的摩尔比较低时会经过Tu-Cu(Ⅱ)配合物前驱物路径最终形成CuS纳米管,而摩尔比较高时会通过Tu-Cu(Ⅰ)前驱物路径从而生成CuS纳米空心球。紫外-吸收光谱表明CuS纳米空心球在481 nm处有一个比较宽的吸收峰,而CuS纳米管却没有这样的峰。室温发光光谱表明CuS纳米空心球在432 nm处有一个发射峰,而对于CuS纳米管却没有探测到发射峰。本实验体系的条件温和,操作方便。研究结果发表在J.Nanosci.Nanotechnol.(2007,7,4501)上。
2.采用水热路径大规模的合成出了单晶的NiTe_2纳米片。这些纳米片具有正六边形的形貌。纳米片的平均边长和厚度分别为350 nm和85 nm。实验结果表明EDTA起着络合剂的作用,在控制产物的相成分和形貌方面都起到了关键作用。该实验体系反应简单,条件温和,费用低廉,具有潜在工业应用价值,使得这种方法更富有意义和吸引力。此方法可以进一步延伸到其他碲化物纳米材料的制备。研究结果发表在J.Nanosci.Nanotechnol.(2009,9.2715)上。
3.设计了一种无外加模板、无表面活性剂的溶液路径,采用乙二醇(EG)还原Cu(CH_3COO)_2的方法,成功的合成出了有序的Cu_2O纳米线阵列。其整体形貌看起来象压缩饼干。Cu_2O纳米线的直径大约为30 nm。对Cu_2O相成分和形貌的影响因素进行了系统的观察。反应体系简单,操作方便。研究结果发表在Mater.Chem.Phys.(2009,114,213)上。
4.设计了表面活性剂聚乙二醇(PEG)辅助的水热合成路线,选择CuCl作为铜源,氨水作为碱性介质,合成了三维的CuO片-片-球分级结构,CuO球的直径大约为3μm,每个微米球都是由无数的二维纳米片通过层层重叠生长模式组成的,这些纳米片的厚度大约为40 nm。而每个纳米片又是由很多更小的二维纳米片以边对边的方式聚集的。对CuO形貌的影响因素进行了系统的观察,其中,PEG的浓度对形貌起着很关键的作用。另外,研究了CuO分级微米球的形成机理。
Based on the chemical solution-phase synthesis,the aim of this dissertation is to explore the synthesis of CuS,NiTe_2,Cu_2O,CuO nanomaterials by room temperature chemical solution route,solvothermal technique and hydrothermal method.A chemical solution route has been developed to selectively prepare covellite(CuS) nanotubes and hollow nanospheres at room temperature;Single-crystalline NiTe_2 nanoplates with the hexagonal shape have been synthesized on a large scale through a hydrothermal method.Well-aligned arrays of cuprous oxide(Cu_2O) nanowires have been synthesized by an ethylene glycol-reduced process;Three-dimensional(3 D) CuO hierarchical microspheres have been prepared via a simple hydrothermal route.The morphologies and structures of as-prepared nanomaterials are characterized in detail.A systematic investigation has been carried out to understand the factors influencing the phase composition and morphology,and their formation mechanisms are also briefly discussed.The main contents can be summarized as follows:
1.A chemical solution route has been developed to synthesize CuS nanostructures through the precitation reaction of CuCl_2·2H_2O,thiourea(Tu) and NaHCO_3 in distilled water at room temperature.By regulating the concentration of Tu,CuS nanotubes and hollow nanospheres with diameters of 100-200 nm have been selectively prepared.Structural characterizations indicate that both nanotubes and hollow spheres are composed of CuS nanoparticles with diameters of about 5-10 nm.A systematic investigation has been carried out to understand the factors influencing the CuS morphology.Two different routes are identified to explain the formation of the nanotubes and hollow nanospheres herein.It is concluded that low concentration of Tu is favorable to CuS nanotubes via the thiourea-copper(Ⅱ) complex precursor route,while high concentration is favourable to CuS hollow spherical structures via the thiourea-copper(Ⅰ) complex precursor route.UV-vis absorption spectra show the CuS product with hollow nanosphere morphology shows a wide absorption peak centered at about 481 nm,while the product with nanotube morphology shows no such peak.Room-temperature PL spectra of CuS hollow nanospheres reveal a peak at around 432 nm,while no such peak for CuS nanotubes.UV-vis absorption and room PL spectra display different morphology-related absorption phenomena for nanotubes and hollow nanospheres. The experimental conditions are mild,and the manipulations are convenient. These results were published in J.Nanosci.Nanotechnol.(2007,7,4501).
2.Single-crystalline NiTe_2 nanoplates have been synthesized on a large scale through a hydrothermal reaction of Ni(CH_3COO)_2 and YeO_2 at 210℃for 48 h.The NiTe_2 nanoplates have hexagonal shape.The average edge sizes and thicknesses of nanoplates are 350 nm and 85 nm,respectively.Here,Ethylenediaminetetraacetic acid(EDTA) is employed as a chelating agent.Furthermore,EDTA plays crucial roles in controlling phase composition and morphology of the resultant products. The simple process,mild conditon and cheap cost in this work make the present route attractive and significant.It has potential industrial application.This method may be extended to prepare other tellurides nanomaterials.This study was published in J.Nanosci.Nanotechnol.(2009,9,2715).
3.Well-aligned arrays of Cuprous oxide(Cu_2O) nanowires were synthesized through the reduction of Cu(CH_3COO)_2 by ethylene glycol(EG) without the assistance of externally introduced template and surfactant.The panorama of well-aligned arrays of Cu_2O nanowires looks like a biscuit.These Cu_2O nanowires are～30 nm in diameter.A systematic investigation has been carried out to understand the factors influencing the phase composition and Cu_2O morphologies.The experimental system is simple and the manipulation is convenient.This study was published in Mater.Chem.Phys.(2009,114,213).
4.A simple hydrothermal route was developed to synthesize CuO three-dimensional (3D) hierarchical microspheres using CuCl as the copper source and PEG as the morphology-directing agent in ammonia aqueous medium.The microspheres with average diameter of about 3μm were constructed from two-dimensional(2D) nanosheets with average thickness of about 40 nm via a layer-by-layer growth style and the nanosheets were composed of tiny nanoplates through orientation attachment.The quantity of PEG played crucial roles in the formation of CuO hierarchical structures and a systematic investigation was carried out to understand the factors influencing the CuO morphology.The possible growth mechanism was identified to explain the formation of CuO architectures herein.
1.室温下,以CuCl_2,硫脲(Tu)和NaHCO_3作为反应物,通过调节Tu/CuCl_2的摩尔比选择性地合成了CuS纳米管和纳米空心球,其直径约为100-200nm,结构观察表明这些CuS纳米管和纳米空心球都是由大量尺寸约为5-10 nm的CuS小颗粒组成。对CuS形貌的影响因素进行了系统的探讨,并对CuS不同形貌的形成过程提出了两种可能的生长路径。当Tu/CuCl_2的摩尔比较低时会经过Tu-Cu(Ⅱ)配合物前驱物路径最终形成CuS纳米管,而摩尔比较高时会通过Tu-Cu(Ⅰ)前驱物路径从而生成CuS纳米空心球。紫外-吸收光谱表明CuS纳米空心球在481 nm处有一个比较宽的吸收峰,而CuS纳米管却没有这样的峰。室温发光光谱表明CuS纳米空心球在432 nm处有一个发射峰,而对于CuS纳米管却没有探测到发射峰。本实验体系的条件温和,操作方便。研究结果发表在J.Nanosci.Nanotechnol.(2007,7,4501)上。
2.采用水热路径大规模的合成出了单晶的NiTe_2纳米片。这些纳米片具有正六边形的形貌。纳米片的平均边长和厚度分别为350 nm和85 nm。实验结果表明EDTA起着络合剂的作用,在控制产物的相成分和形貌方面都起到了关键作用。该实验体系反应简单,条件温和,费用低廉,具有潜在工业应用价值,使得这种方法更富有意义和吸引力。此方法可以进一步延伸到其他碲化物纳米材料的制备。研究结果发表在J.Nanosci.Nanotechnol.(2009,9.2715)上。
3.设计了一种无外加模板、无表面活性剂的溶液路径,采用乙二醇(EG)还原Cu(CH_3COO)_2的方法,成功的合成出了有序的Cu_2O纳米线阵列。其整体形貌看起来象压缩饼干。Cu_2O纳米线的直径大约为30 nm。对Cu_2O相成分和形貌的影响因素进行了系统的观察。反应体系简单,操作方便。研究结果发表在Mater.Chem.Phys.(2009,114,213)上。
4.设计了表面活性剂聚乙二醇(PEG)辅助的水热合成路线,选择CuCl作为铜源,氨水作为碱性介质,合成了三维的CuO片-片-球分级结构,CuO球的直径大约为3μm,每个微米球都是由无数的二维纳米片通过层层重叠生长模式组成的,这些纳米片的厚度大约为40 nm。而每个纳米片又是由很多更小的二维纳米片以边对边的方式聚集的。对CuO形貌的影响因素进行了系统的观察,其中,PEG的浓度对形貌起着很关键的作用。另外,研究了CuO分级微米球的形成机理。
Based on the chemical solution-phase synthesis,the aim of this dissertation is to explore the synthesis of CuS,NiTe_2,Cu_2O,CuO nanomaterials by room temperature chemical solution route,solvothermal technique and hydrothermal method.A chemical solution route has been developed to selectively prepare covellite(CuS) nanotubes and hollow nanospheres at room temperature;Single-crystalline NiTe_2 nanoplates with the hexagonal shape have been synthesized on a large scale through a hydrothermal method.Well-aligned arrays of cuprous oxide(Cu_2O) nanowires have been synthesized by an ethylene glycol-reduced process;Three-dimensional(3 D) CuO hierarchical microspheres have been prepared via a simple hydrothermal route.The morphologies and structures of as-prepared nanomaterials are characterized in detail.A systematic investigation has been carried out to understand the factors influencing the phase composition and morphology,and their formation mechanisms are also briefly discussed.The main contents can be summarized as follows:
1.A chemical solution route has been developed to synthesize CuS nanostructures through the precitation reaction of CuCl_2·2H_2O,thiourea(Tu) and NaHCO_3 in distilled water at room temperature.By regulating the concentration of Tu,CuS nanotubes and hollow nanospheres with diameters of 100-200 nm have been selectively prepared.Structural characterizations indicate that both nanotubes and hollow spheres are composed of CuS nanoparticles with diameters of about 5-10 nm.A systematic investigation has been carried out to understand the factors influencing the CuS morphology.Two different routes are identified to explain the formation of the nanotubes and hollow nanospheres herein.It is concluded that low concentration of Tu is favorable to CuS nanotubes via the thiourea-copper(Ⅱ) complex precursor route,while high concentration is favourable to CuS hollow spherical structures via the thiourea-copper(Ⅰ) complex precursor route.UV-vis absorption spectra show the CuS product with hollow nanosphere morphology shows a wide absorption peak centered at about 481 nm,while the product with nanotube morphology shows no such peak.Room-temperature PL spectra of CuS hollow nanospheres reveal a peak at around 432 nm,while no such peak for CuS nanotubes.UV-vis absorption and room PL spectra display different morphology-related absorption phenomena for nanotubes and hollow nanospheres. The experimental conditions are mild,and the manipulations are convenient. These results were published in J.Nanosci.Nanotechnol.(2007,7,4501).
2.Single-crystalline NiTe_2 nanoplates have been synthesized on a large scale through a hydrothermal reaction of Ni(CH_3COO)_2 and YeO_2 at 210℃for 48 h.The NiTe_2 nanoplates have hexagonal shape.The average edge sizes and thicknesses of nanoplates are 350 nm and 85 nm,respectively.Here,Ethylenediaminetetraacetic acid(EDTA) is employed as a chelating agent.Furthermore,EDTA plays crucial roles in controlling phase composition and morphology of the resultant products. The simple process,mild conditon and cheap cost in this work make the present route attractive and significant.It has potential industrial application.This method may be extended to prepare other tellurides nanomaterials.This study was published in J.Nanosci.Nanotechnol.(2009,9,2715).
3.Well-aligned arrays of Cuprous oxide(Cu_2O) nanowires were synthesized through the reduction of Cu(CH_3COO)_2 by ethylene glycol(EG) without the assistance of externally introduced template and surfactant.The panorama of well-aligned arrays of Cu_2O nanowires looks like a biscuit.These Cu_2O nanowires are～30 nm in diameter.A systematic investigation has been carried out to understand the factors influencing the phase composition and Cu_2O morphologies.The experimental system is simple and the manipulation is convenient.This study was published in Mater.Chem.Phys.(2009,114,213).
4.A simple hydrothermal route was developed to synthesize CuO three-dimensional (3D) hierarchical microspheres using CuCl as the copper source and PEG as the morphology-directing agent in ammonia aqueous medium.The microspheres with average diameter of about 3μm were constructed from two-dimensional(2D) nanosheets with average thickness of about 40 nm via a layer-by-layer growth style and the nanosheets were composed of tiny nanoplates through orientation attachment.The quantity of PEG played crucial roles in the formation of CuO hierarchical structures and a systematic investigation was carried out to understand the factors influencing the CuO morphology.The possible growth mechanism was identified to explain the formation of CuO architectures herein.
引文
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