Pt、Co和TiO_2一维纳米阵列的制备、表征及性能研究
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摘要
目前对于一维纳米材料的研究主要集中在三个方面:第一,探索可控制备一维纳米材料的方法。第二,研究单个纳米单元的基本性质,探讨在低维材料体系中的物理、化学规律。第三,以一维纳米结构为基本单元,探索纳米材料在低功耗、高性能、集成化的功能性器件中的应用。本论文着眼纳米科技的发展趋势,以阳极氧化法制备多孔的Al_2O3(AAO)和TiO_2(ATO)薄膜为基础,在以上三个方面进行了有益的探索。
通过改进的阳极氧化技术,开发了具有规则锯齿形分枝孔道的AAO薄膜。其制备方法简单易行,操作电压在10～80 V范围内可调。通过分析实验结果,深入研究了氧化膜的成分和结构特点。结合高场电导理论、阴离子在氧化膜中的迁移机理以及场致流动模型,并以有限元法多物理场建模与分析为辅助手段,解释了其特殊结构的形成机制。规则锯齿形孔道的形成和发展归因于阳极氧化过程中O_2气泡的产生以及氧化膜中的塑性变形。随后,利用多步阳极氧化技术,交替在磷酸和草酸溶液中进行阳极氧化,制备了多层堆垛的三维周期性结构。在熟悉AAO的结构特点、深入了解不同形貌AAO的实验技术的基础上,以AAO为模板制备了一系列不同的材料体系,研究了Pt纳米线阵列的电催化活性和Co纳米线/纳米管阵列的磁性能。
利用电沉积技术,分别在具有光滑孔道和锯齿形孔道的AAO模板中制备了不同形貌的Pt纳米线阵列。对于锯齿形Pt纳米线,其锯齿之间的距离(Db),锯齿的长度(lb)以及纳米线的总长度分别约为250 nm,250 nm和4μm。结构分析表明,Pt纳米线具有多晶结构,晶粒大小在5～9 nm范围内。结合实验结果和多物理场建模与分析,对Pt纳米线在甲醇溶液中的电催化性能进行了研究。结果表明,由于锯齿形结构的存在,纳米线周围的电场强度显著增强,纳米线电极表面具有更多的活性区域,因而其电催化活性明显优于具有光滑表面的Pt纳米线。
以具有光滑孔壁的AAO为模板,通过控制实验参数分别制备了Co纳米线和纳米管阵列。对于纳米线的分析表明,Co纳米线为六角密堆积(hcp)的单晶结构,其c轴垂直于纳米线的长轴方向。纳米线的电阻率约为75μ?·cm。磁滞回线研究表明,高的长径比使形状各向异性能占据主导优势,因而其长轴方向为易磁化方向。在对纳米线的磁力显微分析中发现,纳米线两端存在一对强烈的磁偶极子,同时沿纳米线方向有一个周期性的空间磁化调制现象。该现象是由于平行于纳米线方向的形状各向异性能和垂直于纳米线方向的磁晶各向异性能的竞争所致。
随后,利用电沉积技术在两端开口的纳米孔道中成功地制备了高填充率的Co纳米管阵列。结构分析表明,Co纳米管同样具有结晶质量较高的单晶hcp结构,其c轴垂直于纳米管的长轴方向。综合考虑纳米管中的形状各向异性能、磁晶各向异性能、交换作用能和塞曼能,磁矩在卷曲态的时候系统能量最低。因此当施加磁场的方向平行于纳米管时,磁化反转是一个缓慢的过程,磁滞回线呈现出一个扁平的环。同时,磁力显微分析也只测量到非常微弱的磁信号。从而,从实验的角度证实了这种卷曲模型,即在无外加磁场时,磁矩绕着纳米管管壁排列,并与管壁相切,组成一个封闭的环。
基于AAO的研究基础,利用类似的二次阳极氧化技术在NH4F的乙二醇溶液中制备了TiO_2纳米管阵列。在60 V的阳极电压下,纳米管的生长速率约为167 nm/min。元素分析表明,TiO_2纳米管中含有少量的F元素。这是由于阳极氧化过程中F-离子对TiO_2的溶解所致。经过退火处理,无定形的TiO_2纳米管转变为结晶态的锐钛矿相,并伴有少量的金红石结构。同时退火处理使其电导提高了3个数量级。随后利用原位的还原掺杂技术对纳米管底部阻挡层处理,从而选择性地进一步提高了纳米管底部的电导率。
研究开发了以TiO_2纳米管阵列为光阳极制备染料敏化太阳能电池(DSSCs)的技术。通过对TiO_2纳米管的热处理和TiCl4修饰处理工艺,DSSCs的光电转换效率达到了2.94 %。值得注意的是,纳米管底部封闭的阻挡层结构使DSSCs中的串联电阻较大,从而一定程度上阻碍了电池的光电转换效率的提高。随后,利用底部经还原掺杂的TiO_2纳米管为光阳极制备了DSSCs。由于串联电阻的减小,其短路光电流提高了约7 %,达到8.28 mA/cm2;总的光电转换效率提高了34 %,达到3.95 %。
纳米管底部阻挡层电导率的提高使在TiO_2中电沉积纳米线成为可能。并且,基于TiO_2本身的功能性,三维结构的复合材料有望在光电转换及能量储存领域显示出更优异的性能。利用电沉积技术成功地将p型半导体Cu_2O填充进TiO_2纳米管阵列中,构筑了三维结构的Cu_2O/TiO_2 p-n结薄膜。其光电转换效率达到0.009 %。这种新型的全固态金属氧化物电池全部是在溶液中利用电化学方法制备出来的,环境友好、原材料丰富、性能稳定、成本极低。因此如果能进一步通过优化工艺提高电池效率,有希望成为新型的固态廉价太阳能电池。同时三维结构的Cu_2O/TiO_2 p-n结还有可能具有更优异的光催化性能。
Significant research progresses of one-dimensional (1-D) systems have been achieved in the past decades. Researchers have been focusing on the following three areas. First, explore controllable synthesis approaches on 1-D materials. Second, study the fundamental physical and chemical properties on individual units. Third, assemble the 1-D nanomaterials as building blocks in low power consumption, high performance and highly integrated devices. In this study, we devote our efforts on the three different but close-related areas based on the novel structures of porous anodic aluminum and titanium oxides.
A unique and robust method is developed to design and fabricate anodic aluminum oxide (AAO) membranes with serrated nanochannels in phosphoric acid solution. The synthesis can be carried out under room temperature and in a wide operation voltage (10~80 V). Due to high field conduction and anionic incorporation, an increase of anodizing voltage leads to the increase of the impurity levels as well as the electric field across the barrier layer. The initialization and formation of serrated channels are attributed to the evolution of oxygen gas bubbles followed by plastic deformation in the oxide film based on both experiment and simulation results. Alternating anodization in oxalic and phosphoric acids is applied to construct multilayered membranes with smooth and serrated channels, which demonstrates three-dimensional hierarchical system with controllable morphology and composition.
To reveal the inside serrated channel structure, platinum is electrodeposited into the template. The interval distances, branch length, and total length of the as-synthesized serrated nanowires are about 250 nm, 250 nm, and 4μm, which are in accordance with the serrated channel spacing, length, and template thickness, respectively. X-ray diffraction (XRD) pattern and high resolution transmission electron microscope (HRTEM) image indicate that the crystal size is in the range of 5~9 nm. The electrocatalytic activities for methanol oxidation are evaluated on serrated nanowires in a conventional three-electrode system, which exhibits superior electrocatalytic activity compared to the straight nanowires. Combined with finite-element numerical simulation, we believe that the strengthened electric field around the serrated tips contributes predominantly to the enhanced electrocatalytic activities in addition to the increased surface area per unit Pt mass.
The AAO with smooth channels are used as templates to synthesize ferromagnetic cobalt nanowires and nanotubes. HRTEM and XRD results on Co nanowires (diameter~90 nm) show predominantly single crystal hexagonal close-packed (hcp) structure with the magnetocrystalline easy axis (c-axis) perpendicular to the wire axis. The conductivity of Co nanocrystal performed on an individual wire is around 75μ? ? cm. Hysteresis loops illustrate the dominance of shape anisotropy. Furthermore, the magnetic structures of Co nanowires are studied using magnetic force microscopy (MFM), which reveals a strong dipole at the two ends of the wire, together with a spatial magnetization modulation along the wire. Based on theoretical modeling, such intrinsic modulation is attributed to magnetization frustration due to the competition between the magnetocrystalline polarization along the easy axis and the shape anisotropy along the wire axis.
Subsequently, Co nanotubes are demonstrated by direct electroplating method inside the through-hole AAO membranes. The results manifest that the nanotubes are mainly hcp single crystals with the c-axis perpendicular to the tube axis. MFM imaging shows a weak magnetic signal and SQUID measurement reveals sheared hysteresis responses for field applied along the tube axis. Combined with theoretical modeling taking into account the shape demagnetization, crystal anisotropy, magnetic exchange, and external magnetic interaction energies, our measurements confirm that the magnetization curls circumferentially around the tube in order to minimize the total magnetic energy for small external fields.
Based on our successful achievement on the AAO, self-organized TiO_2 nanotube arrays are demonstrated by two-step anodization method in NH4F based electrolyte. The growth rate of TiO_2 nanotubes is ~167 nm/min under 60 V bias voltage in fresh electrolyte. The energy dispersive X-ray analysis (EDX) on TiO_2 nanotubes indicates trace amount F element resulting from the dissolution effect of NH4F. After the annealing treatment under 500℃for 6 h, the amorphous TiO_2 is converted to dominant anatase phase and trace amount of thermally grown rutile structure. Moreover, a conductive AFM tip coated with Ti/Au is contacted on an individual nanotube for the conductance measurement which exhibits three orders of magnitude higher than that of amorphous nanotubes. In order to further increase the conductance at the nanotube bottom, reductive doping method is adopted to facilitate more conductive barrier layer.
TiO_2 nanotube membranes are employed as photoanode in dye-sensitized solar cells (DSSCs). The energy conversion efficiency is achieved to be 2.94 % by optimizing the annealing parameters and TiCl4 treatment. The condensed barrier layer at nanotube bottom causes a relative high series resistance, corresponding to the low fill factor and conversion efficiency. Thus, the reductive doping of TiO_2 nanotubes is performed before the solar cell assembling. The packaged device exhibits improved performance with higher short circuit current density (8.28 mA/cm2) and energy conversion efficiency (3.95 %).
The enhanced conductivity of TiO_2 nanotube bottom makes it feasible to electrochemically deposit desired materials. Due to the 1-D structure and functionality of TiO_2 itself, three-dimensional core-shell structures is promising to exhibit superior performance in photovoltaics and energy storage devices. Herein, p-type Cu_2O is successfully filled into TiO_2 nanotube channels by electrodeposition. The three-dimensional Cu_2O/TiO_2 p-n junction films exhibit an energy conversion efficiency up to 0.009 %, which is much enhanced compared to the two-dimensional Cu_2O/TiO_2 films. The improved photovoltaic performances benefit from the high junction interface as well as the 1-D carriers’pathway due to the radial hetero-junction nature. Conclusively, the presented Cu_2O/TiO_2 system would be a promising candidate of solid-state low cost solar cell and photocatalyst due to their abundant, inexpensive and environmental friendly nature once the efficiency could be further improved by optimizing the device parameters.
通过改进的阳极氧化技术,开发了具有规则锯齿形分枝孔道的AAO薄膜。其制备方法简单易行,操作电压在10～80 V范围内可调。通过分析实验结果,深入研究了氧化膜的成分和结构特点。结合高场电导理论、阴离子在氧化膜中的迁移机理以及场致流动模型,并以有限元法多物理场建模与分析为辅助手段,解释了其特殊结构的形成机制。规则锯齿形孔道的形成和发展归因于阳极氧化过程中O_2气泡的产生以及氧化膜中的塑性变形。随后,利用多步阳极氧化技术,交替在磷酸和草酸溶液中进行阳极氧化,制备了多层堆垛的三维周期性结构。在熟悉AAO的结构特点、深入了解不同形貌AAO的实验技术的基础上,以AAO为模板制备了一系列不同的材料体系,研究了Pt纳米线阵列的电催化活性和Co纳米线/纳米管阵列的磁性能。
利用电沉积技术,分别在具有光滑孔道和锯齿形孔道的AAO模板中制备了不同形貌的Pt纳米线阵列。对于锯齿形Pt纳米线,其锯齿之间的距离(Db),锯齿的长度(lb)以及纳米线的总长度分别约为250 nm,250 nm和4μm。结构分析表明,Pt纳米线具有多晶结构,晶粒大小在5～9 nm范围内。结合实验结果和多物理场建模与分析,对Pt纳米线在甲醇溶液中的电催化性能进行了研究。结果表明,由于锯齿形结构的存在,纳米线周围的电场强度显著增强,纳米线电极表面具有更多的活性区域,因而其电催化活性明显优于具有光滑表面的Pt纳米线。
以具有光滑孔壁的AAO为模板,通过控制实验参数分别制备了Co纳米线和纳米管阵列。对于纳米线的分析表明,Co纳米线为六角密堆积(hcp)的单晶结构,其c轴垂直于纳米线的长轴方向。纳米线的电阻率约为75μ?·cm。磁滞回线研究表明,高的长径比使形状各向异性能占据主导优势,因而其长轴方向为易磁化方向。在对纳米线的磁力显微分析中发现,纳米线两端存在一对强烈的磁偶极子,同时沿纳米线方向有一个周期性的空间磁化调制现象。该现象是由于平行于纳米线方向的形状各向异性能和垂直于纳米线方向的磁晶各向异性能的竞争所致。
随后,利用电沉积技术在两端开口的纳米孔道中成功地制备了高填充率的Co纳米管阵列。结构分析表明,Co纳米管同样具有结晶质量较高的单晶hcp结构,其c轴垂直于纳米管的长轴方向。综合考虑纳米管中的形状各向异性能、磁晶各向异性能、交换作用能和塞曼能,磁矩在卷曲态的时候系统能量最低。因此当施加磁场的方向平行于纳米管时,磁化反转是一个缓慢的过程,磁滞回线呈现出一个扁平的环。同时,磁力显微分析也只测量到非常微弱的磁信号。从而,从实验的角度证实了这种卷曲模型,即在无外加磁场时,磁矩绕着纳米管管壁排列,并与管壁相切,组成一个封闭的环。
基于AAO的研究基础,利用类似的二次阳极氧化技术在NH4F的乙二醇溶液中制备了TiO_2纳米管阵列。在60 V的阳极电压下,纳米管的生长速率约为167 nm/min。元素分析表明,TiO_2纳米管中含有少量的F元素。这是由于阳极氧化过程中F-离子对TiO_2的溶解所致。经过退火处理,无定形的TiO_2纳米管转变为结晶态的锐钛矿相,并伴有少量的金红石结构。同时退火处理使其电导提高了3个数量级。随后利用原位的还原掺杂技术对纳米管底部阻挡层处理,从而选择性地进一步提高了纳米管底部的电导率。
研究开发了以TiO_2纳米管阵列为光阳极制备染料敏化太阳能电池(DSSCs)的技术。通过对TiO_2纳米管的热处理和TiCl4修饰处理工艺,DSSCs的光电转换效率达到了2.94 %。值得注意的是,纳米管底部封闭的阻挡层结构使DSSCs中的串联电阻较大,从而一定程度上阻碍了电池的光电转换效率的提高。随后,利用底部经还原掺杂的TiO_2纳米管为光阳极制备了DSSCs。由于串联电阻的减小,其短路光电流提高了约7 %,达到8.28 mA/cm2;总的光电转换效率提高了34 %,达到3.95 %。
纳米管底部阻挡层电导率的提高使在TiO_2中电沉积纳米线成为可能。并且,基于TiO_2本身的功能性,三维结构的复合材料有望在光电转换及能量储存领域显示出更优异的性能。利用电沉积技术成功地将p型半导体Cu_2O填充进TiO_2纳米管阵列中,构筑了三维结构的Cu_2O/TiO_2 p-n结薄膜。其光电转换效率达到0.009 %。这种新型的全固态金属氧化物电池全部是在溶液中利用电化学方法制备出来的,环境友好、原材料丰富、性能稳定、成本极低。因此如果能进一步通过优化工艺提高电池效率,有希望成为新型的固态廉价太阳能电池。同时三维结构的Cu_2O/TiO_2 p-n结还有可能具有更优异的光催化性能。
Significant research progresses of one-dimensional (1-D) systems have been achieved in the past decades. Researchers have been focusing on the following three areas. First, explore controllable synthesis approaches on 1-D materials. Second, study the fundamental physical and chemical properties on individual units. Third, assemble the 1-D nanomaterials as building blocks in low power consumption, high performance and highly integrated devices. In this study, we devote our efforts on the three different but close-related areas based on the novel structures of porous anodic aluminum and titanium oxides.
A unique and robust method is developed to design and fabricate anodic aluminum oxide (AAO) membranes with serrated nanochannels in phosphoric acid solution. The synthesis can be carried out under room temperature and in a wide operation voltage (10~80 V). Due to high field conduction and anionic incorporation, an increase of anodizing voltage leads to the increase of the impurity levels as well as the electric field across the barrier layer. The initialization and formation of serrated channels are attributed to the evolution of oxygen gas bubbles followed by plastic deformation in the oxide film based on both experiment and simulation results. Alternating anodization in oxalic and phosphoric acids is applied to construct multilayered membranes with smooth and serrated channels, which demonstrates three-dimensional hierarchical system with controllable morphology and composition.
To reveal the inside serrated channel structure, platinum is electrodeposited into the template. The interval distances, branch length, and total length of the as-synthesized serrated nanowires are about 250 nm, 250 nm, and 4μm, which are in accordance with the serrated channel spacing, length, and template thickness, respectively. X-ray diffraction (XRD) pattern and high resolution transmission electron microscope (HRTEM) image indicate that the crystal size is in the range of 5~9 nm. The electrocatalytic activities for methanol oxidation are evaluated on serrated nanowires in a conventional three-electrode system, which exhibits superior electrocatalytic activity compared to the straight nanowires. Combined with finite-element numerical simulation, we believe that the strengthened electric field around the serrated tips contributes predominantly to the enhanced electrocatalytic activities in addition to the increased surface area per unit Pt mass.
The AAO with smooth channels are used as templates to synthesize ferromagnetic cobalt nanowires and nanotubes. HRTEM and XRD results on Co nanowires (diameter~90 nm) show predominantly single crystal hexagonal close-packed (hcp) structure with the magnetocrystalline easy axis (c-axis) perpendicular to the wire axis. The conductivity of Co nanocrystal performed on an individual wire is around 75μ? ? cm. Hysteresis loops illustrate the dominance of shape anisotropy. Furthermore, the magnetic structures of Co nanowires are studied using magnetic force microscopy (MFM), which reveals a strong dipole at the two ends of the wire, together with a spatial magnetization modulation along the wire. Based on theoretical modeling, such intrinsic modulation is attributed to magnetization frustration due to the competition between the magnetocrystalline polarization along the easy axis and the shape anisotropy along the wire axis.
Subsequently, Co nanotubes are demonstrated by direct electroplating method inside the through-hole AAO membranes. The results manifest that the nanotubes are mainly hcp single crystals with the c-axis perpendicular to the tube axis. MFM imaging shows a weak magnetic signal and SQUID measurement reveals sheared hysteresis responses for field applied along the tube axis. Combined with theoretical modeling taking into account the shape demagnetization, crystal anisotropy, magnetic exchange, and external magnetic interaction energies, our measurements confirm that the magnetization curls circumferentially around the tube in order to minimize the total magnetic energy for small external fields.
Based on our successful achievement on the AAO, self-organized TiO_2 nanotube arrays are demonstrated by two-step anodization method in NH4F based electrolyte. The growth rate of TiO_2 nanotubes is ~167 nm/min under 60 V bias voltage in fresh electrolyte. The energy dispersive X-ray analysis (EDX) on TiO_2 nanotubes indicates trace amount F element resulting from the dissolution effect of NH4F. After the annealing treatment under 500℃for 6 h, the amorphous TiO_2 is converted to dominant anatase phase and trace amount of thermally grown rutile structure. Moreover, a conductive AFM tip coated with Ti/Au is contacted on an individual nanotube for the conductance measurement which exhibits three orders of magnitude higher than that of amorphous nanotubes. In order to further increase the conductance at the nanotube bottom, reductive doping method is adopted to facilitate more conductive barrier layer.
TiO_2 nanotube membranes are employed as photoanode in dye-sensitized solar cells (DSSCs). The energy conversion efficiency is achieved to be 2.94 % by optimizing the annealing parameters and TiCl4 treatment. The condensed barrier layer at nanotube bottom causes a relative high series resistance, corresponding to the low fill factor and conversion efficiency. Thus, the reductive doping of TiO_2 nanotubes is performed before the solar cell assembling. The packaged device exhibits improved performance with higher short circuit current density (8.28 mA/cm2) and energy conversion efficiency (3.95 %).
The enhanced conductivity of TiO_2 nanotube bottom makes it feasible to electrochemically deposit desired materials. Due to the 1-D structure and functionality of TiO_2 itself, three-dimensional core-shell structures is promising to exhibit superior performance in photovoltaics and energy storage devices. Herein, p-type Cu_2O is successfully filled into TiO_2 nanotube channels by electrodeposition. The three-dimensional Cu_2O/TiO_2 p-n junction films exhibit an energy conversion efficiency up to 0.009 %, which is much enhanced compared to the two-dimensional Cu_2O/TiO_2 films. The improved photovoltaic performances benefit from the high junction interface as well as the 1-D carriers’pathway due to the radial hetero-junction nature. Conclusively, the presented Cu_2O/TiO_2 system would be a promising candidate of solid-state low cost solar cell and photocatalyst due to their abundant, inexpensive and environmental friendly nature once the efficiency could be further improved by optimizing the device parameters.
引文
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