自组织结构的形成及其应用的实验研究
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摘要
自组织结构是在一定的内部和外部条件下系统自发形成的有序结构。沉积结晶生长的花样是典型的自组织结构。对自组织结构形成机理的研究不仅具有重要的理论意义,还能指导实际生产从而改善材料的质量和性能。铝阳极氧化形成的具有纳米孔阵列的多孔阳极氧化铝膜也是一种典型的自组织结构,以其为模板再采用气相或液相反应可产生许多金属、半导体及其它材料的纳米阵列。以气相或液相反应合成的氧化锌纳米棒阵列也属此种。自组织形成的纳米结构材料具有重要的意义：一方面,由于纳米材料的独特性质,可望发展出新型的功能材料和功能器件；另一方面,自组织生长纳米结构的方法具有成本低,简单易行的特点,更有实际价值。本文在自组织结构的形成及其应用方面开展了一些研究工作,主要内容包括以下几个方面：
(1)氯化铵在琼脂凝胶衬底上周期性自组织结构的形成
我们在琼脂衬底上的氯化铵结晶生长过程中得到了两种奇特的自发形成的形态交替转变的自组织花样。一种是密枝形态和稀枝形态之间的交替性转变,另一种是密枝和zigzag形态之间的交替性转变。在这些形态转变中,枝的变化是在一个包络线上同时发生的,另一方面,转变是不断重复发生的,并且不仅仅发生在晶体生长的末期,所以它们不同于以往报道过的形态转变现象。对这两种交替形态转变的自组织形成机理的研究有助于我们对复杂系统中晶体生长动力学的理解。
我们对这两种形态交替转变的自组织生长过程进行了研究,发现密枝形态比稀枝和zigzag形态的生长都快很多,并且在形态转变时生长速率也突然发生变化。为了弄清这两种形态交替转变的自组织形成机理,我们通过改变实验条件做了较全面的研究,并得到了一个相图。我们发现氯化铵结晶体的形态由两个主要因素决定,即初始溶液中的琼脂浓度与氯化铵浓度的比值和晶体生长时的相对湿度。在这个相图上有8个典型的花样,由交替性形态转变形成的花样位于某些花样之间。进一步的研究发现,根据宏观形态特征,这些花样可以分为三类：密枝、分形和团簇；而按照微观表面形貌,又可以分为两类：粗糙表面和光滑表面。于是我们对相图进行了重新的分区,并发现根据宏观形态特征的三个分区的分布主要依赖于Ca/CN的值,而根据微观表面形貌得到的两个分区的分布主要依赖于相对湿度的值。我们认为它们分别是由宏观溶质输运动力学和由微观界面生长动力学决定的。我们从这两方面分析了这些不同花样的形成机理,并基于此提出了形态交替转变的自组织形成机理。我们认为这两种形态性交替转变都是由生长界面前端溶质浓度的振荡导致的,而这种振荡又是由在适当的浓度比时晶体生长和溶质输运之间的竞争引起的。这两种交替性形态转变中究竟哪一种出现则依赖于相对湿度,因为相对湿度控制过饱和度。
(2)琼脂对薄层电沉积锌的沉积物形态的影响
薄层电沉积中沉积物的不同形态主要依赖于生长界面附近的物理化学环境。我们研究了琼脂对薄层电沉积锌沉积物形态的影响。在我们选择的生长条件下,未加琼脂时,沉积物宏观形态为枝晶型。随着琼脂浓度的增加,规则的枝晶形态逐渐消失,被密枝形态所取代。我们用扫描电镜和X射线衍射仪对沉积物进行了微观晶粒组织和结构特性的分析。从微观上看,枝晶形态由具有择优取向的晶粒有序地排列组成,密枝形态的晶粒则呈随机取向并杂乱分布,其晶粒尺寸也比枝晶形态的小。我们认为宏观上的形态转变是由微观上晶粒择优取向的被抑制导致的,这种抑制是由于琼脂对电结晶过程的随机干扰造成的。晶粒的细化可以认为有两个因素造成：首先,琼脂的添加降低了成核需要的活化能,导致成核率增加；其次,琼脂分子吸附在生长界面上,阻碍电结晶过程,导致晶粒生长速率减小。(3)锡掺杂和铁掺杂的二氧化钛纳米管阵列的形成及其光催化性质
在各种氧化物半导体光催化剂材料中,二氧化钛被认为是最适合被广泛应用于环境治理的材料。在实际应用方面,TiO2纳米管阵列又相对于其他的结构具有很多的优势,因为它具有比表面积大,并有易操作、易回收的特点。我们利用自组织多孔阳极氧化铝膜结合液相沉积方法分别制备了Sn掺杂和Fe掺杂的TiO2纳米管阵列。用扫描电镜、透射电镜、X射线衍射、紫外—可见吸收光谱对样品的形貌、结构和光学性质进行了分析。我们用紫外光下亚甲基蓝的降解反应考察了Sn掺杂的TiO2纳米管阵列的光催化活性。结果表明适量的Sn掺杂能有效地提高TiO2纳米管阵列的紫外光波段的光催化效率,我们实验中最佳掺Sn量为5.6at%。相对于未掺杂样品,Fe掺杂的TiO2纳米管阵列的紫外—可见吸收光谱上出现吸收边的红移和可见光区光吸收的增强。我们用可见光下亚甲基蓝的降解反应考察了Fe掺杂的TiO2纳米管阵列的光催化活性。结果表明Fe掺杂的TiO2纳米管阵列在可见光照射下具有良好的光催化活性,实验中得到的最佳掺Fe量为5.9at%。
(4)ZnO@SnO2核壳型纳米棒阵列的制备及其光致发光性质
用不同材料组成的核壳型一维纳米结构,由于它们具有优良的组合或独特性质以及它们在光电纳米器件应用方面的巨大潜力而引起了人们极大的关注。我们用一个简单的、低成本的方法合成了ZnO@SnO2核壳型纳米棒阵列。我们首先采用水溶液化学生长的方法得到自组织的ZnO纳米棒阵列,然后用液相沉积的方法将SnO2沉积在ZnO纳米棒上。我们用扫描电镜、透射电镜、X射线衍射对样品的形貌、结构进行了分析,并进行了光致发光特性的研究。实验发现,相对于单一的ZnO纳米棒阵列,ZnO@SnO2核壳型纳米棒阵列的光致发光特性显示出明显的紫外和绿光发光峰的增强。
Self-organized structures are ordered structures formed by systems in a spontaneous way under certain inside or outside conditions. Morphologies formed by deposition or crystal growth are the most typical self-organized structure. The study on the formation mechanism of self-organized structures is not only theoretically meaningful, but also can guide the practical manufacturing and thus improve the quality and property of the materials. The porous anodic alumina with nanohole arrays formed by anodization of Al is also a typical self-organized structure, which can be used as template by gas or liquid reactions to fabricate nanoarrays of metal, semiconductor or other materials. The ZnO nanoarrays obtained from gas or liquid reaction also belong to this kind. These nanostructures formed by self-organized process have significant im-portance. On one hand, the nanostructures possess of unique properties, which may lead to the development of new functional materials and devices, one the other hand, the method of self-organization is low cost and simple, which is more practically significant. In this thesis, we carried out some research on the formation and application of self-organized structures, the main contents including the following aspects:
(1) Alternating morphology transitions in crystallization of NH4Cl on agar plates
Two novel self-organized patterns formed by spontaneously alternating morphology transitions have been obtained in crystallization of NH4Cl on agar plates. One is the alternating morphology transitions between dense branching morphology and sparse branching morphology, and the other is the alternating morphology transitions between dense branching mor-phology and zigzag branching morphology. In these morphology transitions, the changes of branches happen simultaneously on an envelope, on the other hand, the transitions are continuously repeated, and do not just happen in the final stages of crystallization, so they are different from the previously mentioned morphology transitions. The investigation on the underlying mechanisms of these alternating morphology transitions would be helpful to understand the crystallization dynamics under a complex condition.
The self-organized growing process of these alternating morphology transitions was investigated, it was found that the dense branching morphology grew faster than the sparse branching morphology and the zigzag morphology, and the growth rate suddenly changed during the transitions. To clarify the self-organized growth mechanism of the two novel al-ternating morphology transitions, overall investigations with various experimental conditions were carried out, and a morphological phase diagram was obtained. It was found out that the mass proportion of agar to NH4Cl and the relative humidity were the key factors to determine the morphologies of the NH4Cl aggregate. There exist eight typical patterns in this morphological phase diagram, and the patterns formed by al-ternating morphology transitions were located between some patterns. Further studies found that based on the macroscopic morphological features, these patterns could be divided into three types:DBM, fractal and cluster, while according to the characteristics of the microscopic surface morphology, these patterns could be divided into two types:rough and smooth surface. Thus we proposed a new partition of the previous morphological phase diagram, and found that the distribution of the three regions divided according to the macroscopic morphological features mainly depend on the value of Ca/CN, while the distribution of the two regions based on the characteristics of microscopic surface morphology mainly depend on the relative humidity. We considered that they were controlled by macroscopic solute transport dynamics and microscopic interfacial growth kinetics, respectively. The formation mechanisms of the different patterns were discussed from these two aspects. Based on this, the self-organized formation mechanisms of the alternating morphology transitions were suggested. We considered that both the two alternating morphology transitions result from the oscillation of solute concentration in front of the growing interface caused by the competition of crystal growth and solute transfer at a moderate mass proportion. Which one of them occurs depends on the relative humidity, which controls the supersaturation.
(2) Effect of agar on the deposit morphology from thin-layer elec-trodeposition of Zn
The different morphologies of deposits from the thin-layer elec-trodeposition depend on the physicochemical environment in the vicinity of the growing interface. The effect of agar on the morphology of the Zn deposits from thin-layer electrodeposition was investigated. Under the chosen conditions and without agar, the macroscopic morphology of deposit is dendritic. As the concentration of agar increases, the regular dendritic morphology disappears progressively and gives place to the dense branch morphology. The microscopical grain texture and structural characteristics of the deposits have been investigated by scanning electron microscopy and X-ray diffraction. Microscopically, the den-dritic morphology displays an orderly alignment of grains with a preferred orientation, while the dense branch morphology has a randomly oriented grain texture and diminished grain size compared to that of the dendritic morphology. This macroscopical morphological transition can be asso-ciated to the impediment of preferential oriented growth of grains at the small scale, which is caused by the random perturbations on the electrocrystallization process introduced by agar gel. The refinement of grains caused by the gel can be attributed to two factors. Firstly, agar additives reduce the activation energy of nucleation, so the nucleation rate increases. Secondly, agar molecules adsorb at the growing interface and impede the electrocrystallization process, as a result, the growth rate decreases.
(3) Formation and photocatalytic properties of Sn-doped and Fe-doped TiO2 nanotube arrays
Among various oxide semiconductor photocatalysts, TiO2 has been considered to be the most suitable materials for widespread environmental applications. Compared to other structures, TiO2 nanotube arrays show some advantages for practical applications, because of their high specific surface area and easiness in operation, recovery and recycling. We produced Sn-doped and Fe-doped TiO2 nanotube arrays by the template-based LPD method with the self—organized AAO membrane as the template. Their morphologies, structures and optical properties have been investigated by scanning electron microscope, transmission electron microscope, X-ray diffraction, UV-visible absorption spectroscopy. The photocatalytic properties of the Sn-doped nanotube arrays were evaluated with the degradation of methylene blue under UV irradiation. The result showed that doping an appropriate amount of Sn can effectively improve the photocatalytic activity of TiO2 nanotube arrays under UV irradiation, and the optimum dopant amount is found to be 5.6at% in our experiments. The UV-visible absorption spectra of the Fe-doped TiO2 nanotube arrays showed a red shift and an enhancement of the absorption in the visible region compared to the undoped sample. The photocatalytic properties of the Fe-doped TiO2 nanotube arrays were evaluated with the degradation of methylene blue under visible light. The result showed that the Fe-doped TiO2 nanotube arrays exhibited good photocatalytic activities under visible light irradiation, and the optimum dopant amount was found to be 5.9at% in our experiments.
(4) Synthesis and photoluminescence properties of the ZnO@SnO2 core-shell nanorod arrays
Coaxial one-dimensional nanostructures consisting of different materials have attracted considerable research attention because of their combined or unique properties and great potential for applications in electronic and optoelectronic nanodevices. We produced ZnO@SnO2 core-shell nanorod arrays by using a very simple and low cost method. In this method, self-organized ZnO nanorod arrays were first obtained by aqueous chemical growth method, and then SnO2 was deposited on the ZnO nanorod arrays by liquid phase deposition method. Scanning electron microscopy, transmission electron microscopy and X-ray diffraction were used to characterize the structure and morphologies of the products. Photoluminescence properties were also investigated. It was found that the ZnOiSnO2 nanorod arrays showed enhanced UV and green emissions compared with the bare ZnO nanorod arrays.
(1)氯化铵在琼脂凝胶衬底上周期性自组织结构的形成
我们在琼脂衬底上的氯化铵结晶生长过程中得到了两种奇特的自发形成的形态交替转变的自组织花样。一种是密枝形态和稀枝形态之间的交替性转变,另一种是密枝和zigzag形态之间的交替性转变。在这些形态转变中,枝的变化是在一个包络线上同时发生的,另一方面,转变是不断重复发生的,并且不仅仅发生在晶体生长的末期,所以它们不同于以往报道过的形态转变现象。对这两种交替形态转变的自组织形成机理的研究有助于我们对复杂系统中晶体生长动力学的理解。
我们对这两种形态交替转变的自组织生长过程进行了研究,发现密枝形态比稀枝和zigzag形态的生长都快很多,并且在形态转变时生长速率也突然发生变化。为了弄清这两种形态交替转变的自组织形成机理,我们通过改变实验条件做了较全面的研究,并得到了一个相图。我们发现氯化铵结晶体的形态由两个主要因素决定,即初始溶液中的琼脂浓度与氯化铵浓度的比值和晶体生长时的相对湿度。在这个相图上有8个典型的花样,由交替性形态转变形成的花样位于某些花样之间。进一步的研究发现,根据宏观形态特征,这些花样可以分为三类：密枝、分形和团簇；而按照微观表面形貌,又可以分为两类：粗糙表面和光滑表面。于是我们对相图进行了重新的分区,并发现根据宏观形态特征的三个分区的分布主要依赖于Ca/CN的值,而根据微观表面形貌得到的两个分区的分布主要依赖于相对湿度的值。我们认为它们分别是由宏观溶质输运动力学和由微观界面生长动力学决定的。我们从这两方面分析了这些不同花样的形成机理,并基于此提出了形态交替转变的自组织形成机理。我们认为这两种形态性交替转变都是由生长界面前端溶质浓度的振荡导致的,而这种振荡又是由在适当的浓度比时晶体生长和溶质输运之间的竞争引起的。这两种交替性形态转变中究竟哪一种出现则依赖于相对湿度,因为相对湿度控制过饱和度。
(2)琼脂对薄层电沉积锌的沉积物形态的影响
薄层电沉积中沉积物的不同形态主要依赖于生长界面附近的物理化学环境。我们研究了琼脂对薄层电沉积锌沉积物形态的影响。在我们选择的生长条件下,未加琼脂时,沉积物宏观形态为枝晶型。随着琼脂浓度的增加,规则的枝晶形态逐渐消失,被密枝形态所取代。我们用扫描电镜和X射线衍射仪对沉积物进行了微观晶粒组织和结构特性的分析。从微观上看,枝晶形态由具有择优取向的晶粒有序地排列组成,密枝形态的晶粒则呈随机取向并杂乱分布,其晶粒尺寸也比枝晶形态的小。我们认为宏观上的形态转变是由微观上晶粒择优取向的被抑制导致的,这种抑制是由于琼脂对电结晶过程的随机干扰造成的。晶粒的细化可以认为有两个因素造成：首先,琼脂的添加降低了成核需要的活化能,导致成核率增加；其次,琼脂分子吸附在生长界面上,阻碍电结晶过程,导致晶粒生长速率减小。(3)锡掺杂和铁掺杂的二氧化钛纳米管阵列的形成及其光催化性质
在各种氧化物半导体光催化剂材料中,二氧化钛被认为是最适合被广泛应用于环境治理的材料。在实际应用方面,TiO2纳米管阵列又相对于其他的结构具有很多的优势,因为它具有比表面积大,并有易操作、易回收的特点。我们利用自组织多孔阳极氧化铝膜结合液相沉积方法分别制备了Sn掺杂和Fe掺杂的TiO2纳米管阵列。用扫描电镜、透射电镜、X射线衍射、紫外—可见吸收光谱对样品的形貌、结构和光学性质进行了分析。我们用紫外光下亚甲基蓝的降解反应考察了Sn掺杂的TiO2纳米管阵列的光催化活性。结果表明适量的Sn掺杂能有效地提高TiO2纳米管阵列的紫外光波段的光催化效率,我们实验中最佳掺Sn量为5.6at%。相对于未掺杂样品,Fe掺杂的TiO2纳米管阵列的紫外—可见吸收光谱上出现吸收边的红移和可见光区光吸收的增强。我们用可见光下亚甲基蓝的降解反应考察了Fe掺杂的TiO2纳米管阵列的光催化活性。结果表明Fe掺杂的TiO2纳米管阵列在可见光照射下具有良好的光催化活性,实验中得到的最佳掺Fe量为5.9at%。
(4)ZnO@SnO2核壳型纳米棒阵列的制备及其光致发光性质
用不同材料组成的核壳型一维纳米结构,由于它们具有优良的组合或独特性质以及它们在光电纳米器件应用方面的巨大潜力而引起了人们极大的关注。我们用一个简单的、低成本的方法合成了ZnO@SnO2核壳型纳米棒阵列。我们首先采用水溶液化学生长的方法得到自组织的ZnO纳米棒阵列,然后用液相沉积的方法将SnO2沉积在ZnO纳米棒上。我们用扫描电镜、透射电镜、X射线衍射对样品的形貌、结构进行了分析,并进行了光致发光特性的研究。实验发现,相对于单一的ZnO纳米棒阵列,ZnO@SnO2核壳型纳米棒阵列的光致发光特性显示出明显的紫外和绿光发光峰的增强。
Self-organized structures are ordered structures formed by systems in a spontaneous way under certain inside or outside conditions. Morphologies formed by deposition or crystal growth are the most typical self-organized structure. The study on the formation mechanism of self-organized structures is not only theoretically meaningful, but also can guide the practical manufacturing and thus improve the quality and property of the materials. The porous anodic alumina with nanohole arrays formed by anodization of Al is also a typical self-organized structure, which can be used as template by gas or liquid reactions to fabricate nanoarrays of metal, semiconductor or other materials. The ZnO nanoarrays obtained from gas or liquid reaction also belong to this kind. These nanostructures formed by self-organized process have significant im-portance. On one hand, the nanostructures possess of unique properties, which may lead to the development of new functional materials and devices, one the other hand, the method of self-organization is low cost and simple, which is more practically significant. In this thesis, we carried out some research on the formation and application of self-organized structures, the main contents including the following aspects:
(1) Alternating morphology transitions in crystallization of NH4Cl on agar plates
Two novel self-organized patterns formed by spontaneously alternating morphology transitions have been obtained in crystallization of NH4Cl on agar plates. One is the alternating morphology transitions between dense branching morphology and sparse branching morphology, and the other is the alternating morphology transitions between dense branching mor-phology and zigzag branching morphology. In these morphology transitions, the changes of branches happen simultaneously on an envelope, on the other hand, the transitions are continuously repeated, and do not just happen in the final stages of crystallization, so they are different from the previously mentioned morphology transitions. The investigation on the underlying mechanisms of these alternating morphology transitions would be helpful to understand the crystallization dynamics under a complex condition.
The self-organized growing process of these alternating morphology transitions was investigated, it was found that the dense branching morphology grew faster than the sparse branching morphology and the zigzag morphology, and the growth rate suddenly changed during the transitions. To clarify the self-organized growth mechanism of the two novel al-ternating morphology transitions, overall investigations with various experimental conditions were carried out, and a morphological phase diagram was obtained. It was found out that the mass proportion of agar to NH4Cl and the relative humidity were the key factors to determine the morphologies of the NH4Cl aggregate. There exist eight typical patterns in this morphological phase diagram, and the patterns formed by al-ternating morphology transitions were located between some patterns. Further studies found that based on the macroscopic morphological features, these patterns could be divided into three types:DBM, fractal and cluster, while according to the characteristics of the microscopic surface morphology, these patterns could be divided into two types:rough and smooth surface. Thus we proposed a new partition of the previous morphological phase diagram, and found that the distribution of the three regions divided according to the macroscopic morphological features mainly depend on the value of Ca/CN, while the distribution of the two regions based on the characteristics of microscopic surface morphology mainly depend on the relative humidity. We considered that they were controlled by macroscopic solute transport dynamics and microscopic interfacial growth kinetics, respectively. The formation mechanisms of the different patterns were discussed from these two aspects. Based on this, the self-organized formation mechanisms of the alternating morphology transitions were suggested. We considered that both the two alternating morphology transitions result from the oscillation of solute concentration in front of the growing interface caused by the competition of crystal growth and solute transfer at a moderate mass proportion. Which one of them occurs depends on the relative humidity, which controls the supersaturation.
(2) Effect of agar on the deposit morphology from thin-layer elec-trodeposition of Zn
The different morphologies of deposits from the thin-layer elec-trodeposition depend on the physicochemical environment in the vicinity of the growing interface. The effect of agar on the morphology of the Zn deposits from thin-layer electrodeposition was investigated. Under the chosen conditions and without agar, the macroscopic morphology of deposit is dendritic. As the concentration of agar increases, the regular dendritic morphology disappears progressively and gives place to the dense branch morphology. The microscopical grain texture and structural characteristics of the deposits have been investigated by scanning electron microscopy and X-ray diffraction. Microscopically, the den-dritic morphology displays an orderly alignment of grains with a preferred orientation, while the dense branch morphology has a randomly oriented grain texture and diminished grain size compared to that of the dendritic morphology. This macroscopical morphological transition can be asso-ciated to the impediment of preferential oriented growth of grains at the small scale, which is caused by the random perturbations on the electrocrystallization process introduced by agar gel. The refinement of grains caused by the gel can be attributed to two factors. Firstly, agar additives reduce the activation energy of nucleation, so the nucleation rate increases. Secondly, agar molecules adsorb at the growing interface and impede the electrocrystallization process, as a result, the growth rate decreases.
(3) Formation and photocatalytic properties of Sn-doped and Fe-doped TiO2 nanotube arrays
Among various oxide semiconductor photocatalysts, TiO2 has been considered to be the most suitable materials for widespread environmental applications. Compared to other structures, TiO2 nanotube arrays show some advantages for practical applications, because of their high specific surface area and easiness in operation, recovery and recycling. We produced Sn-doped and Fe-doped TiO2 nanotube arrays by the template-based LPD method with the self—organized AAO membrane as the template. Their morphologies, structures and optical properties have been investigated by scanning electron microscope, transmission electron microscope, X-ray diffraction, UV-visible absorption spectroscopy. The photocatalytic properties of the Sn-doped nanotube arrays were evaluated with the degradation of methylene blue under UV irradiation. The result showed that doping an appropriate amount of Sn can effectively improve the photocatalytic activity of TiO2 nanotube arrays under UV irradiation, and the optimum dopant amount is found to be 5.6at% in our experiments. The UV-visible absorption spectra of the Fe-doped TiO2 nanotube arrays showed a red shift and an enhancement of the absorption in the visible region compared to the undoped sample. The photocatalytic properties of the Fe-doped TiO2 nanotube arrays were evaluated with the degradation of methylene blue under visible light. The result showed that the Fe-doped TiO2 nanotube arrays exhibited good photocatalytic activities under visible light irradiation, and the optimum dopant amount was found to be 5.9at% in our experiments.
(4) Synthesis and photoluminescence properties of the ZnO@SnO2 core-shell nanorod arrays
Coaxial one-dimensional nanostructures consisting of different materials have attracted considerable research attention because of their combined or unique properties and great potential for applications in electronic and optoelectronic nanodevices. We produced ZnO@SnO2 core-shell nanorod arrays by using a very simple and low cost method. In this method, self-organized ZnO nanorod arrays were first obtained by aqueous chemical growth method, and then SnO2 was deposited on the ZnO nanorod arrays by liquid phase deposition method. Scanning electron microscopy, transmission electron microscopy and X-ray diffraction were used to characterize the structure and morphologies of the products. Photoluminescence properties were also investigated. It was found that the ZnOiSnO2 nanorod arrays showed enhanced UV and green emissions compared with the bare ZnO nanorod arrays.
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