Zn基微/纳米超结构的可控合成、表征及性能
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摘要
无机微/纳米超结构的成分、尺寸、形貌和结构等对其性能有着十分重要的影响,探索它们之间的关系已经成为现代微/纳米材料领域研究的热点。在光子学、电子学、物理与化学领域,Zn基超结构有着重要的应用前景。本论文系统的研究和探索了ZnO、硅酸锌、Ag/ZnO和Cu/ZnO等Zn基超结构的可控合成、组装和性能。
1.在不使用表面活性剂与模板的条件下,用简单的水热技术,仅仅通过调节反应参数,成功地合成了形貌、尺寸可控的ZnO三维超结构,包括花形、星形、球形与海胆形结构。ZnO超结构气敏性能测试表明,不同形貌的ZnO超结构对乙醇的灵敏度与选择性不同,其中,放射状花形ZnO超结构对乙醇的灵敏度高达11.3。
随后,使用表面活性剂在导电玻璃表面,水热合成了ZnO三维花状超结构薄膜。通过调节表面活性剂种类与锌源的用量,获得了不同大小和表面粗糙度可控的ZnO三维花状超结构薄膜。研究表明ZnO三维花状超结构薄膜的表面粗糙度是影响其荧光性质的一个重要因素
2.使用水热合成方法,在Si基片上首次制备了形貌可控的Zn4Si2O7(OH)2·H2O(下文简称ZSO)空心花形分级超结构,这种超结构的特点是,很多根平行的初级亚微米棒组装成单个次级棒束,多个次级棒束的一端连接在起、组装成空心花形分级超结构。研究了反应物浓度、反应时间、反应温度、表面活性剂、Zn源种类及后处理温度,对ZSO花形分级超结构形貌与晶体结构的影响。(a)Zn2+浓度的变化主要影响构成ZSO超结构中次级棒束的形貌,随着浓度的降低,组成次级棒束的初级单元依次变为亚微米棒、扁棱柱形亚微米片薄纳米片、圆柱形亚微米棒。(b)反应时间的变化,直接决定是否能够得到正交晶型ZSO的花形超结构薄膜：反应时间越长,薄膜中ZSO的含量越高；反应时间为12h时,得到较纯的正交晶型ZSO花形分级超结构薄膜。(c)反应温度不仅影响超结构的形貌,还改变超结构的成分；温度越高,次级棒束的分级特征越明显、次级棒束中含有的初级棒尺寸越小,超结构中正交晶型ZSO的含量也越高。(d)表面活性剂主要改变正交晶型ZSO分级超结构的次级棒束形貌,使用表面活性剂,可以实现分级结构中次级棒束的进一步分级,也可以实现次级棒束向不分级的单根次级棒转变。(e)使用Zn源的种类,可以控制次级棒束的分级程度,即实现次级棒束向单根次级微米棒、或向直径逐渐变小的单根次级微/纳微米棒转化。(f)后处理温度主要影响晶体结构,低于500℃时,对ZSO的晶体结构与形貌无影响；后处理温度为950℃时,正交晶型的ZSO转变为三角晶型的Zn2SiO4,而对ZSO的形貌影响不大。随后讨论了ZSO花形分级超结构的形成机理。
正交晶型的ZSO的荧光性质研究表明,组成花形超结构的次级棒束的分级特征越明显、表面粗糙度越大,荧光光谱的强度越强,反之越弱。表面润湿性研究表明,接触角与表面形貌有关,不同表面形貌的ZSO超结构薄膜与水的接触角不同,次级结构为棒束的ZSO接触角最大,达到143.1°。
3.用ZnO超结构和AgNO3为原料,以浸涂的方法,制备了对甲醇气敏响应较好的Ag/ZnO三维花形超结构；在Ag/ZnO三维花形超结构中,将Ag+负载到ZnO三维花形超结构中亚微米棒的表面,80℃烘干后,Ag+以AgNO3、Ag20的形式存住；300℃热处理后,Ag+转变为金属Ag,同时在ZnO棒表而出现长方形孔。研究发现,Ag+对ZnO亚微米棒的表面有较强的刻蚀作用；Ag+的浓度越高、反应时间越长,刻蚀作用越明显；在Ag+浓度与反应时间不变的情况下,热处理温度决定Ag+对ZnO亚微米棒表面的刻蚀效果。此外,热处理对Ag/ZnO三维花形超结构的气敏性能影响较大,热处理前,超结构对CH30H的灵敏度仅为2.3,而热处理后对CH30H的灵敏度达到9.3。
通过掺杂的方式,获得了光催化性能较好的Cu/ZnO三维花形超结构。在Cu/ZnO三维花形超结构中,当Cu2+的掺杂量低于5%时,Cu2+的作用主要是改变ZnO花形超结构中棒的数量与形貌,即Cu2+掺杂导致组成ZnO三维花形超结构中棒的数量增加,棒的尖端出现台阶形结构,或者刻蚀棒的侧而；Zn2+:Cu2+摩尔比为7:1时,Cu2+负载在六棱柱形ZnO棒的表面,形成CuO/ZnO花形核壳超结构；Zn2+:Cu2+摩尔比为3:1时,产品中单斜晶型CuO与六方晶型ZnO共存；Zn2+:Cu2+摩尔比为3:4时,产物为掺Zn的CuO海胆形纳米超结构。荧光光谱研究表明,Cu2+掺杂量增加,Cu/ZnO三维花形超结构的荧光强度减弱；Cu/ZnO三维花形超结构的光催化性能研究表明,Zn2+:Cu2+摩尔比为7:1时,制备的Cu/ZnO三维花形超结构催化剂在连续降解甲基橙与直接湖蓝染料的过程中表现出良好的催化稳定性,在180 min内,降解率分别达到84.7%、77.6%。
4.以金属Zn为原料,在透射电子显微镜内,用电子束原位辐照的方法制备了形状多样、尺寸可控、单分散、高纯度的金属Zn纳米粒子。Zn纳米粒子形状多样,包括长方形、三角形、菱形与六棱柱形等,它们的直径在10-30 nm之间。在Zn纳米粒子形成过程中,电子束在原材料内部产生的热柱导致材料局部温度迅速升高；电流密度越大,电子剂量越多、电子束的直径越小,导致局部原料升华越迅速,纳米晶体的生长过程越快,得到的Zn纳米粒子越小；辐照时间增长时,小的Zn粒子可以融合成大的Zn纳米粒子。
The properties of inorganic micro/nano-superstructures are dependent on their composition, size, shape and crystalline structure. Investigation on the relationships among these features has attracted increasing attentions in modern science and technology. Zn-based materials superstructures are important for the potential applications, including, photonics, electronics, physics, and chemistry. In this thesis, we have systematically studied and explored the controllable synthesis, assembly, and properties of Zn-based materials superstructures, which include ZnO, Zn silicates, Ag/ZnO and Cu/ZnO composite materials.
1. ZnO 3-dimensiaonal (3D) superstructures with controlled morphology and size, including flower-like, star-like, sphere-like and sea urchin-like shapes, are fabricated by a simple hydrothermal method without any surfactant or template. The gas sensing examinations show that the different Zn-based superstructures have different sensitivity to ethanol, and the sensitivity of the radial-like ZnO 3D flower-like superstructures to ethanol can reach 11.3.
The films made of the ZnO 3D flower-like superstructures on the glass are fabricated by a simple hydrothermal method using the surfactant, and the surface roughness of the ZnO 3D superstructure films can be conveniently controlled by changing the different surfactants and dosage of Zn sources, with excellent reproducibility. The photoluminescence (PL) spectra of the ZnO 3D superstructure films show that their PL properties are dependent on the surface roughness of as-synthesized ZnO superstructure films.
2. Zn4Si2O7(OH)2·H2O (ZSO) 3D hollow flower-like hierarchical superstructure films deposited on the Si substrate are firstly prepared by a simple hydrothermal route. Each hollow superstructure is consisted of secondary rod bundles which are assembled by many primary rods. The morphologies of the ZSO 3D superstructures can be tuned by changing the concentration of reactant, reaction time and temperature, surfactant, the Zn sources and annealing temperature. The results are summarized as follows:(a) The morphology of the secondary rod bundles within the ZSO 3D superstructures can be conveniently controlled from micrometer-sized prism to sub-micrometer slice, sub-micrometer rods and nanorods by only tuning the concentration of Zn2+. (b) The morphology and structure of the ZSO 3D superstructures are related to the reaction time; with the temperature increasing, the rod size of the bundles is getting smaller and the molar ratio of the ZSO:ZnO is increasing. (c) The reaction temperature not only affects the shape of the superstructures, but also changes their compositions. The higher the temperature, the more remarkable is the hierarchical feature of the secondary rod bundle, and the smaller is the size of the primary rods in the secondary bundles, and the higher is the molar ratio of the ZSO:ZnO within a superstructure. (d) The surfactant has effects on the morphology of the secondary rod bundles within the ZSO hierarchical superstructures; it realizes further hierarchy of the secondary bundles as well as their transformation to single non-hierarchical secondary rod. (e) The hierarchical structures of the secondary rod bundles, which realize the transformation from their united secondary bundles to a single secondary micrometer-sized rod, or to a single secondary micro- or nanometer-sized rod with its diameter varying, can be controlled by using different Zn sources. (f) The crystal structure is mainly depended on heating treatment temperature; below 500℃, the crystal structure of the ZSO is not changed, and at 950℃, orthorhombic ZSO superstructure can be transferred into monoclinic Zn2SiO4.
The PL spectra from the orthorhombic ZSO 3D superstructures films show that the stronger the intensity of the PL spectra, the smaller is the diameter of primary rod in secondary rod bundles, and the bigger is the ZSO surface roughness. The investigation on the wettability of the ZSO superstructures films shows that the angle of contact (CA) is mostly relied on the surface shape, and the CA of the ZSO superstructure films varying with their surface shape. It is found that the CA of the ZSO superstructure films consisted of the secondary rod bundles is the highest and reach to 143.1.
3. Ag/ZnO 3D superstructures are prepared by the dip coating process, using as-synthesized ZnO 3D supperstructures and AgN03 as the source materials; these composite superstructures show excellent gas sensitivity to methyl alcohol. Ag+ on the surface of the ZnO submicrorods exits in a form of AgNO3 or Ag2O after being dried at～80℃. Annealing at 300℃, AgNO3 or Ag2O is transformed into metal Ag (nanoparticles) and the rectangular holes form on the surface of the ZnO rods, suggesting that the surface of the ZnO submicrorods can be etched by metal Ag nanoparticles. The etching is enhanced with the increase of the concentration of Ag+ solution and reaction time, and it is also dependent on the heating treatment temperature. The Ag/ZnO 3D superstructures by annealing at 300℃can improve their selectivity to methyl alcohol, and their sensitivity is up to 9.3.
The Cu/ZnO 3D flower-like superstructures with excellent photocatalysis property can be fabricated by doping method. These morphologies of the Cu/ZnO 3D superstructures can be varied by tuning the reactant concentration. When the content of Cu2+ is below 5%, the Cu2+ mainly change the amount and shape of the ZnO rods inside the ZnO 3D superstructure; the doping of Cu2+ leads to the increase of the rods in ZnO 3D superstructure, companying the formation of the step-like shape at the rod top. When the molar ratio of Zn2+: Cu2+ is 7:1, Cu2+ is loaded on the surface of ZnO rods, forming CuO/ZnO core-shell rods. When the molar ratio of Zn2+:Cu2+ is 3:1, the mixture of the CuO and ZnO flower-like rods is obtained. When the molar ratio of Zn2+:Cu2+ is 3:4, the Zn doped CuO urchin-like superstructures are fabricated. The PL intensity of the Cu/ZnO 3D superstructures will decrease with the increasing doping of Cu2+. The Cu/ZnO 3D structures fabricated with the molar ratio of Zn2+ Cu2+ of 7:1 exhibit a higher photocatalytic activity. The efficiencies of the photocatalytic degradation of methyl orange and direct shy blue 5B are investigated; the degradation ratio of the samples reaches 84.7% and 77.6%, respectively.
4. In situ electron-beam irradiation in a transmission electron microscope is performed to fabricate different shape, controllable size, monodispersed, and high pure Zn nanoparticles by using Zn powders as the source material. As-synthesized Zn nanocrystals display various regular geometrical shapes, including rectangle, rhombus, triangle, and hexagon, with a diameter of 10-30 nm. During the formation of Zn nanoparticles, a convergent electron beam is focused on an raw Zn particle, and then cause partial melting and evaporation of the particle and subsequent nucleation and growth of Zn nanoparticles on the C film; the higher the dose of the electron beam, the smaller the diameter of the electron beam, the smaller is the diameters of Zn nanoparticles; while the smaller particles are merged each other under a longer period of the irradiation, resulting in the particles'growth.
1.在不使用表面活性剂与模板的条件下,用简单的水热技术,仅仅通过调节反应参数,成功地合成了形貌、尺寸可控的ZnO三维超结构,包括花形、星形、球形与海胆形结构。ZnO超结构气敏性能测试表明,不同形貌的ZnO超结构对乙醇的灵敏度与选择性不同,其中,放射状花形ZnO超结构对乙醇的灵敏度高达11.3。
随后,使用表面活性剂在导电玻璃表面,水热合成了ZnO三维花状超结构薄膜。通过调节表面活性剂种类与锌源的用量,获得了不同大小和表面粗糙度可控的ZnO三维花状超结构薄膜。研究表明ZnO三维花状超结构薄膜的表面粗糙度是影响其荧光性质的一个重要因素
2.使用水热合成方法,在Si基片上首次制备了形貌可控的Zn4Si2O7(OH)2·H2O(下文简称ZSO)空心花形分级超结构,这种超结构的特点是,很多根平行的初级亚微米棒组装成单个次级棒束,多个次级棒束的一端连接在起、组装成空心花形分级超结构。研究了反应物浓度、反应时间、反应温度、表面活性剂、Zn源种类及后处理温度,对ZSO花形分级超结构形貌与晶体结构的影响。(a)Zn2+浓度的变化主要影响构成ZSO超结构中次级棒束的形貌,随着浓度的降低,组成次级棒束的初级单元依次变为亚微米棒、扁棱柱形亚微米片薄纳米片、圆柱形亚微米棒。(b)反应时间的变化,直接决定是否能够得到正交晶型ZSO的花形超结构薄膜：反应时间越长,薄膜中ZSO的含量越高；反应时间为12h时,得到较纯的正交晶型ZSO花形分级超结构薄膜。(c)反应温度不仅影响超结构的形貌,还改变超结构的成分；温度越高,次级棒束的分级特征越明显、次级棒束中含有的初级棒尺寸越小,超结构中正交晶型ZSO的含量也越高。(d)表面活性剂主要改变正交晶型ZSO分级超结构的次级棒束形貌,使用表面活性剂,可以实现分级结构中次级棒束的进一步分级,也可以实现次级棒束向不分级的单根次级棒转变。(e)使用Zn源的种类,可以控制次级棒束的分级程度,即实现次级棒束向单根次级微米棒、或向直径逐渐变小的单根次级微/纳微米棒转化。(f)后处理温度主要影响晶体结构,低于500℃时,对ZSO的晶体结构与形貌无影响；后处理温度为950℃时,正交晶型的ZSO转变为三角晶型的Zn2SiO4,而对ZSO的形貌影响不大。随后讨论了ZSO花形分级超结构的形成机理。
正交晶型的ZSO的荧光性质研究表明,组成花形超结构的次级棒束的分级特征越明显、表面粗糙度越大,荧光光谱的强度越强,反之越弱。表面润湿性研究表明,接触角与表面形貌有关,不同表面形貌的ZSO超结构薄膜与水的接触角不同,次级结构为棒束的ZSO接触角最大,达到143.1°。
3.用ZnO超结构和AgNO3为原料,以浸涂的方法,制备了对甲醇气敏响应较好的Ag/ZnO三维花形超结构；在Ag/ZnO三维花形超结构中,将Ag+负载到ZnO三维花形超结构中亚微米棒的表面,80℃烘干后,Ag+以AgNO3、Ag20的形式存住；300℃热处理后,Ag+转变为金属Ag,同时在ZnO棒表而出现长方形孔。研究发现,Ag+对ZnO亚微米棒的表面有较强的刻蚀作用；Ag+的浓度越高、反应时间越长,刻蚀作用越明显；在Ag+浓度与反应时间不变的情况下,热处理温度决定Ag+对ZnO亚微米棒表面的刻蚀效果。此外,热处理对Ag/ZnO三维花形超结构的气敏性能影响较大,热处理前,超结构对CH30H的灵敏度仅为2.3,而热处理后对CH30H的灵敏度达到9.3。
通过掺杂的方式,获得了光催化性能较好的Cu/ZnO三维花形超结构。在Cu/ZnO三维花形超结构中,当Cu2+的掺杂量低于5%时,Cu2+的作用主要是改变ZnO花形超结构中棒的数量与形貌,即Cu2+掺杂导致组成ZnO三维花形超结构中棒的数量增加,棒的尖端出现台阶形结构,或者刻蚀棒的侧而；Zn2+:Cu2+摩尔比为7:1时,Cu2+负载在六棱柱形ZnO棒的表面,形成CuO/ZnO花形核壳超结构；Zn2+:Cu2+摩尔比为3:1时,产品中单斜晶型CuO与六方晶型ZnO共存；Zn2+:Cu2+摩尔比为3:4时,产物为掺Zn的CuO海胆形纳米超结构。荧光光谱研究表明,Cu2+掺杂量增加,Cu/ZnO三维花形超结构的荧光强度减弱；Cu/ZnO三维花形超结构的光催化性能研究表明,Zn2+:Cu2+摩尔比为7:1时,制备的Cu/ZnO三维花形超结构催化剂在连续降解甲基橙与直接湖蓝染料的过程中表现出良好的催化稳定性,在180 min内,降解率分别达到84.7%、77.6%。
4.以金属Zn为原料,在透射电子显微镜内,用电子束原位辐照的方法制备了形状多样、尺寸可控、单分散、高纯度的金属Zn纳米粒子。Zn纳米粒子形状多样,包括长方形、三角形、菱形与六棱柱形等,它们的直径在10-30 nm之间。在Zn纳米粒子形成过程中,电子束在原材料内部产生的热柱导致材料局部温度迅速升高；电流密度越大,电子剂量越多、电子束的直径越小,导致局部原料升华越迅速,纳米晶体的生长过程越快,得到的Zn纳米粒子越小；辐照时间增长时,小的Zn粒子可以融合成大的Zn纳米粒子。
The properties of inorganic micro/nano-superstructures are dependent on their composition, size, shape and crystalline structure. Investigation on the relationships among these features has attracted increasing attentions in modern science and technology. Zn-based materials superstructures are important for the potential applications, including, photonics, electronics, physics, and chemistry. In this thesis, we have systematically studied and explored the controllable synthesis, assembly, and properties of Zn-based materials superstructures, which include ZnO, Zn silicates, Ag/ZnO and Cu/ZnO composite materials.
1. ZnO 3-dimensiaonal (3D) superstructures with controlled morphology and size, including flower-like, star-like, sphere-like and sea urchin-like shapes, are fabricated by a simple hydrothermal method without any surfactant or template. The gas sensing examinations show that the different Zn-based superstructures have different sensitivity to ethanol, and the sensitivity of the radial-like ZnO 3D flower-like superstructures to ethanol can reach 11.3.
The films made of the ZnO 3D flower-like superstructures on the glass are fabricated by a simple hydrothermal method using the surfactant, and the surface roughness of the ZnO 3D superstructure films can be conveniently controlled by changing the different surfactants and dosage of Zn sources, with excellent reproducibility. The photoluminescence (PL) spectra of the ZnO 3D superstructure films show that their PL properties are dependent on the surface roughness of as-synthesized ZnO superstructure films.
2. Zn4Si2O7(OH)2·H2O (ZSO) 3D hollow flower-like hierarchical superstructure films deposited on the Si substrate are firstly prepared by a simple hydrothermal route. Each hollow superstructure is consisted of secondary rod bundles which are assembled by many primary rods. The morphologies of the ZSO 3D superstructures can be tuned by changing the concentration of reactant, reaction time and temperature, surfactant, the Zn sources and annealing temperature. The results are summarized as follows:(a) The morphology of the secondary rod bundles within the ZSO 3D superstructures can be conveniently controlled from micrometer-sized prism to sub-micrometer slice, sub-micrometer rods and nanorods by only tuning the concentration of Zn2+. (b) The morphology and structure of the ZSO 3D superstructures are related to the reaction time; with the temperature increasing, the rod size of the bundles is getting smaller and the molar ratio of the ZSO:ZnO is increasing. (c) The reaction temperature not only affects the shape of the superstructures, but also changes their compositions. The higher the temperature, the more remarkable is the hierarchical feature of the secondary rod bundle, and the smaller is the size of the primary rods in the secondary bundles, and the higher is the molar ratio of the ZSO:ZnO within a superstructure. (d) The surfactant has effects on the morphology of the secondary rod bundles within the ZSO hierarchical superstructures; it realizes further hierarchy of the secondary bundles as well as their transformation to single non-hierarchical secondary rod. (e) The hierarchical structures of the secondary rod bundles, which realize the transformation from their united secondary bundles to a single secondary micrometer-sized rod, or to a single secondary micro- or nanometer-sized rod with its diameter varying, can be controlled by using different Zn sources. (f) The crystal structure is mainly depended on heating treatment temperature; below 500℃, the crystal structure of the ZSO is not changed, and at 950℃, orthorhombic ZSO superstructure can be transferred into monoclinic Zn2SiO4.
The PL spectra from the orthorhombic ZSO 3D superstructures films show that the stronger the intensity of the PL spectra, the smaller is the diameter of primary rod in secondary rod bundles, and the bigger is the ZSO surface roughness. The investigation on the wettability of the ZSO superstructures films shows that the angle of contact (CA) is mostly relied on the surface shape, and the CA of the ZSO superstructure films varying with their surface shape. It is found that the CA of the ZSO superstructure films consisted of the secondary rod bundles is the highest and reach to 143.1.
3. Ag/ZnO 3D superstructures are prepared by the dip coating process, using as-synthesized ZnO 3D supperstructures and AgN03 as the source materials; these composite superstructures show excellent gas sensitivity to methyl alcohol. Ag+ on the surface of the ZnO submicrorods exits in a form of AgNO3 or Ag2O after being dried at～80℃. Annealing at 300℃, AgNO3 or Ag2O is transformed into metal Ag (nanoparticles) and the rectangular holes form on the surface of the ZnO rods, suggesting that the surface of the ZnO submicrorods can be etched by metal Ag nanoparticles. The etching is enhanced with the increase of the concentration of Ag+ solution and reaction time, and it is also dependent on the heating treatment temperature. The Ag/ZnO 3D superstructures by annealing at 300℃can improve their selectivity to methyl alcohol, and their sensitivity is up to 9.3.
The Cu/ZnO 3D flower-like superstructures with excellent photocatalysis property can be fabricated by doping method. These morphologies of the Cu/ZnO 3D superstructures can be varied by tuning the reactant concentration. When the content of Cu2+ is below 5%, the Cu2+ mainly change the amount and shape of the ZnO rods inside the ZnO 3D superstructure; the doping of Cu2+ leads to the increase of the rods in ZnO 3D superstructure, companying the formation of the step-like shape at the rod top. When the molar ratio of Zn2+: Cu2+ is 7:1, Cu2+ is loaded on the surface of ZnO rods, forming CuO/ZnO core-shell rods. When the molar ratio of Zn2+:Cu2+ is 3:1, the mixture of the CuO and ZnO flower-like rods is obtained. When the molar ratio of Zn2+:Cu2+ is 3:4, the Zn doped CuO urchin-like superstructures are fabricated. The PL intensity of the Cu/ZnO 3D superstructures will decrease with the increasing doping of Cu2+. The Cu/ZnO 3D structures fabricated with the molar ratio of Zn2+ Cu2+ of 7:1 exhibit a higher photocatalytic activity. The efficiencies of the photocatalytic degradation of methyl orange and direct shy blue 5B are investigated; the degradation ratio of the samples reaches 84.7% and 77.6%, respectively.
4. In situ electron-beam irradiation in a transmission electron microscope is performed to fabricate different shape, controllable size, monodispersed, and high pure Zn nanoparticles by using Zn powders as the source material. As-synthesized Zn nanocrystals display various regular geometrical shapes, including rectangle, rhombus, triangle, and hexagon, with a diameter of 10-30 nm. During the formation of Zn nanoparticles, a convergent electron beam is focused on an raw Zn particle, and then cause partial melting and evaporation of the particle and subsequent nucleation and growth of Zn nanoparticles on the C film; the higher the dose of the electron beam, the smaller the diameter of the electron beam, the smaller is the diameters of Zn nanoparticles; while the smaller particles are merged each other under a longer period of the irradiation, resulting in the particles'growth.
引文
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