氧化物及氢氧化物纳米材料的制备和表征
摘要
本文采用液相法(水热法和溶剂热法)成功地制备了方形花状层次结构的ZnO微晶、类球形ZnO微球、六边形β-Ni(OH)2纳米片和花状β-Ni(OH)2微球,利用透射电镜、扫描电镜、X-射线衍射、紫外可见光谱等手段,研究了实验条件对产物结构、形貌和性质的影响以及可能的反应机理。
1.以硝酸锌为锌源,以SDBS和OP-10为表面活性剂,利用它们的协同作用来共同修饰氧化锌,以柠檬酸三钠为配位剂,在100℃进行水热反应24h,可以得到方形花状的ZnO微晶。采用SEM对产物的形貌和微观形态进行表征,结果表明,所得ZnO层次结构为方形花状,大小均匀,分散性好。每个方形ZnO微晶的长度约为2.7μm,宽度约为2.1μm。ZnO层次结构微晶是由厚度为20nm的ZnO纳米片自组装成的。我们在室温下研究了ZnO微晶的光致发光性质和光催化性质,结果表明ZnO具有良好的光学性质。我们还详细考察了各种实验条件对产物微观形态的影响和产物的反应机理。
2.在保持其他条件不变的情况下,选用乙二醇作为溶剂,采用溶剂热法在170℃制备了类球形的ZnO微晶。采用SEM和TEM对ZnO的形貌和微观结构进行表征,结果表明,产物主要为表面粗糙的类球形ZnO微晶,直径约为0.35μm。并且ZnO微球是由ZnO纳米粒子组装成的。我们在室温下考察了ZnO微晶的光致发光性质和紫外特性,结果表明ZnO具有良好的光学性质。我们还详细考察了各种实验条件对产物微观形态的影响和产物的反应机理。
3.以硫酸镍为镍源,NaOH为碱源,在有机添加剂草酸铵的作用下,采用水热法可以在170℃下反应24h得到了氢氧化镍纳米片。而当使用乙二胺作为添加剂时,得到了花状氢氧化镍微球。采用SEM对产物的形貌和微观形态进行表征,结果表明,以草酸铵作为添加剂得到的六边形氢氧化镍纳米片大小约为96nm,厚度为约20nm;以乙二胺作为添加剂得到的花状氢氧化镍微球直径约为2.2μm,是由厚度为0.13μm六边形的纳米片的组装成的。我们采用循环伏安法测试了β-Ni(OH)2电化学性质,结果表明β-Ni(OH)2具有较好的电化学性质。
In this paper, cuboid-shaped ZnO with hierarchical structures, sphere-shaped ZnO microstructures, hexagon-likeβ-Ni(OH)2 nanoflakes and flower-likeβ-Ni(OH)2 microspheres were successfully prepared through a facile hydrothermal approach. The influence of fabrication conditions on the structure and morphology of ordered nanostuctures were characterized by TEM, SEM, XRD,PL and UV-Vis spectrometer. The synthesis mechanism and experiment conditions were also studied. The results and conclusions are as followed:
1. Cuboid-shaped ZnO with hierarchical structures were prepared by rection of Zn(NO3)2 and NaOH through a mixed surfactants mediated hydrothermal method at 100℃for 24h. The morphologies and the structures were characterized by SEM and TEM. It has been found that the product consist of a large quantity of nearly monodisperse cuboid-shaped microparticles of 2.7μm in length and 2.1μm in width, and almost all of them have uniform size and present one kind of structure. The as-prepared samples were constructed with many interleaving nanosheets in a perfectly aligned manner. The nanosheet building blocks are about 20 nm in thickness and several hundred nanometers in width. Room temperature photoluminescence spectrum of the as-obtained ZnO hierarchitectures was recorded showing multiple peaks of visible emissions in bluegreen region. The influence of various experimental conditions on the reaction has been investigated in detail.
2. ZnO microspheres has been successfully synthesized in glycol mixed solvent via a facile solvothermal process with SDBS and OP-10 surfactants in the presence of Trisodium citrate at 170℃for 24h. The results were characterized using scanning electron microscopy (SEM) and transmission electron microscope(TEM). It has been found that the products were consisted of a large quantity of nearly monodisperse microspheres of 3.5μm in diameter. The microspheres were constructed with ZnO nanoparticles and the surface of the microspheres is rough. The influence of various experimental conditions on the reaction has been investigated in detail.
3.β-Ni(OH)2 nanoflakes and flower-likeβ-Ni(OH)2 microspheres were synthesized by rection of NiSO4 and NaOH via a simple hydrothermal process with additives of ammonium oxalate or 1,2-ethylenediamine at 170℃for 24h. The SEM observation results displayed that the samples were uniform in size. The electrochemical property of the sample was obtained through cyclic voltammetry method.
1.以硝酸锌为锌源,以SDBS和OP-10为表面活性剂,利用它们的协同作用来共同修饰氧化锌,以柠檬酸三钠为配位剂,在100℃进行水热反应24h,可以得到方形花状的ZnO微晶。采用SEM对产物的形貌和微观形态进行表征,结果表明,所得ZnO层次结构为方形花状,大小均匀,分散性好。每个方形ZnO微晶的长度约为2.7μm,宽度约为2.1μm。ZnO层次结构微晶是由厚度为20nm的ZnO纳米片自组装成的。我们在室温下研究了ZnO微晶的光致发光性质和光催化性质,结果表明ZnO具有良好的光学性质。我们还详细考察了各种实验条件对产物微观形态的影响和产物的反应机理。
2.在保持其他条件不变的情况下,选用乙二醇作为溶剂,采用溶剂热法在170℃制备了类球形的ZnO微晶。采用SEM和TEM对ZnO的形貌和微观结构进行表征,结果表明,产物主要为表面粗糙的类球形ZnO微晶,直径约为0.35μm。并且ZnO微球是由ZnO纳米粒子组装成的。我们在室温下考察了ZnO微晶的光致发光性质和紫外特性,结果表明ZnO具有良好的光学性质。我们还详细考察了各种实验条件对产物微观形态的影响和产物的反应机理。
3.以硫酸镍为镍源,NaOH为碱源,在有机添加剂草酸铵的作用下,采用水热法可以在170℃下反应24h得到了氢氧化镍纳米片。而当使用乙二胺作为添加剂时,得到了花状氢氧化镍微球。采用SEM对产物的形貌和微观形态进行表征,结果表明,以草酸铵作为添加剂得到的六边形氢氧化镍纳米片大小约为96nm,厚度为约20nm;以乙二胺作为添加剂得到的花状氢氧化镍微球直径约为2.2μm,是由厚度为0.13μm六边形的纳米片的组装成的。我们采用循环伏安法测试了β-Ni(OH)2电化学性质,结果表明β-Ni(OH)2具有较好的电化学性质。
In this paper, cuboid-shaped ZnO with hierarchical structures, sphere-shaped ZnO microstructures, hexagon-likeβ-Ni(OH)2 nanoflakes and flower-likeβ-Ni(OH)2 microspheres were successfully prepared through a facile hydrothermal approach. The influence of fabrication conditions on the structure and morphology of ordered nanostuctures were characterized by TEM, SEM, XRD,PL and UV-Vis spectrometer. The synthesis mechanism and experiment conditions were also studied. The results and conclusions are as followed:
1. Cuboid-shaped ZnO with hierarchical structures were prepared by rection of Zn(NO3)2 and NaOH through a mixed surfactants mediated hydrothermal method at 100℃for 24h. The morphologies and the structures were characterized by SEM and TEM. It has been found that the product consist of a large quantity of nearly monodisperse cuboid-shaped microparticles of 2.7μm in length and 2.1μm in width, and almost all of them have uniform size and present one kind of structure. The as-prepared samples were constructed with many interleaving nanosheets in a perfectly aligned manner. The nanosheet building blocks are about 20 nm in thickness and several hundred nanometers in width. Room temperature photoluminescence spectrum of the as-obtained ZnO hierarchitectures was recorded showing multiple peaks of visible emissions in bluegreen region. The influence of various experimental conditions on the reaction has been investigated in detail.
2. ZnO microspheres has been successfully synthesized in glycol mixed solvent via a facile solvothermal process with SDBS and OP-10 surfactants in the presence of Trisodium citrate at 170℃for 24h. The results were characterized using scanning electron microscopy (SEM) and transmission electron microscope(TEM). It has been found that the products were consisted of a large quantity of nearly monodisperse microspheres of 3.5μm in diameter. The microspheres were constructed with ZnO nanoparticles and the surface of the microspheres is rough. The influence of various experimental conditions on the reaction has been investigated in detail.
3.β-Ni(OH)2 nanoflakes and flower-likeβ-Ni(OH)2 microspheres were synthesized by rection of NiSO4 and NaOH via a simple hydrothermal process with additives of ammonium oxalate or 1,2-ethylenediamine at 170℃for 24h. The SEM observation results displayed that the samples were uniform in size. The electrochemical property of the sample was obtained through cyclic voltammetry method.
引文
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