Ramos-Justicia Juan Francisco, Urbieta Ana, Fernández Paloma
Department of Materials Physics, Faculty of Physics, Complutense University of Madrid, 28040 Madrid, Spain.
Materials (Basel). 2023 Dec 30;17(1):208. doi: 10.3390/ma17010208.
The aim of this study is to prove that resistive heating enables the synthesis of metal/metal oxide composites in the form of core-shell structures. The thickness and morphology of the oxide layer depends strongly on the nature of the metal, but the influences of parameters such as the time and current profiles and the presence of an external field have also been investigated. The systems chosen for the present study are Zn/ZnO, Ti/TiO, and Ni/NiO. The characterization of the samples was performed using techniques based on scanning electron microscopy (SEM). The thicknesses of the oxide layers varied from 10 μm (Zn/ZnO) to 50 μm (Ni/NiO). In the case of Zn- and Ti-based composites, the growth of nanostructures on the oxide layer was observed. Micro- and nanoneedles formed on the ZnO layer while prism-like structures appeared on the TiO. In the case of the NiO layer, micro- and nanocrystals were observed. Applying an external electric field seemed to align the ZnO needles, whereas its effect on TiO and NiO was less appreciable, principally affecting the shape of their grain boundaries. The chemical compositions were analysed using X-ray spectroscopy (EDX), which confirmed the existence of an oxide layer. Structural information was obtained by means of X-ray diffraction (XRD) and was later checked using Raman spectroscopy. The oxide layers seemed to be crystalline and, although some non-stoichiometric phases appeared, the stoichiometric phases were predominant; these were wurtzite, rutile, and cubic for Zn, Ti, and Ni oxides, respectively. The photoluminescence technique was used to study the distribution of defects on the shell, and mainly visible bands (2-2.5 eV), attributed to oxygen vacancies, were present. The near-band edges of ZnO and TiO were also observed around 3.2-3.3 eV.
本研究的目的是证明电阻加热能够合成核壳结构形式的金属/金属氧化物复合材料。氧化层的厚度和形态在很大程度上取决于金属的性质,但也研究了诸如时间和电流分布以及外部场的存在等参数的影响。本研究选择的体系是Zn/ZnO、Ti/TiO和Ni/NiO。使用基于扫描电子显微镜(SEM)的技术对样品进行表征。氧化层的厚度从10μm(Zn/ZnO)到50μm(Ni/NiO)不等。在Zn基和Ti基复合材料中,观察到氧化层上有纳米结构生长。在ZnO层上形成了微米级和纳米级的针状物,而在TiO上出现了棱柱状结构。在NiO层的情况下,观察到了微米级和纳米级晶体。施加外部电场似乎使ZnO针状物排列整齐,而其对TiO和NiO的影响不太明显,主要影响其晶界形状。使用X射线光谱(EDX)分析化学成分,证实了氧化层的存在。通过X射线衍射(XRD)获得结构信息,随后使用拉曼光谱进行检查。氧化层似乎是结晶的,尽管出现了一些非化学计量相,但化学计量相占主导地位;对于Zn、Ti和Ni的氧化物,这些相分别是纤锌矿、金红石和立方相。使用光致发光技术研究壳层上缺陷的分布,主要存在归因于氧空位的可见带(2 - 2.5 eV)。在3.2 - 3.3 eV左右也观察到了ZnO和TiO的近带边。