Brunckova Helena, Mudra Erika, Streckova Magdalena, Medvecky Lubomir, Sopcak Tibor, Shepa Ivan, Kovalcikova Alexandra, Lisnichuk Maksym, Kolev Hristo
Institute of Materials Research, Slovak Academy of Sciences, Watsonova 47, 040 01 Kosice, Slovakia.
Institute of Catalysis, Bulgarian Academy of Sciences, Acad. G. Bonchev St., 1113 Sofia, Bulgaria.
Nanomaterials (Basel). 2022 Aug 17;12(16):2817. doi: 10.3390/nano12162817.
The present study is focused on the synthesis and structural properties of amorphous terbium metal-organic framework thin film (TbMOF-TF) and its transformation to terbium oxide by pyrolysis at 450 °C in the air. The crystalline (cTbMOF) and amorphous (aTbMOF) films were prepared by solvothermal synthesis using different amounts (0.4 and 0.7 mmol) of the modulator (sodium acetate), respectively. The powders were characterized by differential scanning calorimetry (DSC), thermogravimetry (TG), Fourier transform infrared (FTIR), Raman spectroscopy, and scanning electron microscopy (SEM). The varied chemical composition of the surface of TbMOFs and TbO was investigated by X-ray photoelectron spectroscopy (XPS). X-ray diffraction (XRD) and transmission electron microscopy (TEM) revealed that aTbMOF had been fully transformed to a TbO phase with a cubic crystal structure at 450 °C. The amorphous aTbMOF-TF film was prepared by dropping a colloidal solution of amorphous precursor nanocrystals on the SiO/Si substrates covered with Pt as an interlayer. XPS confirmed the presence of Tb in two states, Tb and Tb. The amorphous film has a rough, porous microstructure and is composed of large clusters of worm-like particles, while terbium oxide film consists of fine crystallites of cubic fluorite cF-TbO, c-TbO and c-TbO phases. The surface topography was investigated by a combination of confocal (CM) and atomic force microscopy (AFM). The amorphous film is porous and rough, which is contrast to the crystalline terbium oxide film.
本研究聚焦于非晶态铽金属有机框架薄膜(TbMOF-TF)的合成及其结构性质,以及其在空气中450℃热解转化为氧化铽的过程。分别使用不同量(0.4和0.7 mmol)的调节剂(醋酸钠)通过溶剂热合成制备了晶体(cTbMOF)和非晶态(aTbMOF)薄膜。通过差示扫描量热法(DSC)、热重分析法(TG)、傅里叶变换红外光谱(FTIR)、拉曼光谱和扫描电子显微镜(SEM)对粉末进行了表征。通过X射线光电子能谱(XPS)研究了TbMOFs和TbO表面的不同化学成分。X射线衍射(XRD)和透射电子显微镜(TEM)表明,aTbMOF在450℃时已完全转变为具有立方晶体结构的TbO相。通过将非晶态前驱体纳米晶体的胶体溶液滴在覆盖有Pt作为中间层的SiO/Si衬底上制备了非晶态aTbMOF-TF薄膜。XPS证实了存在两种状态的Tb,即Tb和Tb。非晶态薄膜具有粗糙的多孔微观结构,由大量蠕虫状颗粒簇组成,而氧化铽薄膜由立方萤石cF-TbO、c-TbO和c-TbO相的细晶粒组成。通过共聚焦显微镜(CM)和原子力显微镜(AFM)相结合的方法研究了表面形貌。非晶态薄膜是多孔且粗糙的,这与晶体氧化铽薄膜形成对比。