Chemistry of Light Elements and Clusters Laboratory, Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences, 119991 Moscow, Russia.
Institute of Materials for Modern Energy and Nanotechnology IMSEN-IFH, Mendeleev University of Chemical Technology of Russia, 125047 Moscow, Russia.
Molecules. 2023 Mar 9;28(6):2515. doi: 10.3390/molecules28062515.
The hydrothermal synthesis of nickel oxide in the presence of triethanolamine was studied. Furthermore, the relationship between the synthesis conditions, thermal behavior, crystal structure features, phase composition and microstructure of semi-products, and the target oxide nanopowders was established. The thermal behavior of the semi-products was studied using a simultaneous thermal analysis (in particular, using one that involved thermogravimetric analysis and differential scanning calorimetry, TGA/DSC). An X-ray diffraction (XRD) analysis revealed that varying the triethanolamine and nickel chloride concentration in the reaction system can govern the formation of α- and β-Ni(OH)-based semi-products that contain Ni(HCO) or Ni(CO)(OH) as additional components. The set of functional groups in the powders was determined using a Fourier-transform infrared (FTIR) spectroscopy analysis. Using microextrusion printing, a composite NiO-(CeO)(SmO) anode film was fabricated. Using XRD, scanning electron microscopy (SEM), and atomic force microscopy (AFM) analyses, it was demonstrated that the crystal structure, dispersity, and microstructure character of the obtained material correspond to the initial nanopowders. Using Kelvin probe force microscopy (KPFM) and scanning capacitance microscopy (SCM), the local electrophysical properties of the printed composite film were examined. The value of its conductivity was evaluated using the four-probe method on a direct current in the temperature range of 300-650 °C. The activation energy for the 500-650 °C region, which is of most interest in the context of intermediate-temperature SOFCs working temperatures, has been estimated.
采用三乙醇胺研究了水热条件下氧化镍的合成。此外,建立了半产物的合成条件、热行为、晶体结构特征、相组成和微观结构与目标氧化物纳米粉末之间的关系。通过同步热分析(特别是使用热重分析和差示扫描量热法,TGA/DSC)研究了半产物的热行为。X 射线衍射(XRD)分析表明,改变反应体系中三乙醇胺和氯化镍的浓度可以控制基于α-和β-Ni(OH)的半产物的形成,其中包含 Ni(HCO)或 Ni(CO)(OH)作为附加成分。使用傅里叶变换红外(FTIR)光谱分析确定了粉末中的官能团。通过微挤出打印制备了复合 NiO-(CeO)(SmO)阳极膜。通过 XRD、扫描电子显微镜(SEM)和原子力显微镜(AFM)分析,证明了所获得材料的晶体结构、分散性和微观结构特征与初始纳米粉末相对应。使用 Kelvin 探针力显微镜(KPFM)和扫描电容显微镜(SCM)研究了打印复合膜的局部电物理性质。使用直流四探针法在 300-650°C 的温度范围内评估了其电导率值。估计了 500-650°C 区域的活化能,这在中温 SOFC 工作温度范围内最感兴趣。