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在水热条件下合成了三个镧系超分子化合物[Ln(HBIC)3]n[Ln=Sm(1),Ho(2),Yb(3);H2BIC=1H-苯并咪唑-2-羧酸],其中化合物1、2呈单晶态,化合物3则为粉末样品;借助单晶X射线衍射(XRD)、粉末衍射、元素分析、红外(IR)光谱、热分析等手段对化合物进行了表征.结构分析表明,1-3为同构化合物,都呈现二维的平面结构,其中每一个镧系金属中心与来自五个HBIC-配体的三个氮原子和五个氧原子以两种新的配位模式配位形成一个轻微扭曲的双帽三棱柱几何构型,相邻的二维(2D)平面进一步通过强的氢键作用形成了一个三维(3D)的超分子结构.热重分析结果表明,化合物1-3在360°C前均保持稳定,呈现出良好的热稳定性.基于Kissinger和Ozawa-Doyle两种方法,通过差示扫描量热(DSC)技术研究得到了化合物1热分解的动力学参数(指前因子AK=1.286×108s-1;活化能EK=199.3kJ·mol-1,EO=205.2kJ·mol-1).另外,也研究了室温下化合物1和3的固态发光性能,结果表明,化合物1和3分别在可见光区和近红外光区呈现出相应镧系金属离子的特征发射.
Three Ln (HBn) 3] n [Ln = Sm (1), Ho (2) and Yb (3) were synthesized under hydrothermal conditions. H2BIC = 1H-benzimidazol- Carboxylic acid]. Compounds 1, 2 were single crystal and compound 3 was powder. The compounds were characterized by X-ray diffraction (XRD), powder diffraction, elemental analysis, infrared spectrum and thermal analysis The structural analysis shows that 1-3 are isomorphic compounds, all present a two-dimensional planar structure in which each lanthanide metal center with five HBIC-ligand from three nitrogen atoms and five oxygen atoms in two The new coordination mode coordination forms a slightly twisted double cap triangular prism geometry, and the adjacent two-dimensional (2D) plane further forms a three-dimensional (3D) supramolecular structure by strong hydrogen bonding. The results of reanalysis showed that compound 1-3 remained stable and showed good thermal stability before 360 ° C. Based on the Kissinger and Ozawa-Doyle methods, the compounds were obtained by differential scanning calorimetry (DSC) The kinetic parameters of thermal decomposition (pre-factor AK = 1.286 × 108s-1; activation energy EK = 199.3kJ · mol-1 and EO = 205.2kJ · mol-1) Compound 1 and 3 of the solid state light emitting properties, the results indicate that compounds 1 and 3 wherein each transmitter corresponding rendered lanthanide metal ions in the visible and near infrared regions.