Faculty of Chemistry and Food Chemistry, Technische Universität Dresden, 01062, Dresden, Germany.
Department of Inorganic Chemistry, University of Yaoundé I, P.O. Box 812, Yaoundé, Cameroon.
ChemistryOpen. 2023 Apr;12(4):e202300045. doi: 10.1002/open.202300045.
In search of a suitable single-source precursor for the deposition of nanostructured PbS thin films at moderate temperatures under ambient conditions, we have synthesized the ligand N-(thiomorpholine-4-carbothioyl)benzamide and its corresponding lead(II) complex. The structures of both compounds were determined by single-crystal X-ray diffraction. In the complex, two ligands coordinate to a lead(II) atom in hemi-directed geometry through S and O atoms. Secondary intermolecular Pb⋅⋅⋅S interactions group the complexes into pairs. As bulk powders, both the ligand and complex show nominal composition and purity as evidenced by elemental analysis, H NMR and IR spectroscopy. Thermal analysis of the lead(II) complex was carried out to understand its thermal decomposition behaviour for establishing a thin film fabrication protocol. Thin films of phase-pure PbS were fabricated using this new molecular precursor at the comparatively low annealing temperature of 250 °C. The film showed nanoparticles with cuboidal morphology and a blue-shifted optical absorption.
为了寻找一种合适的单源前体，以便在环境条件下于中温沉积纳米结构的 PbS 薄膜，我们合成了配体 N-(硫代吗啉-4-甲酰硫基)苯甲酰胺及其相应的铅(II)配合物。这两种化合物的结构均通过单晶 X 射线衍射确定。在配合物中，两个配体通过 S 和 O 原子以半指向性几何构型与一个铅(II)原子配位。次级的分子间 Pb⋅⋅⋅S 相互作用将配合物成对组合在一起。作为块状粉末，配体和配合物均表现出标称组成和纯度，这一点通过元素分析、1H NMR 和 IR 光谱得到了证实。对铅(II)配合物进行了热分析，以了解其热分解行为，从而建立一个薄膜制造方案。使用这种新的分子前体，在相对较低的 250°C 退火温度下制备出了相纯的 PbS 薄膜。该薄膜表现出具有立方体形貌和蓝移光吸收的纳米颗粒。
